CN208921669U - Sulfur-resistant transformation catalyst mesohigh activity assay device - Google Patents

Sulfur-resistant transformation catalyst mesohigh activity assay device Download PDF

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Publication number
CN208921669U
CN208921669U CN201821457383.5U CN201821457383U CN208921669U CN 208921669 U CN208921669 U CN 208921669U CN 201821457383 U CN201821457383 U CN 201821457383U CN 208921669 U CN208921669 U CN 208921669U
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China
Prior art keywords
sulfur
mesohigh
activity assay
assay device
transformation catalyst
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CN201821457383.5U
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钟立宏
史志刚
陆建国
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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Abstract

The utility model relates to sulfur-resistant transformation catalyst mesohigh activity assay device, main includes unstripped gas air admission unit, gas flow and temperature control unit, vulcanization unit, reaction member, product separative unit and the component analysis unit successively coupled.The control condition that utility model device simulates industrial sulphur-resistant conversion production technology is designed, and the degree of automation is higher, so that inspection data is with more scientific, accuracy.Two reactors can once detect two samples simultaneously, and the collimation of device and repdocutbility are preferable, greatly improve working efficiency.

Description

Sulfur-resistant transformation catalyst mesohigh activity assay device
Technical field
The utility model relates to the activity assay device of sulfur-resistant transformation catalyst mesohigh, which is mainly used in resistant to sulfur Activity assay and performance evaluation of the transformation catalyst under the conditions of mesohigh.
Background technique
Widely used mesohigh sulfur-resistant transformation catalyst is using cobalt molybdenum as main active component both at home and abroad at present, magnalium point Spar is carrier, and suitable auxiliary agent is added, is prepared using Particular craft.Its specific surface area with higher, lower heap density And the physical properties such as suitable pore size distribution, the catalyst for making carrier with it have the warm active region of excellent width, especially low temperature is living Property is good.Therefore it can not only make low change use in low in the and low process of middle string, and Fe-Cr can be replaced in total-low process High conversion catalyst makees hts catalyst use.To obtain significant economic benefit.Therefore this kind of catalyst is widely used Synthesis ammonia and methanol production enterprise in different scales.Many units are dedicated to the research of sulfur-resistant transformation catalyst, technology with It is continued to introduce new on product, develops premium quality product.Co-Mo system sulfur-resistant transformation catalyst is using its preceding active component with oxygen Change state (CoO and MoO) form to exist, activity is lower, needs to carry out the presulfurization of catalyst before normal process production, to obtain sulphur Change catalyst activity composition (CoS and MoS) such catalyst and technology industrially extensive utilization of state.Existing various big rule Mould industrial production equipment, its main feature is that reactor is big, loaded catalyst is big, catalyst service life is longer, each manufacturing enterprise The technology of offer serves primarily in industrial application.Lack the activity assay device for applying to evaluate catalyst activity superiority and inferiority, to visitor Arbitration of the family when selecting product, mode of examining goods and quality dispute occurring all causes certain difficulty.
Summary of the invention
The utility model mainly solves the problems, such as it is sulfur-resistant transformation catalyst activity performance superior and inferior evaluating under the conditions of mesohigh, A kind of small-sized sulfur-resistant transformation catalyst mesohigh activity assay device is provided, by simulating sulphur-resistant conversion industrial flow, is controlled resistance to The test conditions such as temperature, pressure, the air speed of sulphur conversion process, to obtain catalyst activity inspection data.Reaction unit tool Have the advantages that small in size, unstripped gas consumption is low, loaded catalyst is few and easy to loading and unloading, unique single tube reactor designs energy Each reaction tube temperature is effectively ensured, pressure, is consistent, two reactors can once detect two samples simultaneously, and guarantee dress The collimation and repdocutbility set, it is biggish to improve work efficiency, reduce the waste of cost of labor and unstripped gas.
The technical solution of the utility model: sulfur-resistant transformation catalyst mesohigh activity assay device, it is characterised in that: The device include unstripped gas air admission unit, gas flow and the temperature control unit successively coupled, vulcanization unit, reaction member, Product separative unit and component analysis unit.Mainly by high pressure tank, mass flowmenter, vulcanizing tank, caustic treater, mixer, Reactor, condenser, condensing collector, gas-chromatography composition.
Generally, the unstripped gas air admission unit includes high pressure tank and pressure maintaining valve, and high pressure tank volume is 0.4~ 0.6m3, pressure be 15~20MPa.
The gas flow rate control unit includes mass flowmenter, mass flowmenter range be 0~100mL/min, 0~ 3000mL/min, control precision are 0.1 grade.
The temperature control unit includes temperature control instrument and DCS system, and temperature control precision is 0.5 DEG C of 0.5~﹢ of ﹣.
The vulcanization unit includes vulcanizing tank, vulcanizing tank calandria, caustic treater, and vulcanizing tank calandria is added using water-bath circulation Hot mode, heating temperature are 0~90 DEG C.
The reaction member includes being examined simultaneously using the mixer and single tube reactor of pressure resistance, corrosion-resistant stainless steel material Test two catalyst samples.
The reaction tube of the single tube reactor having a size of 44 × 6mm, reaction pressure is 0~10MPa, reaction temperature be 0~ It 550 DEG C, is threadedly coupled using soft seal.
The product separative unit includes cooling water circulation machine, condenser, condensing collector, and cooling water temperature can be adjusted to Minimum subzero 10 DEG C.
The component analysis unit includes gas chromatograph and carry gas cleanser, is reacted front and back gas using TCS thermal conductivity The analysis of the volume fraction of carbon monoxide in body.
Utility model device core is reactor, mainly includes thermocouple sheath, reaction tube, catalyst filling zone, resistance to Press heat storage, insulating layer and reactor outer wall, reactor using temperature is 0~550 DEG C, pressure is 0~10Mpa;Reaction tube is Reactor core component, sealing are attached in the form of soft seal by nut using graphite pads;Temperature thermocouple sleeve Positioned at reaction tube centre, interpolation thermocouple;Reactor is heated by electric heating body, and electric heating body is by heating cylinder and heating Element composition carries out temperature programmed control to reactor by temperature control system;Insulating layer is located at heating cylinder and reactor outer wall Between, the high-temperature-resistant thermal-insulation material of filling stablizes temperature of reactor control, it is ensured that sulfur-tolerant water gas shift steadily carries out;Reaction Device outer wall is stainless steel material, is fixed on activity assay device frame by metallic support.
Reactor provides unstrpped gas and is preheated, reacts use in above-mentioned apparatus, because it is in high temperature, high pressure and high steam Under the conditions of, and therefore the corrosion containing carbon monoxide, carbon dioxide, hydrogen need to select corrosion-resistant, heat-resisting, high-intensitive special type Steel alloy;Skin temperature is lower, and corrosivity is few, and the common stainless steel of general material can be used, and nut preferably uses hardness higher Chrome-molybdenum steel.
Above-mentioned reactor inlet connects mixer, the condenser of lower end outlet connection verifying attachment, condensate collector and Analysis system, reaction tube are sealed in the form of soft seal by nut.
Above-mentioned reaction tube upper and lower ends fill silica magnetic ball, and medium position loads sulfur-resistant transformation catalyst, silica magnetic Ball is separated by the sieve plate with hole with catalyst, so that unstripped gas air-flow carries out therewith evenly into catalyst bed Reaction.
Above-mentioned reaction tube is 0~550 DEG C using temperature, pressure is 0~10MP, all using alloy having a size of 44 × 6mm Pipe connection.
Above-mentioned electric heating body is made of heating cylinder and heating element, is carried out by DCS temperature control system to reactor Temperature programmed control.
Above-mentioned insulation layer thickness is 5~15cm, fills high-temperature-resistant thermal-insulation material.
Core reaction pipe built in outer shell is appealed, electric heating body, thermal insulation material by metallic support and are fixed on activity On verifying attachment frame.
The technological merit of the utility model are as follows:
1, activity assay device is rationally distributed, clear in structure, easy to operate, has preferable stability.
2, activity assay device all uses stainless steel tubing to connect, good seal performance.Temperature carries out essence using DCS system Quasi- control is, it can be achieved that control temperature ± 0.5 DEG C.
3, the air speed of unstripped gas and reaction temperature control range are big, and accuracy is high, are conducive to the repdocutbility of catalyst sample, So that inspection data is with more science.
4, reaction tube uses stainless steel material, conducts heat, and is more advantageous to reaction inner axial tube equalized temperature.
5, the Heat preservation of vulcanizing tank and vaporizer all uses water-cycling mode, it is ensured that the stability of heating and uniformly Property.
6, it is unique design so that in set of device install two reactors, can once simultaneously detect two samples.And energy Temperature between reaction tube is enough effectively ensured, pressure is consistent, the timeliness for sulfur-resistant transformation catalyst sample survey provides Guarantee, also significantly improves work efficiency.
Detailed description of the invention
Fig. 1 is the utility model embodiment activity assay schematic device.
In figure: 1, pressure storage tank;2-1~2-2, pressure maintaining valve;3-1~3-4, flowmeter;4-1~4-2, vulcanizing tank;5-1~ 5-2, mixer;6-1~6-2, head tank;7-1~7-2, constant-flux pump;8-1~8-2, vaporizer;9-1~9-2, reactor; 10-1~10-2 condenser;11-1~11-2 condensate collector;12-1~12-2 caustic treater;13 gas chromatographs.
Specific embodiment
The utility model is described further below with reference to embodiment and attached drawing.
Embodiment
Sulfur-resistant transformation catalyst mesohigh activity assay device referring to attached drawing 1, it is main comprising the unstripped gas that successively couples into Gas unit, gas flow and temperature control unit, vulcanization unit, reaction member, product separative unit, component analysis unit.It is main It will be by pressure storage tank (1), pressure maintaining valve (2-1~2-2), flowmeter (3-1~3-4), vulcanizing tank (4-1~4-2), mixer (5- 1~5-2), head tank (6-1~6-2), constant-flux pump (7-1~7-2), vaporizer (8-1~8-2), reactor (9-1~9-2), Condenser (10-1~10-2), condensate collector (11-1~11-2), caustic treater (12-1~12-2), gas chromatograph (13) Deng composition.
In general, high pressure tank volume is 0.4~0.6m3, pressure be 15~20MPa;Mass flowmenter range be 0~ 100mL/min, 0~3000mL/min, control precision are 0.1 grade;Temperature control control precision is 0.5 DEG C of 0.5~﹢ of ﹣;Vulcanizing tank Calandria uses water-bath circulating-heating mode, and heating temperature is 0~90 DEG C;Reaction member includes using pressure-resistant, corrosion-resistant stainless The mixer and single tube reactor of steel material, while examining two catalyst samples;The reaction tube of single tube reactor is having a size of 44 × 6mm, reaction pressure are 0~10MPa, reaction temperature is 0~550 DEG C, are threadedly coupled using soft seal;Cooling water temperature is adjustable Save minimum subzero 10 DEG C;Component analysis unit includes gas chromatograph and carry gas cleanser, before being reacted using TCS thermal conductivity Afterwards in gas the volume fraction of carbon monoxide analysis.
By pressure storage tank (1) Lai gas control certain sky through pressure maintaining valve (2-2), through mass flowmenter (3-2,3-4) Enter reactor (9-1,9-2) after speed, reactor (9-1,9-2) carries out elevated temperature cure by pre-set program segment.Vulcanization Tail gas is through condenser (10-1,10-2), condensate collector (11-1~11-2) and caustic treater (12-1,12-2) alkali cleaning, warp Tail gas after crossing alkali cleaning is vented.
After vulcanization, system boosting, the unstripped gas from pressure storage tank (1) is through pressure maintaining valve (2-2), mass flow at this time It counts after (3-1,3-3) controls certain air speed and enters mixer (5-1,5-2), come from raw material with by constant-flux pump (7-1,7-2) The raw material of tank (6-1,6-2) is mixed, and mixed gas enters reactor (9-1,9-2) under certain temperature and pressure It is reacted.Air-liquid mixture after reaction enters condenser (10-1,10-2), condensate collector (11-1,11-2).It is cold Tail gas and unstripped gas after solidifying calculates one oxidation through the carbon monoxide volume fraction in gas chromatograph (13) analysis gas Efficiency of carbon con version.
The core component of above-mentioned activity assay device is reactor, by reaction tube and accumulation of heat shell, electric heater, thermal insulating material Material composition.Reaction tube is located in the middle part of reactor, and built-in thermocouple casing, tube length of reaction tube is about 500mm, in reaction tube when filling sample One layer of stainless steel sieve is padded in bottom, will handle the porcelain ball that clean granularity is 3~¢ of ¢ 5mm and is packed into reaction tube, and strike reality, fills out Identified position when to measurement isothermal region.Add one layer of stainless steel sieve on porcelain ball again, the catalyst handled well is carefully fallen Enter in reaction tube, gently tap tube wall, keep catalyst bed filling close, and measure its catalyst bed filling height, then In addition one layer of stainless steel sieve, it is packed into the porcelain ball of appropriate granularity in stainless steel sieve, gently strikes reality, reactor spiral shell is tightened after filling Reactor access pilot system is carried out leak test, after leak test meets the requirements, can carry out activity assay by cap.

Claims (9)

1. sulfur-resistant transformation catalyst mesohigh activity assay device, it is characterised in that: the device includes the unstripped gas successively coupled Air admission unit, gas flow and temperature control unit, vulcanization unit, reaction member, product separative unit and component analysis unit.
2. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that unstripped gas air inlet Unit includes high pressure tank and pressure maintaining valve, and air storage tank volume is 0.4~0.6m3, pressure be 15~20MPa.
3. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that gas flow control Unit processed includes mass flowmenter, and mass flowmenter range is 0~100mL/min, 0~3000mL/min, and control precision is 0.1 Grade.
4. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that temperature control is single Member includes temperature control instrument and DCS system, and temperature control precision is 0.5 DEG C of 0.5~﹢ of ﹣.
5. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that vulcanization unit packet Vulcanizing tank, vulcanizing tank calandria, caustic treater are included, vulcanizing tank calandria uses water-bath circulating-heating mode, and heating temperature is 0~90 ℃。
6. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that reaction member packet The mixer and single tube reactor using pressure resistance, corrosion-resistant stainless steel material are included, while examining two catalyst samples.
7. sulfur-resistant transformation catalyst mesohigh activity assay device as claimed in claim 6, it is characterised in that single tube reactor Reaction tube having a size of 44 × 6mm, reaction pressure be 0~10MPa, reaction temperature is 0~550 DEG C, connected using soft seal screw thread It connects.
8. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that product separation is single Member includes cooling water circulation machine, condenser, condensing collector, and cooling water temperature can be adjusted to minimum subzero 10 DEG C.
9. sulfur-resistant transformation catalyst mesohigh activity assay device as described in claim 1, it is characterised in that component analysis list Member includes gas chromatograph and carry gas cleanser, and the volume fraction of carbon monoxide in the gas of front and back is reacted using TCS thermal conductivity Analysis.
CN201821457383.5U 2018-09-06 2018-09-06 Sulfur-resistant transformation catalyst mesohigh activity assay device Active CN208921669U (en)

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Application Number Priority Date Filing Date Title
CN201821457383.5U CN208921669U (en) 2018-09-06 2018-09-06 Sulfur-resistant transformation catalyst mesohigh activity assay device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201821457383.5U CN208921669U (en) 2018-09-06 2018-09-06 Sulfur-resistant transformation catalyst mesohigh activity assay device

Publications (1)

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