Catalyst quantitative carbon supplementing device applied to methanol-to-olefin micro-reaction device

Abstract

The utility model discloses a catalyst quantitative carbon supplementing device applied to a methanol-to-olefin micro-reaction device, and belongs to the technical field of catalysts. The device is composed of a first needle valve, a first glass rotameter, a first one-way valve, a gas mixing tank, a second one-way valve, a second glass rotameter, a vaporization buffer tank, a second needle valve, a liquid steel cylinder, a third one-way valve and a stop valve. According to the device, C4 components are diluted through nitrogen, so that a proper amount of C4 components are subjected to cracking and chemical bonding with a catalyst at a certain temperature, and the quantitative carbon supplementing effect of the catalyst is further realized; the carbon supplementing device disclosed by the utility model is simple in composition, low in preparation cost, simple in operation process, capable of rapidly realizing quantitative carbon supplementing of the catalyst, and good in repeatability of quantitative carbon supplementing of the catalyst. The device is a supplement for a methanol-to-olefin micro-reaction device, can realize rapid and accurate preparation and repeated verification of catalysts with different carbon contents, and helps to solve the research work of the influence of the carbon contents on the performance of the catalyst.

Description

Technical Field

[0001] The utility model belongs to the technical field of catalysts, and in particular relates to a catalyst quantitative carbon replenishing device applied to a methanol to olefin micro-reaction device. Background Art

[0002] After running for a period of time in an industrial reactor, the methanol to olefins catalyst will be deactivated due to excessive carbon deposition. The deactivated catalyst needs to be further regenerated and carbonized before it can be reloaded into the reactor for reuse. Due to the complexity of industrial production, the characteristics of each batch of deactivated catalysts are different. After the deactivated catalyst is regenerated, different amounts of carbon four components (i.e. carbonization) need to be added to optimize the performance of the catalyst, thereby maximizing the production capacity of industrial products. The methanol to olefins fixed fluidized bed microreactor is an important equipment for laboratory evaluation of industrial catalysts. It has fast testing and low energy consumption, and can provide detailed data support for the improvement of the performance of industrial catalysts in enterprises. Through the methanol to olefins fixed fluidized bed microreactor, the optimal carbonization amount of industrial catalysts can be studied at the lowest cost, thereby assisting production to improve the performance of industrial catalysts and increase the output of industrial products. However, there is currently no report on a quantitative carbonization device suitable for the methanol to olefins microreactor, so it is impossible to accurately calculate the optimal carbonization amount of industrial catalysts. Utility Model Content

[0003] The utility model aims to provide a catalyst quantitative carbon replenishment device used in a methanol to olefins micro-reactor, and its advantages are: first, the device is simple in design and convenient to connect, and complete vaporization of C4 liquid components and dilution of C4 gas components are achieved through a vaporization buffer tank and a gas mixing tube, thereby achieving different quantitative carbon replenishment of the catalyst; second, the device has strong operability and good experimental repeatability, and can achieve quantitative carbon replenishment of the catalyst quickly and safely.

[0004] like Figure 1 As shown; the utility model describes a catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor, which is composed of a first needle valve 1, a first glass rotor flowmeter 2, a first non-return valve 3, a gas mixing tank 4, a second non-return valve 5, a second glass rotor flowmeter 6, a vaporization buffer tank 7, a second needle valve 8, a liquid cylinder 9, a third non-return valve 10 and a stop valve 11 connected by a stainless steel pipeline (diameter 3-5 mm); a C4 liquid component feed port and a C4 gas component outlet are respectively arranged at the lower part and the upper part of the side wall of the vaporization buffer tank 7; a C4 component inlet and a nitrogen inlet are respectively arranged at the lower part of the side wall of the gas mixing tank 4, and a mixed gas outlet is arranged at the upper part of the side wall of the gas mixing tank 4.

[0005] When the carbon replenishing device is in operation, the first needle valve 1 and the stop valve 11 are opened, and the nitrogen from the nitrogen storage tank 15 enters the gas mixing tank 4 through the first needle valve 1, the first glass rotor flowmeter 2, the first non-return valve 3 and the nitrogen inlet, and then enters the reactor of the methanol to olefins micro-reactor through the mixed gas outlet, the third non-return valve 10 and the stop valve 11 to activate the catalyst; after the catalyst activation is completed, the second needle valve 8 is opened, and the C4 liquid component in the liquid cylinder 9 enters the vaporization buffer tank 7 through the second needle valve 8 and the C4 liquid component feed port under its own pressure, and is quickly vaporized at room temperature. The vaporized C4 component enters the gas mixing tank 4 through the C4 gas component outlet, the second glass rotor flowmeter 6, and the second non-return valve 5 to mix with the nitrogen, and then enters the reactor of the methanol to olefins micro-reactor through the mixed gas outlet, the third non-return valve 10 and the stop valve 11, and cracks and chemically bonds with the catalyst, thereby realizing quantitative carbon replenishment of the catalyst.

[0006] Furthermore, the first needle valve 1 and the second needle valve 8, the first one-way valve 3, the second one-way valve 5 and the third one-way valve 10 and the stop valve 11 are well-known and commonly used equipment in the market, and are made of 316L stainless steel.

[0007] Furthermore, the liquid cylinder 9 has a capacity of 300-350 mL and is made of 316L stainless steel with a maximum pressure resistance of 20 MPa. It uses industrially known and commonly used equipment to store C4 liquid components; the C4 liquid components are obtained from an external production device, and the main components are butene, butane, isobutylene and isobutane.

[0008] Furthermore, the vaporization buffer tank 7 and the gas mixing tank 4 are of the same cylindrical structure, made of 316L stainless steel, with a wall thickness of 2 to 4 mm, a height of 200 to 240 mm, and a bottom radius of 50 to 70 mm.

[0009] Furthermore, the maximum working pressure of the first glass rotor flowmeter 2 and the second glass rotor flowmeter 6 is 1.0 MPa, the measuring range is 0-500 mL / min, and industrially known and commonly used equipment is adopted.

[0010] The methanol to olefins micro-reactor of the utility model is composed of a vaporizer 13, a reactor 12 and a gas chromatograph 14. The system operation process is as follows: after the catalyst is loaded into the reactor 12, nitrogen is introduced to activate it at a certain temperature, and then liquid methanol is converted into gaseous methanol through the vaporizer 13 and enters the reactor 12 to react with the catalyst, and the gas product after the reaction enters the gas chromatograph 14 for qualitative and quantitative analysis.

[0011] The catalyst quantitative carbon replenishment device is a supplement to the methanol to olefins micro-reactor. It can realize the rapid and accurate preparation and repeated verification of catalysts with different carbon contents, and help solve the research work on the influence of carbon content on catalyst performance. The operation process of the catalyst quantitative carbon replenishment is as follows: weigh the industrial catalyst (the industrial catalyst is SAPO-34 molecular sieve, and the effective ingredient is silicon aluminum compound) and load it into the reactor of the methanol to olefins micro-reactor. Open the first needle valve 1, the first glass rotor flowmeter 2 and the stop valve 11. Nitrogen first enters the reactor 12 through the first needle valve 1, the first glass rotor flowmeter 2, the first one-way valve 3, the gas mixing tank 4, the third one-way valve 10, and the stop valve 11 at a flow rate of 40 to 60 mL / min (the flow rate is adjusted by the first glass rotor flowmeter 2); the reactor 12 is programmed to heat up and the catalyst is activated; when the reactor 12 is heated to 450 to 550°C, the second needle valve 8 and the second glass rotor flowmeter 6 are opened, and the liquid steel The C4 liquid component in the bottle 9 enters the vaporization buffer tank 7 through the second needle valve 8 under its own pressure and is quickly vaporized. The vaporized C4 gas component enters the gas mixing tank 4 through the second glass rotor flowmeter 6 and the second one-way valve 5 at a flow rate of 20 to 50 mL / min (the flow rate is adjusted by the second glass rotor flowmeter 6) and is mixed with nitrogen at a flow rate of 300 to 500 mL / min (the nitrogen flow rate is adjusted by the second glass rotor flowmeter 6). The mixed gas enters the reactor 12 and reacts with the catalyst to replenish carbon. A small amount of the catalyst after replenishing carbon is taken out for thermogravimetric analysis to test the carbon content, and the remaining catalyst is evaluated for catalytic performance according to the operating process of the methanol to olefins micro-reactor (the gas chromatograph 14 is an instrument for analyzing the content of the product generated after the reaction).

[0012] The beneficial effects of the catalyst quantitative carbon replenishment device involved in the utility model include: (1) by diluting the C4 component with nitrogen, an appropriate amount of C4 component is prompted to undergo cracking and chemical bonding with the catalyst at a certain temperature, thereby achieving the catalyst quantitative carbon replenishment effect; (2) the carbon replenishment device has a simple composition, low preparation cost, and simple operation process, and can quickly achieve the catalyst quantitative carbon replenishment, and the catalyst quantitative carbon replenishment has good repeatability. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] In order to more clearly illustrate the utility model patent, the utility model patent is introduced in detail through embodiments. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, it is difficult to obtain the process parameters of the carbon replenishing device in the drawings without creative work.

[0014] Figure 1 It is a schematic diagram of the structure of a methanol to olefins micro-reactor including a carbon feeding device;

[0015] Figure 2It is a schematic diagram of the structure of the vaporization buffer tank and the gas mixing tank. DETAILED DESCRIPTION

[0016] Example 1

[0017] This example is an experiment of using a carbon replenishing device to perform quantitative carbon replenishment on an industrial catalyst. The industrial catalyst is obtained from an external production device and has a carbon content of 1.3 wt%.

[0018] The carbon replenishing device includes a first needle valve 1, a first glass rotor flowmeter 2, a first non-return valve 3, a gas mixing tank 4, a second non-return valve 5, a second glass rotor flowmeter 6, a vaporization buffer tank 7, a second needle valve 8, a liquid cylinder 9, a third non-return valve 10 and a stop valve 11; the liquid cylinder has a capacity of 300 mL, is made of 316L stainless steel, and has a maximum pressure resistance of 20 MPa, and is used to store C4 liquid components obtained from an external production device, and the C4 components are composed of butene, butane, isobutylene, and isobutane; the vaporization buffer tank 7 and the gas mixing tank 4 have the same cylindrical structure, are made of 316L stainless steel, have a wall thickness of 2 mm, a height of 220 mm, and a bottom radius of 50 mm; the glass rotor flowmeter has a maximum working pressure of 1.0 MPa and a range of 0 to 500 mL / min.

[0019] The operation process of quantitative carbon replenishment of the catalyst is as follows: 7.6g of industrial catalyst is weighed and loaded into the reactor 12, the first needle valve 1, the first glass rotor flowmeter 2, and the stop valve 11 are opened, and the nitrogen flow rate at the outlet of the first glass rotor flowmeter 2 is adjusted to 60mL / min, and the nitrogen enters the reactor 12 through the gas mixing tank 4; the reactor 12 is programmed to heat up in order to activate the catalyst; after the reactor 12 is heated to 500°C, the second needle valve 8 and the second glass rotor flowmeter 6 are opened, and the C4 liquid component in the liquid cylinder 9 enters the vaporization buffer tank 7 through the second needle valve 8 under its own pressure and is quickly vaporized. The vaporized C4 component enters the gas mixing tank 4 at a flow rate of 20 mL / min through the second glass rotor flowmeter 6 and the second one-way valve 5 to be mixed with nitrogen (the outlet flow rate of the first glass rotor flowmeter 2 is adjusted to 300 mL / min), and the mixed gas enters the reactor through the third one-way valve 10 and the stop valve 11 to react with the catalyst for carbon replenishment. After carbon replenishment for 5 minutes, the temperature control system of the device and the second glass rotor flowmeter 6 are closed, and the catalyst is purged with nitrogen. After the reactor is cooled to room temperature, 0.1 g of the catalyst is taken out and the carbon content is tested by a thermogravimetric analyzer, and the catalytic performance of the remaining catalyst is evaluated according to the operating process of the methanol to olefins micro-reactor.

[0020] Three parallel experiments were carried out according to the above method. The catalyst carbon contents (catalyst carbon content refers to the content of organic matter adsorbed on the catalyst, tested by thermogravimetric analyzer) obtained in the three experiments were 1.80wt%, 1.77wt% and 1.82wt%, respectively. The results showed that the carbon replenishment device can achieve quantitative carbon replenishment of industrial catalysts with good repeatability.

[0021] Example 2

[0022] This example is an experiment of using a carbon replenishing device to carry out quantitative carbon replenishment on an industrial catalyst. The industrial catalyst is obtained from a production device and has a carbon content of 1.3 wt%.

[0023] The carbon replenishing device includes a first needle valve 1, a first glass rotor flowmeter 2, a first non-return valve 3, a gas mixing tank 4, a second non-return valve 5, a second glass rotor flowmeter 6, a vaporization buffer tank 7, a second needle valve 8, a liquid cylinder 9, a third non-return valve 10, a stop valve 11 and other equipment; the liquid cylinder has a capacity of 300mL, is made of 316L stainless steel, and has a maximum pressure resistance of 20MPa, and is used to store C4 liquid components obtained from production. The C4 component consists of butene, butane, isobutylene, and isobutane; the vaporization buffer tank and the gas mixing tank have the same cylindrical structure, are made of 316L stainless steel, have a wall thickness of 2mm, a height of 210mm, and a bottom radius of 60mm; the maximum working pressure of the glass rotor flowmeter is 1.0MPa, and the range is 0-500mL / min.

[0024] The catalyst recarbonization operation process is as follows: weigh 7.6g of industrial catalyst and load it into the reactor, open the first needle valve 1, the first glass rotor flowmeter 2, and the stop valve 11, adjust the nitrogen flow rate at the outlet of the first glass rotor flowmeter 2 to 50mL / min, and the nitrogen enters the reactor 12 through the gas mixing tank 4, and the reactor 12 is programmed to be heated to activate the catalyst; after the reactor 12 is heated to 550°C, open the second needle valve 8 and the second glass rotor flowmeter 6, and the C4 liquid component in the liquid cylinder 9 enters the vaporization buffer tank 7 through the second needle valve 8 under its own pressure and is quickly vaporized. The C4 component is mixed with nitrogen by entering the gas mixing tank 4 at 50 mL / min through the second glass rotor flowmeter 6 and the second one-way valve 5 (the outlet flow rate of the first glass rotor flowmeter 2 is adjusted to 300 mL / min). The mixed gas enters the reactor through the third one-way valve 10 and the stop valve 11 to react with the catalyst for carbon replenishment. After carbon replenishment for 5 minutes, the temperature control system of the device and the second glass rotor flowmeter 6 are closed, and the catalyst is purged with nitrogen. After the reactor is cooled to room temperature, 0.1 g of the catalyst is taken out and the carbon content is tested by thermogravimetric analyzer. The catalytic performance of the remaining catalyst is evaluated according to the operation process of the methanol to olefins micro-reactor.

[0025] Three parallel experiments were carried out according to the above method. The catalyst carbon contents (catalyst carbon content refers to the content of organic matter adsorbed on the catalyst, tested by thermogravimetric analyzer) obtained in the three experiments were 2.20wt%, 2.23wt% and 2.21wt%, respectively. The results showed that the carbon replenishment device can achieve quantitative carbon replenishment of industrial catalysts with good repeatability.

[0026] Anything not described in detail in this utility model is a conventional technical means known to those skilled in the art. The above description is only a preferred embodiment of this utility model and is not intended to limit this utility model. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this utility model shall be included in the protection scope of this utility model.

Claims

1. A catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor, characterized by: The invention is composed of a first needle valve (1), a first glass rotor flowmeter (2), a first non-return valve (3), a gas mixing tank (4), a second non-return valve (5), a second glass rotor flowmeter (6), a vaporization buffer tank (7), a second needle valve (8), a liquid cylinder (9), a third non-return valve (10) and a stop valve (11) connected by a stainless steel pipeline; a C4 liquid component feed port and a C4 gas component gas outlet are respectively arranged at the lower part and the upper part of the side wall of the vaporization buffer tank (7). A C4 component gas inlet and a nitrogen gas inlet are respectively provided at the lower part of the side wall of the gas mixing tank (4), and a mixed gas outlet is provided at the upper part of the side wall of the gas mixing tank (4); when the carbon replenishing device is in operation, the first needle valve (1), the first glass rotor flowmeter (2) and the stop valve (11) are opened, and the nitrogen from the nitrogen storage tank (15) enters the gas mixing tank (4) through the first needle valve (1), the first glass rotor flowmeter (2), the first check valve (3) and the nitrogen inlet, and then After passing through the mixed gas outlet, the third one-way valve (10) and the stop valve (11), the gas enters the reactor (12) of the methanol to olefins microreactor at a flow rate of 40 to 60 mL / min to activate the catalyst; after the catalyst activation is completed, the second needle valve (8) and the second glass rotor flowmeter (6) are opened, and the C4 liquid component in the liquid cylinder (9) enters the vaporization buffer tank (7) through the second needle valve (8) and the C4 liquid component feed port under its own pressure to be vaporized; the vaporized C4 component enters the gas mixing tank (4) through the C4 gas component outlet, the second glass rotor flowmeter (6) and the second one-way valve (5) at a flow rate of 20 to 50 mL / min to be mixed with nitrogen at a flow rate of 300 to 500 mL / min, and then enters the reactor of the methanol to olefins microreactor through the mixed gas outlet, the third one-way valve (10) and the stop valve (11), and undergoes cracking and chemical bonding with the catalyst, thereby achieving quantitative carbon replenishment of the catalyst.

2. A catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor according to claim 1, characterized in that: The first needle valve (1), the second needle valve (8), the first one-way valve (3), the second one-way valve (5), the third one-way valve (10) and the stop valve (11) are made of 316L stainless steel.

3. A catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor according to claim 1, characterized in that: The capacity of the liquid cylinder (9) is 300-350 mL, the material is 316L stainless steel, and the maximum pressure resistance is 20 MPa.

4. A catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor according to claim 1, characterized in that: The vaporization buffer tank (7) and the gas mixing tank (4) are of the same cylindrical structure, made of 316L stainless steel, with a wall thickness of 2 to 4 mm, a height of 200 to 240 mm, and a bottom radius of 50 to 70 mm.

5. The catalyst quantitative carbon replenishing device used in a methanol to olefins micro-reactor according to claim 1, characterized in that: The maximum working pressure of the first glass rotor flowmeter (2) and the second glass rotor flowmeter (6) is 1.0 MPa, and the measuring range is 0 to 500 mL / min.

Images