CN108160009B - Reactor capable of self-balancing internal and external pressures of liner tube and use method - Google Patents
Reactor capable of self-balancing internal and external pressures of liner tube and use method Download PDFInfo
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- CN108160009B CN108160009B CN201611114842.5A CN201611114842A CN108160009B CN 108160009 B CN108160009 B CN 108160009B CN 201611114842 A CN201611114842 A CN 201611114842A CN 108160009 B CN108160009 B CN 108160009B
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/042—Pressure vessels, e.g. autoclaves in the form of a tube
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- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
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Abstract
The invention relates to a reactor capable of self-balancing the internal and external pressures of a liner tube and application thereof. The pressure-bearing shell bears high pressure, the lining is made of inert materials and does not participate in reaction, the inlet and the outlet are sealed with the pressure-bearing shell, the pressure-bearing shell is protected from being corroded by reactants, meanwhile, the shell materials are prevented from interfering with reaction results, the pressure balance valve and the self-protection pressure release valve guarantee that the pressure inside and outside the lining is balanced in the pressure increasing and reducing process, the pressure difference is avoided, the lining is broken, and meanwhile, the function of the safety valve is achieved under the condition that the pressure at the front end is too high or. The reactor can be used at room temperature of-800 ℃ and 0pa-13Mpa, and has the advantages of simple manufacture, low cost, convenient installation and use, more reliable data, corrosion resistance, high safety and the like.
Description
Technical Field
The invention relates to a high-temperature high-pressure multiphase reactor and a using method thereof, in particular to a high-temperature high-pressure multiphase reactor with a lining pipe for self-balancing internal and external pressures of a lining pipe and a using method thereof.
Background
The gas-solid phase reaction is the most common and important reaction in heterogeneous catalysis, and the corresponding reaction device is widely used. For the catalytic reaction of gas and solid phases, the most commonly used reaction tube material at present is mainly quartz glass, the reaction tube material is high temperature resistant and chemically inert, although the influence of the reaction tube on the catalytic reaction result does not exist, the material is fragile and easy to break, and the material can only be applied to normal pressure reaction. High-pressure reactions are also carried out in gas-solid reactions and in the common synthesis gas chemistry, which is very important in the energy field, for example, ammonia synthesis reactions and the like, under high pressure. Aiming at the problem that a high-pressure reaction researcher usually uses a metal reaction tube for reaction test, the metal reaction tube, such as a stainless steel reaction tube, has the advantages of good heat conduction, high temperature and high pressure resistance and the like, but has the following problems that the metal reaction tube is a high-activity catalyst in a plurality of reactions, elements such as iron, nickel, molybdenum and the like are widely applied to a series of reactions such as synthesis gas conversion, hydrogenation, oxidation, ammonia synthesis and the like, and the direct use of the metal reaction tube as a reactor often causes the reliability of a test result to be greatly reduced because the reaction tube has activity under the reaction conditions, and even misleads the researcher. One method is to measure the difference of the reaction activity of the hollow tube to the performance of the hollow tube in each test, however, the performance of the reaction tube is different under different reaction conditions, and the surface structure composition of the inner wall of the reaction tube is changed continuously along with the long-time activation under some atmosphere, so that the performance of the hollow tube is different every time, and the difference is still large. The inner lining tube is introduced into the metal tube gradually by some researchers, one way is to coat or plate the inner wall of the metal tube with an inert component, such as quartz, and this method is really effective to eliminate the effect of the tube wall effect, however, this method is complex and expensive in processing technology, and the reaction tube usually has the inner coating layer broken and peeled off after a period of use due to different thermal expansion coefficients of the metal and the coating layer at high temperature, which results in the damage of the reaction tube. The other method is to use a quartz liner tube in a metal sleeve, wherein the upper part and the lower part of the liner tube are sealed by O-rings, but the mode of sealing the two ends often causes great pressure difference inside and outside the quartz tube, so that the quartz tube is easy to break. And the other method is to seal the upper end between the metal tube and the quartz tube by using an O-shaped silica gel ring to ensure that the air flow only passes through the quartz tube and the lower end is not sealed, so that the internal and external pressures of the quartz tube are balanced. Although the tube wall effect of the reaction tube is greatly reduced compared with that of a tube without an inner lining tube, after the reaction tube is used for a long time, the fact that dead volume reaction gas exists between the quartz tube and the lower end of the metal tube and is not sealed is discovered, side reaction often occurs in a crack, corresponding products still diffuse to an outlet due to concentration gradient difference, and the final product analysis result is still inevitably influenced. The existing companies have further improved and optimized the reaction tube, and the influence of the tube wall effect is thoroughly eliminated by adding one path of inert gas purging in a dead volume area, but the method greatly improves the complexity and cost of the gas path system on one hand, and on the other hand, the inert gas can dilute the component concentration of the reaction product, so that the detection error of products with low concentration is correspondingly increased, and even the repeatability of data can be reduced due to uneven mixing of the diluent gas.
Disclosure of Invention
Aiming at the problems, the invention discloses a high-temperature high-pressure multiphase reactor with a lining pipe and self-balancing liner pipe internal and external pressures and a using method thereof.
The utility model provides a reactor of self-balancing inside and outside pressure of bushing pipe which characterized in that: the pressure-bearing device comprises a hollow cylindrical pressure-bearing shell with two open ends and a hollow cylindrical inert lining with two open ends, wherein the inert lining is sleeved in the pressure-bearing shell in a penetrating way, a gap is reserved between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, an annular lining inlet sealing ring and an annular lining outlet sealing ring are sleeved on the outer wall surface of the inert lining, the two ends of the gap between the lining inlet sealing ring and the lining outlet sealing ring are sealed, and a sealed crack is formed between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing; two open ends of the inert lining are respectively used as a reaction material inlet and a reaction material outlet; one end of the conduit with two open ends is communicated with the closed crack, the other end is positioned at the inlet end of the inert lining, the conduit is provided with a pressure balance valve, and the pressure balance valve is a one-way valve which allows gas to flow from the inlet end to the crack; and one end of the other conduit with two open ends is communicated with the closed crack, the other end of the conduit is positioned at the outlet end of the inert lining, the conduit is provided with a self-protection pressure release valve, and the self-protection pressure release valve is a one-way valve which only allows gas to flow from the crack to the outlet end.
The inert lining is positioned in the pressure-bearing shell, and the inlet end and the outlet end of the inert lining are sealed with the pressure-bearing shell through an annular sealing ring; a crack is formed between the pressure-bearing shell and the inert lining, the pressure balance valve is connected between an air inlet at the inlet end of the inert lining and the crack through a pipeline, and the air flow direction of the pressure balance valve only allows the air flow from the air inlet to the crack; the self-protection pressure release valve is connected with the crack and a tail gas outlet at the outlet end of the inert lining through a pipeline, and the gas flow direction is only allowed to flow from the crack to the tail gas outlet; in a stable pressure state, the gas only flows through the inner lining pipe and cannot flow through the crack.
The upper end and the lower end of the pressure-bearing shell are respectively connected with the air inlet pipe and the air outlet pipe in a sealing way, and the joint of the upper end of the pressure-bearing shell and the air inlet pipe or the joint of the lower end of the pressure-bearing shell and the air outlet pipe can be opened and closed for sealing, so that the inert lining can be taken and placed.
The pressure-bearing shell is a circular tube, two cylindrical screw caps with external screw threads are sleeved on the external wall surface of the circular tube, an annular boss A is radially arranged on the external wall surface of the opening end of the pressure-bearing shell, the internal diameter of each screw cap is smaller than the external diameter of the annular boss A, an annular boss B is radially arranged on the external wall of the connecting end of the air inlet pipe and the air outlet pipe with the pressure-bearing shell, two cylindrical press covers with internal screw threads are arranged at the upper ends of the lower end openings of the two internal screw threads, through holes are formed in the middle parts of the closed ends of the press covers, the air inlet pipe and the air outlet pipe are respectively sleeved in the through holes of the two press covers, the internal diameter of each through hole is smaller than the external.
The inner wall surface of the two opening ends of the pressure-bearing shell is respectively provided with an annular depressed part which is coaxial with the pressure-bearing shell and is provided with an internal thread, the pressure-bearing shell and the inert lining are respectively a round pipe, the inert lining is coaxially sleeved in the pressure-bearing shell, a lining inlet sealing ring and a lining outlet sealing ring are arranged in the annular depressed parts, two pressure caps with through holes in the middle of the external thread are respectively screwed in the annular depressed parts at the two ends of the pressure-bearing shell, and the two ends of the inert lining are respectively sleeved in the through holes of the two pressure caps; a gap is left between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, and a lining inlet sealing ring and a lining outlet sealing ring are arranged on the inner wall surface of the inert lining.
A catalyst or a sample to be detected is placed in the inert lining, the area for placing the catalyst or the sample to be detected is used as a reaction furnace, the lining inlet sealing ring and the lining outlet sealing ring are positioned at two ends of the reaction furnace or are far away from the area outside the two ends of the reaction furnace, the environmental temperature is ensured to be lower than 200 ℃, and the sealing ring can be made of one or two of rubber, tetrafluoroethylene, graphite and silica gel for sealing;
the pressure-bearing shell is made of high-temperature and high-pressure resistant materials, bears external pressure, and resists pressure of 13Mpa below 600 ℃, such as stainless steel;
the inert lining tube material is one or more than two of quartz, corundum, silicon carbide, titanium oxide and zirconium oxide.
A crack is formed between the pressure-bearing shell and the inert lining, and solid or high-temperature-resistant heat-conducting solid materials can be filled in the crack; the starting pressure of the pressure balancing valve and the self-protection pressure relief valve is less than 3 atmospheres, and preferably 0.5 to 2 atmospheres.
When in use, the upper end or the lower end of the reaction tube is opened, the inert lining is taken out, and a sample to be measured or a catalyst is filled after cleaning; installing an inert lining in the pressure-bearing shell, sealing the upper end and the lower end of the inert lining with the pressure-bearing shell through a sealing ring, sealing the upper end of the reaction tube, and respectively connecting the upper end and the lower end of the pressure-bearing shell with an air inlet pipe and an air outlet pipe; when a high-pressure experiment is carried out, a back pressure valve needs to be installed behind the air outlet, and the outlet end of the self-protection pressure release valve is connected between the air outlet and the back pressure valve.
If corrosive components exist in the raw material atmosphere, the pressure of the inner side and the outer side of the inert lining in the pressure-bearing shell needs to be increased in the non-corrosive atmosphere, and the inert lining is switched to be the same as the reaction raw material gas after the pressure is stable to purge and replace the gas in the inert lining; if the pressure needs to be increased in the process of the experiment, the pressure needs to be increased in the inert atmosphere firstly, and then the reaction atmosphere is switched to purge and replace the atmosphere in the inert lining
If the pressure needs to be reduced in the experimental process, the pressure needs to be firstly released to the target pressure, then the pressure needs to be increased to the target pressure after 2 atmospheric pressures are stable, and the test is carried out.
The invention also uses the gaskets at the upper end and the lower end of the lining pipe for sealing, automatically balances the internal pressure and the external pressure of the lining pipe during pressure boosting by using the pressure balance valve and the self-protection pressure relief valve, ensures that gas only flows through the inner part of the lining pipe and cannot flow through a crack under the pressure stabilizing state by using the starting pressure difference of the one-way valve, and can fill high-pressure inert gas between the pressure-bearing shell and the inert lining pipe through a simple pressure boosting procedure, so that the reaction pipe cannot be corroded by the strong corrosive components in time, and in addition, when the catalyst bed layer and the following blockage and the like occur, the pressure balance valve and the self-protection pressure relief valve can play a pressure relief role so as to ensure. The invention solves the problems, and has the advantages of simple manufacture, lower cost, easy installation and safer use.
The pressure-bearing shell bears high pressure, the lining is made of inert materials and does not participate in reaction, the inlet and the outlet are sealed with the pressure-bearing shell, the pressure-bearing shell is protected from being corroded by reactants, meanwhile, the interference of shell materials on reaction results is prevented, the pressure balance valve and the self-protection pressure release valve guarantee the balance of the internal pressure and the external pressure of the lining in the pressure increasing and reducing process, the lining is prevented from being broken due to pressure difference, and meanwhile, the pressure-bearing shell plays a role of a safety valve under the condition that the pressure at the. The reactor can be used at room temperature of-800 ℃ and 0pa-13Mpa, and has the advantages of simple manufacture, low cost, convenient installation and use, more reliable data, corrosion resistance, high safety and the like.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the claims of the present invention is not limited by these examples. Meanwhile, the examples only show some conditions for realizing the present invention but do not mean that these conditions must be satisfied to achieve the object.
The reactor used in the embodiment is provided with a hollow cylindrical 316 stainless steel pressure-bearing shell with two open ends, an outer diameter of 12mm, an inner diameter of 9mm, a hollow cylindrical inert quartz lining with two open ends, an outer diameter of 8mm, an inner diameter of 6mm, and a porous sand plate at a position 1.5cm lower than half height for supporting a catalyst, wherein the inert lining is sleeved in the pressure-bearing shell in a penetrating way, a gap is reserved between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, an annular lining inlet sealing ring and an annular lining outlet sealing ring are sleeved on the outer wall surface of the inert lining, the sealing rings are made of fluororubber O-shaped ring materials, two ends of the gap between the inner lining inlet sealing ring and the lining outlet sealing ring are sealed, and a sealed crack is formed between; two open ends of the inert lining are respectively used as a reaction material inlet and a reaction material outlet; one end of the conduit with two open ends is communicated with the closed crack, the other end is positioned at the inlet end of the inert lining, the conduit is provided with a pressure balance valve, the pressure balance valve is a one-way valve which allows gas to flow from the inlet end to the crack, and the starting pressure is 1.5 atm; and one end of the other conduit with two open ends is communicated with the closed crack, the other end of the conduit is positioned at the outlet end of the inert lining, the conduit is provided with a self-protection pressure release valve, the self-protection pressure release valve is a one-way valve which only allows gas to flow from the crack to the outlet end, and the starting pressure is 1.5 atm.
The inert lining is positioned in the pressure-bearing shell, and the inlet end and the outlet end of the inert lining are sealed with the pressure-bearing shell through an annular sealing ring; a crack is formed between the pressure-bearing shell and the inert lining, the pressure balance valve is connected between an air inlet at the inlet end of the inert lining and the crack through a pipeline, and the air flow direction of the pressure balance valve only allows the air flow from the air inlet to the crack; the self-protection pressure release valve is connected with the crack and a tail gas outlet at the outlet end of the inert lining through a pipeline, and the gas flow direction is only allowed to flow from the crack to the tail gas outlet; in a stable pressure state, the gas only flows through the inner lining pipe and cannot flow through the crack.
The upper end and the lower end of the pressure-bearing shell are respectively connected with the air inlet pipe and the air outlet pipe in a sealing way, and the joint of the upper end of the pressure-bearing shell and the air inlet pipe or the joint of the lower end of the pressure-bearing shell and the air outlet pipe can be opened and closed for sealing, so that the inert lining can be taken and placed.
The pressure-bearing shell is a circular tube, two cylindrical screw caps with external screw threads are sleeved on the external wall surface of the circular tube, an annular boss A is radially arranged on the external wall surface of the opening end of the pressure-bearing shell, the internal diameter of each screw cap is smaller than the external diameter of the annular boss A, an annular boss B is radially arranged on the external wall of the connecting end of the air inlet pipe and the air outlet pipe with the pressure-bearing shell, two cylindrical press covers with internal screw threads are arranged at the upper ends of the lower end openings of the two internal screw threads, through holes are formed in the middle parts of the closed ends of the press covers, the air inlet pipe and the air outlet pipe are respectively sleeved in the through holes of the two press covers, the internal diameter of each through hole is smaller than the external.
The inner wall surface of the two opening ends of the pressure-bearing shell is respectively provided with an annular depressed part which is coaxial with the pressure-bearing shell and is provided with an internal thread, the pressure-bearing shell and the inert lining are respectively a round pipe, the inert lining is coaxially sleeved in the pressure-bearing shell, a lining inlet sealing ring and a lining outlet sealing ring are arranged in the annular depressed parts, two pressure caps with through holes in the middle of the external thread are respectively screwed in the annular depressed parts at the two ends of the pressure-bearing shell, and the two ends of the inert lining are respectively sleeved in the through holes of the two pressure caps; a gap is left between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, and a lining inlet sealing ring and a lining outlet sealing ring are arranged on the inner wall surface of the inert lining.
A catalyst or a sample to be detected is placed in the inert lining at the crack, the area where the catalyst or the sample to be detected is placed is used as a reaction furnace, the lining inlet sealing ring and the lining outlet sealing ring are positioned at two ends of the reaction furnace or the area far away from the two ends of the reaction furnace, the environment temperature is ensured to be lower than 200 ℃, and the sealing ring is made of fluororubber for sealing;
example 1
The synthesis gas direct conversion empty pipe experiment: opening the upper end or the lower end of the reaction tube, taking out the inert lining, directly installing the inert lining in the pressure-bearing shell without filling a catalyst after cleaning, sealing the upper end and the lower end of the reaction tube with the pressure-bearing shell through a sealing ring, sealing the upper end of the reaction tube, and respectively connecting the upper end and the lower end of the pressure-bearing shell with an air inlet pipe and an air outlet pipe; a back pressure valve is arranged behind the air outlet, and the outlet end of the self-protection pressure release valve is connected between the air outlet and the back pressure valve. And (3) installing an open-hearth tubular furnace in the equal-diameter area in the middle of the pressure-bearing shell, and ensuring that the constant-temperature section of the tubular furnace corresponds to the inert lining catalyst filling area.
After sealing, the pressure of raw material gas (5% Ar (internal standard), 47.5% CO and 47.5% H2) is increased by 4Mpa, leakage detection is carried out by using a combustible gas alarm, after sealing is confirmed, the temperature is increased to 400 ℃, the flow of a mass flow meter is controlled by 24sccm to carry out reaction, and outlet tail gas analysis is carried out by using gas chromatography.
According to the chromatographic result, the CO conversion rate is calculated to be 0 percent
Example 2: and (3) evaluating the reaction of the catalyst for preparing olefin by directly converting the synthesis gas:
opening the upper end or the lower end of the reaction tube, taking out the inert lining, filling quartz wool with the height of 0.3cm after cleaning, and then filling the catalyst: ZnCrAl + SAPO34, 280mg, finally filling 0.3cm high quartz wool, installing an inert lining in the pressure-bearing shell, sealing the upper end and the lower end of the inert lining with the pressure-bearing shell through a sealing ring, sealing the upper end and the lower end of the reaction tube, and respectively connecting the upper end and the lower end of the pressure-bearing shell with an air inlet pipe and an air outlet pipe; a back pressure valve is arranged behind the air outlet, and the outlet end of the self-protection pressure release valve is connected between the air outlet and the back pressure valve. And (3) installing an open-hearth tubular furnace in the equal-diameter area in the middle of the pressure-bearing shell, and ensuring that the constant-temperature section of the tubular furnace corresponds to the inert lining catalyst filling area.
After sealing, the pressure of raw material gas (5% Ar (internal standard), 47.5% CO and 47.5% H2) is increased by 4Mpa, leakage detection is carried out by using a combustible gas alarm, after sealing is confirmed, the temperature is increased to 400 ℃, the flow of a mass flow meter is controlled by 24sccm to carry out reaction, and outlet tail gas analysis is carried out by using gas chromatography.
CO conversion 17%, CO2 selectivity 42% C
Hydrocarbon distribution: methane 2%, ethylene-butene 80%, others 18%.
Comparative example 1: a reactor: a hollow cylindrical 316 stainless steel pipe is provided with a metal orifice plate at the position of 8mm of outer diameter, 6mm of inner diameter and 1.5cm lower than the middle height, 0.3cm of quartz wool is filled firstly, ZnCrAl + SAPO34 and 280mg are filled, 0.3cm of quartz wool is filled on a catalyst, the upper end and the lower end of the 316 stainless steel pipe are sealed by using a 316 stainless steel front and rear sleeve, the 316 stainless steel front and rear sleeve are connected with an air inlet pipe and an air outlet pipe, a back pressure valve is arranged behind an air outlet, and the back pressure valve is also connected with a gas chromatography for product. And installing an open-hearth tube furnace in the middle constant-diameter area of the 316 stainless steel tube, and ensuring that the constant-temperature section of the tube furnace corresponds to the inert lining catalyst filling area.
Using feed gas composition: 5% Ar (internal standard), CO: 47.5%, H2: 47.5 percent; the pressure of the reaction tube is increased by 4Mpa, and the temperature is increased by 400 ℃ after leak detection, and the gas flow is 24sccm
CO conversion 20%, CO2 selectivity 37% C
Hydrocarbon distribution: methane 22%, ethylene-butene 63%, others 15%.
Example 2 and comparative example 1 demonstrate that stainless steel tubes have the ability to catalyze the conversion of syngas under the syngas reaction conditions, as well as the formation of metal carbonyls, resulting in the formation of large amounts of methane under the reaction conditions. If the reactor of the invention is used, the possibility of the reaction of the tube wall can be greatly reduced, and the interference of the reactor to the reaction can be even completely avoided.
Claims (9)
1. The utility model provides a reactor of self-balancing inside and outside pressure of bushing pipe which characterized in that: the pressure-bearing device comprises a hollow cylindrical pressure-bearing shell with two open ends and a hollow cylindrical inert lining with two open ends, wherein the inert lining is sleeved in the pressure-bearing shell in a penetrating way, a gap is reserved between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, an annular lining inlet sealing ring and an annular lining outlet sealing ring are sleeved on the outer wall surface of the inert lining, the two ends of the gap between the lining inlet sealing ring and the lining outlet sealing ring are sealed, and a sealed crack is formed between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing; two open ends of the inert lining are respectively used as a reaction material inlet and a reaction material outlet; one end of the conduit with two open ends is communicated with the closed crack, the other end is positioned at the inlet end of the inert lining, the conduit is provided with a pressure balance valve, and the pressure balance valve is a one-way valve which allows gas to flow from the inlet end to the crack; one end of the other conduit with two open ends is communicated with the closed crack, the other end of the conduit is positioned at the outlet end of the inert lining, the conduit is provided with a self-protection pressure release valve, and the self-protection pressure release valve is a one-way valve which only allows gas to flow from the crack to the outlet end;
the inert lining is positioned in the pressure-bearing shell, and the inlet end and the outlet end of the inert lining are sealed with the pressure-bearing shell through annular sealing rings; a crack is formed between the pressure-bearing shell and the inert lining, the pressure balance valve is connected between an air inlet at the inlet end of the inert lining and the crack through a pipeline, and the air flow direction of the pressure balance valve only allows the air flow from the air inlet to the crack; the self-protection pressure release valve is connected with the crack and a tail gas outlet at the outlet end of the inert lining through a pipeline, and the gas flow direction is only allowed to flow from the crack to the tail gas outlet; in a stable pressure state, the gas only flows through the inner lining pipe and cannot flow through the crack.
2. The reactor of claim 1, wherein: the upper end and the lower end of the pressure-bearing shell are respectively hermetically connected with the air inlet pipe and the air outlet pipe, and the joint of the upper end of the pressure-bearing shell and the air inlet pipe or the joint of the lower end of the pressure-bearing shell and the air outlet pipe can be opened and closed for sealing, so that the inert lining can be taken and placed.
3. The reactor of claim 1, wherein:
the pressure-bearing shell is a circular tube, two cylindrical screw caps with external threads are sleeved on the outer wall surface of the circular tube, an annular boss A is radially arranged on the outer wall surface of the two opening ends of the pressure-bearing shell respectively, the inner diameter of each screw cap is smaller than the outer diameter of the annular boss A, an annular boss B is radially arranged on the outer wall of the connecting end of the air inlet pipe and the air outlet pipe with the pressure-bearing shell respectively, two cylindrical press covers with internal threads are arranged at the upper ends of the lower end openings of the two internal threads in a sealing mode, through holes are formed in the middle of the sealing ends of the press covers, the air inlet pipe and the air outlet pipe are sleeved in the through holes of the two press covers respectively, the inner diameter of each through hole is smaller than.
4. A reactor according to any one of claims 1 to 3, wherein: the inner wall surfaces of the two opening ends of the pressure-bearing shell are respectively provided with an annular sunken part which is coaxial with the pressure-bearing shell and is provided with an internal thread, the pressure-bearing shell and the inert lining are respectively a round pipe, the inert lining is coaxially sleeved in the pressure-bearing shell, a lining inlet sealing ring and a lining outlet sealing ring are arranged in the annular sunken parts, two pressure caps with through holes in the middle of the external thread are respectively screwed in the annular sunken parts at the two ends of the pressure-bearing shell, and the two ends of the inert lining are respectively sleeved in the through holes of the two pressure caps; a gap is left between the outer wall surface of the inert lining and the inner wall surface of the pressure-bearing shell, and a lining inlet sealing ring and a lining outlet sealing ring are arranged on the inner wall surface of the inert lining.
5. The reactor of claim 4, wherein: a catalyst or a sample to be detected is placed in the inert lining, the area for placing the catalyst or the sample to be detected is used as a reaction furnace, the lining inlet sealing ring and the lining outlet sealing ring are positioned at two ends of the reaction furnace or are far away from the area outside the two ends of the reaction furnace, the environmental temperature is ensured to be lower than 200 ℃, and the sealing ring is made of one or two of rubber, tetrafluoroethylene, graphite and silica gel;
the pressure-bearing shell is made of high-temperature and high-pressure resistant materials, bears external pressure and resists pressure of 13Mpa below 600 ℃;
the inert lining tube material is one or more than two of quartz, corundum, silicon carbide, titanium oxide and zirconium oxide.
6. The reactor of claim 1, wherein: a crack is formed between the pressure-bearing shell and the inert lining; and the starting pressure of the pressure balance valve and the self-protection pressure relief valve is less than 3 atmospheres.
7. Use of a reactor according to any of claims 1-6, characterized in that:
when in use, the upper end or the lower end of the reaction tube is opened, the inert lining is taken out, and a sample to be measured or a catalyst is filled after cleaning; installing the inert lining inside the pressure-bearing shell, sealing the upper end and the lower end of the inert lining with the pressure-bearing shell through a sealing ring, sealing the upper end of the reaction tube, and respectively connecting the upper end and the lower end of the pressure-bearing shell with an air inlet pipe and an air outlet pipe; when a high-pressure experiment is carried out, a back pressure valve needs to be installed behind the air outlet, and the outlet end of the self-protection pressure release valve is connected between the air outlet and the back pressure valve.
8. Use according to claim 7, characterized in that: if corrosive components exist in the raw material atmosphere, the pressure inside and outside of the inert lining in the pressure-bearing shell needs to be increased in the non-corrosive atmosphere, the inert lining is switched into reaction raw material gas after the pressure is stable, and the gas in the inert lining is purged and replaced under the same pressure;
if the pressure needs to be increased in the process of the experiment, the pressure needs to be increased in the inert atmosphere, and then the reaction atmosphere is switched to purge and replace the atmosphere in the inert lining.
9. Use according to claim 7 or 8, characterized in that: if the pressure needs to be reduced in the experimental process, the pressure needs to be firstly released to 2 atmospheric pressures below the target pressure, and then the pressure needs to be increased to the target pressure after the pressure is stabilized, so that the test is carried out.
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CN109358079B (en) * | 2018-11-06 | 2023-10-27 | 广州海洋地质调查局 | Device and method for measuring sea area argillaceous silt reservoir structure change by combining CT technology |
CN112705149B (en) * | 2019-10-25 | 2022-10-21 | 中国石油化工股份有限公司 | Quartz reactor with liner |
CN111530376B (en) * | 2020-05-11 | 2022-05-10 | 中国科学院工程热物理研究所 | High-pressure chemical reaction device with pressure balance system |
CN112958006B (en) * | 2021-03-15 | 2022-04-29 | 北京科技大学 | Thick-wall hydrothermal high-pressure kettle and use method thereof |
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