CN1166750C

CN1166750C - Oil slurry charring firing device and its method

Info

Publication number: CN1166750C
Application number: CNB011414693A
Authority: CN
Inventors: 范登利; 蔺玉贵
Original assignee: Sinopec Research Institute of Petroleum Processing; China Petroleum and Chemical Corp
Current assignee: Sinopec Research Institute of Petroleum Processing; China Petroleum and Chemical Corp
Priority date: 2001-09-27
Filing date: 2001-09-27
Publication date: 2004-09-15
Anticipated expiration: 2021-09-27
Also published as: CN1410509A

Abstract

The present invention discloses an oil slurry carbonization firing device and method. The device comprises a machine case, a partition board, a heat preservation jacket, a gas inlet circle pipe, a gas outlet circle pipe, a heat preservation layer, a heating jacket, a heating pipe, a sample case, a gas inlet connection pipe, a gas outlet connection pipe, a top cover part, a connection cup and a smoke channel connection pipe, wherein the gas inlet circle pipe and the gas outlet circle pipe are arranged in the heat preservation jacket, and the heating pipe is arranged in the heating jacket. When the device is used for carbonizing and firing oil slurry, solvent does not need to be used, the operating method is simple, the detection lower limit of the solid content can be enhanced, and the microscopic structure of a catalyst in the oil slurry can not be destroyed.

Description

Oil slurry charring firing device and using method thereof

Technical field

The invention relates to a kind of charring firing device and using method thereof of slurry oil.

Background technology

Contain catalyst fines and micro-ash content in the slurry oil of catalytic cracking process, catalyst fines content is how much relevant with the factors such as separation efficiency of catalyst strength, cyclonic separator in the slurry oil.Along with improving constantly of petrochemical complex oil Refining Technologies, the solid content in the slurry oil, promptly catalyst fines obviously reduces; Simultaneously, also more and more stricter along with the continuous expansion of slurry oil purposes to the requirement of slurry oil solid content, thereby the assay determination of slurry oil solid content also proposed higher requirement.

The method of mensuration slurry oil solid content commonly used is the solvent cut centrifuging at present, this method personal errors is bigger, be difficult to especially separate for heavier slurry oil sample, its detected level is minimum to be 2 grams per liters, because this method measured result has comprised catalyst fines, micro-ash content, coke and the amount of the oil that is wrapped in, so the slurry oil solid content is a relative value.

Also have some other similar approach to be used for reference in addition and introduce the measurement that is used for the slurry oil solid content, as " GB/T508-91 petroleum products determination of ash method (weighting method) ", this method operating process is loaded down with trivial details, analysis time is longer, and 800 ℃ of used service temperatures will damage the microtexture of catalyzer to a certain extent, be unfavorable for the follow-up further research that catalyst fines is formed mechanism; " GB/T511-88 petroleum products and additive mechanical impurity assay method (weighting method) ", this method solvent load is big, operating process is loaded down with trivial details, analysis time is long, main is because organic solvent can not be washed the coke of catalyzer outside off fully, its result and the incomplete content of representing catalyst fines in the slurry oil.

It seems from above-mentioned prior art, owing to there is not suitable processing oil slurry charring firing device, feasible at present not accurate enough to the mensuration of solid content in the slurry oil, and because the destruction of catalyst microstructure can not be done further research to the formation mechanism of catalyst fines.

Summary of the invention

The purpose of this invention is to provide a kind of oil slurry charring firing device and method, can remedy the deficiencies in the prior art, can obtain the solid content value more exactly, can't destroy the microtexture of catalyzer.

For achieving the above object, oil slurry charring firing device provided by the invention comprises cabinet, dividing plate at the cabinet middle part, the insulation jacket that process furnace on the dividing plate is placed from outside to inside along circumference, thermal insulation layer, heating jacket, sales kit (SK), header field on the sales kit (SK), connect cup under the dividing plate, horizontal flue is taken over, run through two flues adapters of dividing plate and add the gentle body flow controlling unit of thermal control units, wherein the upper and lower in insulation jacket is respectively and has advancing of aperture on the tube wall, the endless tube of giving vent to anger, the air inlet endless tube outside on top is connected with an air inlet tube, the endless tube inboard of giving vent to anger of bottom is connected with an outgoing gas connection tube, this outgoing gas connection tube links to each other insulation jacket with heating jacket, be provided with heating tube in heating jacket, the top of sample tank wall evenly has production well.

The present invention is further detailed explanation below in conjunction with drawings and embodiments.

Description of drawings

Fig. 1 is a schematic representation of apparatus provided by the invention.

Fig. 2 is the synoptic diagram of air inlet endless tube, air inlet tube in the device provided by the invention.

Fig. 3 is the synoptic diagram of give vent to anger in the device provided by the invention endless tube, outgoing gas connection tube.

Embodiment

At first referring to Fig. 1, this oil slurry charring firing device is taken over 2,12,25, flue plug 3,5,27, four-way 4,26, dividing plate 6, the endless tube 7 of giving vent to anger, outgoing gas connection tube 8, insulation jacket 9, thermal insulation layer 10,16, heating jacket 11, sales kit (SK) 13, air inlet endless tube 14, top plug 15, production well 17, top cover 18, heating tube 19, heating tube joint 20,24, air inlet tube 21, thermopair 22, thermal cross 23, awl section pipe 28, is connect glass cap 29, connects cup 30 and form by cabinet 1, flue.

Oil slurry charring firing device of the present invention, the shelf in the four directions that cabinet 1 can be welded into by angle bar is outer again to be covered tinned(sheet)iron and forms, and it is divided into two portions up and down by dividing plate 6.6 on dividing plate every upper part be mainly process furnace, insulation jacket 9 and heating jacket 11 are cylindrical shape, between insulation jacket 9 and heating jacket 11, link to each other by outgoing gas connection tube 8, be filled with lagging material in the thermal insulation layer 10, in insulation jacket 9, air inlet endless tube 14 and air inlet tube 21 are arranged at top, bottom give vent to anger endless tube 7 and outgoing gas connection tube 8; Be provided with heating tube 19 in the heating jacket 11, heating tube 19 play sample in the heated sample case 13 and the heating jacket 11 of flowing through in the effect of gas, heating tube 19 and thermopair 22 lead to beyond the insulation interlayer 9 by heating tube joint 20,24 and thermal cross 23 respectively, divide with temperature control part to link to each other; Is exactly sales kit (SK) 13 at the inwall of heating jacket 11 with plug 15 spaces that constituted, top, has several production wells that is evenly distributed 17 at the inwall of heating jacket 11 near the upper end edge circumference, production well 17 be oriented horizontal direction; On the top plug 15 is thermal insulation layer 16 and top cover 18; The bottom of sales kit (SK) 13 has the upper end of flue adapter 25 to link to each other, flue is taken over 25 and is passed lower part that dividing plate 6 enters cabinet 1, the lower end links to each other with four-way 26, horizontal interface one end of four-way 26 is plugs 27, one end is that flue takes over 2, and being connected with awl section pipe 28 at the vertical end interface down of four-way 26, awl section pipe connects cup caps 29 for 28 times and connects cup 30, connects glass cap 29 and connect glasss 30 to link to each other by spiral interface; The other end of flue adapter 2 links to each other with four-way 4, the lower port of horizontal port of another of four-way 4 and vertical direction is connected with flue plug 3 and flue plug 5 respectively, the upper port of vertical direction is connected with flue and takes over 12, and flue is taken over 12 and passed dividing plate 6 and vertically upward beyond the top of cabinet 1.

In device provided by the invention, the pattern of described heating tube 19 can be a coil pipe, but does not get rid of the pattern that other have good even heating mode; Described top cover 15 is slick sphere with the trim of sales kit (SK) 13, to guarantee good gravity sealing effectiveness; Be evenly distributed with aperture on the air inlet endless tube 14 and the endless tube 7 of giving vent to anger, to guarantee that gas can evenly spread, avoid producing bias current, the aperture of being opened is evenly to open along the vertical cross-section circumference of endless tube, and the perforate on all angles should evenly be staggered; Flue plug 3,5 and 27 effect be convenient to flue take over 2 and 12 may be remaining greasy dirt or the cleaning of coke; Behind the oil slurry charring firing from sales kit (SK) 13 through flue take over 25, awl section pipe 28 oil gas that get off and the condensation of flue gas nature enter and connect cup 30, uncooled gas is taken over 12 discharges from flue adapter 2 and flue, the design of described awl section pipe 28 its role is to reduce oil gas that charring firing generates and flue gas in the descending vapour lock that enters when connecing glass.Outer wall in flue adapter 2 and 12 also can be provided with water-cooled or gas cooling interlayer, to reclaim the temperature that heat also reduces flue simultaneously, the oil gas condensation is got off, but does not have such device that designs still to reach the effect of the said device of the present invention.

In the oil slurry charring firing device provided by the present invention, the material of said sales kit (SK), insulation jacket, heating jacket, heating tube, various adapters is stainless steel, and said thermal insulation layer 10 materials are insulating cotton, and thermal insulation layer 16 materials are insulating brick.

Said temperature control unit is used for the temperature programming of heating jacket 11 heating tubes 19, constant temperature, temperature-fall period are controlled.

Said gas control unit is connected in air inlet tube 21, is used to control the switching and the flow size of nitrogen and air.

The using method of oil slurry charring firing device of the present invention is as follows: will prepare to claim the quartz beaker of setting-out product to put into 600 ℃ retort furnace calcination more than 2 hours earlier, take out and in air, be cooled to 200-300 ℃, place the moisture eliminator of no siccative to be cooled to weighing after the room temperature; The slurry oil sample mix that needs are analyzed is even, so that catalyst fines wherein is evenly distributed in the slurry oil sample, thickness or the slurry oil sample that solidifies are answered preheating to make its fusing and are made the slurry oil sample temperature lower under the condition that guarantees sampling smoothly, from the slurry oil sample that mixes, take by weighing slurry oil and put into quartz beaker, again this quartz beaker is weighed up weight and put into sales kit (SK) 13; To push up plug 15, thermal insulation layer 16 and top cover 18 builds successively; Feed low flow velocity nitrogen purging, nitrogen is from air inlet tube 21, air inlet endless tube 14, and enter insulation jacket 9 through the aperture of air inlet endless tube 14, nitrogen is flowed downward by top in insulation jacket 9, enter give vent to anger endless tube 7 and outgoing gas connection tube 8 in proper order by the aperture on the endless tube 7 of giving vent to anger, and enter by the bottom of heating jacket 11, nitrogen in heating jacket 11 from the process that rises in the bottom, be heated pipe 19 heating, aperture 17 by sales kit (SK) 13 tops enters sales kit (SK), slurry oil sample in the sales kit (SK) 13 above-mentioned under the protection of heated nitrogen, through in 1 hour, being warmed up to 600 ℃ by room temperature, and 600 ℃ of constant temperature 20 minutes, in heat-processed, flue gas is constantly arranged from taking over 25 through flue, 2, taking over 12 by flue discharges, reduce to very little when take over 12 discharged flue gas from flue, show that the slurry oil sample has formed the carbonaceous resistates of dryness, nitrogen is switched to air purge 1-3 hour, and the coke that sample is generated all generates carbon dioxide, stops heating then, continuation is at air purge, make sales kit (SK) 13 be cooled to 250 ℃-300 ℃, take out quartz beaker, weigh after the moisture eliminator of putting into no siccative is cooled to room temperature; Said connect to receive in the cup 30 the oil gas that slurry oil produces behind charring firing and the condensation product of flue gas are arranged, when condensation product is filled in connecing cup 30, connect cup 30 condensation products of outwelling wherein by connecing to screw off on glass cap 29.

In the use of the said device of the present invention, the nitrogen of low flow velocity guarantees not bring air in the sales kit (SK), stop the burning of slurry oil sample steam, catalyst fines is taken away in the effect that prevents steam burning generation, under nitrogen purging, in 1 hour, sample slowly is heated to 600 ℃ from room temperature, slowly the process of heating can make sample destructive distillation slowly, slowly produce steam, thereby do not make the slurry oil sample overflow quartz beaker and cause loss, the gaseous purge stream that is entered sales kit (SK) 13 by production well 17 can suppress the ascension effect that steam upwards produces, about 20 minutes of 600 ℃ of constant temperature, can become the coke that destructive distillation produces the breeze of dryness, can prevent from when purging air, to burn fast.

Air purges sales kit (SK) 13 with higher flow velocity, can guarantee to be full of in the sales kit (SK) 13 oxygen containing air, the Heating temperature that is no more than 600 ℃ can guarantee that the microtexture of catalyzer is not destroyed in the slurry oil, be beneficial to further research, when temperature is reduced to 250 ℃, take out sample and can prevent that catalyzer from absorbing airborne moisture content.

In order to make quartz beaker be in the middle part of sales kit (SK), can adopt and make quartz beaker be in the middle part of sales kit (SK) 13, can avoid the direct purging of upper gas like this, can avoid again at the bottom of the case taking over the influence of eddy current that 25 interface forms sample with flue gas to the slurry oil sample.

Adopt oil slurry charring firing device provided by the invention and method thereof to have following advantage: simple to operate, do not use any solvent, pollution-free, can a large amount of samples of weighing, improve and detect lower limit, the microtexture of gained catalyzer can not destroyed, and can be used for further research.

Claims

1, a kind of oil slurry charring firing device, it is characterized in that this device comprises cabinet (1), dividing plate (6) at the cabinet middle part, the insulation jacket (9) that process furnace on the dividing plate (6) is placed from outside to inside along circumference, thermal insulation layer (10), heating jacket (11), sales kit (SK) (13), header field on the sales kit (SK) (13), under the dividing plate connect the cup (30), horizontal flue is taken over (2), two flues that run through dividing plate are taken over (12) and (25) and are added the gentle body flow controlling unit of thermal control units, wherein be respectively air inlet endless tube (14) that has aperture on the tube wall and the endless tube of giving vent to anger (7) in the upper and lower of insulation jacket (9), air inlet endless tube (14) outside on top is connected with an air inlet tube (21), the endless tube of giving vent to anger (7) inboard of bottom is connected with an outgoing gas connection tube (8), this outgoing gas connection tube (8) links to each other insulation jacket (9) with heating jacket (11), be provided with heating tube (19) in heating jacket (11), the top of sample tank wall evenly has production well (17).

2,, it is characterized in that said header field is made up of top plug (15), thermal insulation layer (16) and top cover (18) according to the said device of claim 1.

3, according to the said device of claim 1, it is characterized in that said horizontal flue gas takes over an end of (2) and link to each other with flue gas adapter (12) by four-way (4), the other end is taken over (25) by four-way (26) and flue and is linked to each other, two other interface of four-way (4) is flue plug (3) and (5), the lower port of four-way (26) is connected with awl section pipe (28), and side ports is flue plug (27).

4,, it is characterized in that the aperture of being opened on said air inlet endless tube (14) and the endless tube of giving vent to anger (7) is evenly to open along the vertical cross-section circumference of endless tube, and the perforate on all angles is staggered evenly according to the said device of claim 1.

5, according to the said device of claim 1, it is characterized in that said thermal insulation layer (10) material therefor is an insulating cotton, thermal insulation layer (16) material therefor is an insulating brick.

6,, it is characterized in that the pattern of said heating tube (19) is a coil pipe according to the said device of claim 1.

7, use the method for the said oil slurry charring firing device of claim 1, it is characterized in that the slurry oil sample in the quartz beaker is put in the sales kit (SK) (13), to push up plug (15), thermal insulation layer (16) and top cover (18) are built successively, under the purging of nitrogen, in 1 hour sales kit (SK) is heated to 600 ℃ from room temperature, said nitrogen is from air inlet tube (21), air inlet endless tube (14), and enter insulation jacket (9) through the aperture of air inlet endless tube (14), nitrogen is flowed downward by top in insulation jacket (9), enter endless tube of giving vent to anger (7) and outgoing gas connection tube (8) in proper order by the aperture on the endless tube of giving vent to anger (7), and enter by the bottom of heating jacket (11), nitrogen in heating jacket (11) from the process that rises in the bottom, be heated pipe (19) heating, aperture (17) by sales kit (SK) (13) top enters sales kit (SK), slurry oil sample in the sales kit (SK) (13) above-mentioned under the protection of heated nitrogen, through in 1 hour, being warmed up to 600 ℃ by room temperature, and 600 ℃ of constant temperature 20 minutes, in heat-processed, flue gas is constantly arranged from taking over (25) through flue, (2), taking over (12) by flue discharges, reduce to very little when taking over (12) discharged flue gas from flue, show that the slurry oil sample has formed the carbonaceous resistates of dryness, nitrogen is switched to air purge 1-3 hour, the coke that sample is generated all generates carbon dioxide, stop heating then, continuation is at air purge, make sales kit (SK) (13) be cooled to 250 ℃-300 ℃, take out quartz beaker, weigh after the moisture eliminator of putting into no siccative is cooled to room temperature; Said connect to receive in the cup (30) the oil gas that slurry oil produces behind charring firing and the condensation product of flue gas are arranged, when condensation product is filled in connecing cup (30), connect cup (30) and outwell wherein condensation product by connecing to screw off on glass cap (29).