CN1676206B - Gas and solid granular reaction method - Google Patents
Gas and solid granular reaction method Download PDFInfo
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- CN1676206B CN1676206B CN 200410029864 CN200410029864A CN1676206B CN 1676206 B CN1676206 B CN 1676206B CN 200410029864 CN200410029864 CN 200410029864 CN 200410029864 A CN200410029864 A CN 200410029864A CN 1676206 B CN1676206 B CN 1676206B
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention relates to a method for making gas and solid granules produce reaction. Said method includes that making gas be contacted with solid granules, the described contact is simplemented in a reaction equipment, said reaction equipment comprises a reaction kettle, a material inlet and a gas outlet, in which the interior of reaction kettle is equipped with a stirring device, and on the gas outlet a gas-solid separator is mounted. Said invention also provides the connection mode of them and working principle of said method and reaction equipment.
Description
Technical field
The invention relates to the method for a kind of fluid and solid particle reaction, more specifically say so about the method for a kind of gas and solid particle reaction.
Background technology
Existing gas comprises with the method that solid particle reacts gas is contacted with solid particle, described contact is carried out in a consersion unit, described consersion unit is made up of a reaction tube (or being called reactor) and an air inlet and a gas outlet of being positioned at the reaction tube two ends, and described solid particle is a solid particle material fixed body bed.When carrying out the reaction of gas and solid particle, the solid particle material fixed body bed of packing in the centre position of reactor, fill with fillers such as porcelain ring or quartz materials at two, enrich to guarantee that solid particle is filled, the stage casing that is present in reactor regularly, and guarantee that gas flows through solid particle reposefully.Gas that reacts with solid particle or the gas that carries the material that reacts with solid particle react with solid particle by the solid particle bed time.The waste gas that unreacted gas and reaction generate is discharged through the gas outlet.
The method of existing gas and solid particle reaction has significant disadvantages.For example, adopt the reaction method of existing gas and solid particle,, can not move, and solid particle mass transfer and heat transfer character are relatively poor because the solid particle in the solid particle bed is static.When exothermic reaction, heat is difficult for diffusion rapidly, causes the bigger reaction temperature gradient of generation in fixed bed, makes the reaction of solid particle and gas inhomogeneous, and the solid product character that obtains is inhomogeneous.More under the serious situation, easily produce hot-spot, the temperature difference of solid particle bed is destroyed the structure of some solid particle itself up to 200 ℃.When the endothermic reaction, easily produce local quenching, in time additional heat so just makes the reaction of part solid particle and gas incomplete, also makes the solid product character that obtains inhomogeneous.
In course of reaction, some solid particle such as particle diameter are the superfine powder below 5 microns, because electrostatic interaction and the character of itself decision are easy to be agglomerated into fine and close block.The material that gas that has and solid particle reaction generate (reacting the aluminium compound that removes as zeolite and silicon tetrachloride) has the effect of binding agent, also makes solid particles agglomerate become fine and close block easily.The formation of a large amount of compact massive things is bonded on the wall of reactor the block of formation on the one hand, causes product loss and needs the cleaning wall.On the other hand, the generation of compact massive thing makes gas contact become inhomogeneous with solid, and the character of the product that obtains is also inhomogeneous.
Again for example, adopt the reaction method of existing gas and solid particle, because solid particle is a static fixed bed, two ends must have filler to fill, so just caused the inconvenience of solid particle dismounting, also will separate with filler solid particle, not only labour intensity is big, and the conveying of solid particle and draw off from consersion unit and be difficult for to realize automation.Particularly, when solid particle is when having the superfine powder material of corrosivity and penetrating odor, because loading and unloading are inconvenient, easy contaminated environment, fragile operating personnel are healthy.
Also be because solid particle is a static fixed bed, gas that reacts with solid particle or the gas that carries the material that reacts with solid particle must be the gas that flows, the gas that reacts with solid particle, very big like this as the consumption that carries gas and reactive material that carries reactive material, contain the waste gas that unreacted gas and reaction produce, perhaps contain as the treating capacity of carrying the waste gas material that gas, the reactive material that does not react with solid and reaction back produce of carrying reactive material very big.
Summary of the invention
The objective of the invention is to overcome the above-mentioned shortcoming of prior art, provide a kind of new, the reaction of gas and solid particle can evenly be carried out, and the reaction condition of gas and solid particle is easy to control, and solid particle is difficult for being agglomerated into the gas of piece and the method for solid particle reaction.
Method provided by the invention comprises gas is contacted with solid particle, described contact is carried out in a consersion unit, wherein, described consersion unit comprises a reactor 1, a charging aperture 2 and a gas outlet 3, wherein, also comprise an agitator 4 in the inside of reactor 1, a gas-solid separator 5 is installed on the gas outlet 3, the bore dia of gas-solid separator 5 contained holes and porosity guarantee gas can by and solid particle can not pass through, the puddler of agitator 4 stretches out outside the reactor 1, and it is local airtight that puddler contacts with reactor 1, and reactor 1 is not in communication with the outside; The material of solid particle and gas or energy process gas is joined in the reactor 1 through charging aperture 2, and under the stirring of agitator 4, described solid particle contacts with the gas that described gas maybe can generate the material generation of gas.。
Owing to comprise a stirring in the described consersion unit of method provided by the invention, solid particle under agitation, evenly roll, not only overcome use fixed bed mass transfer, heat transfer property is poor, the reaction condition of gas and solid particle is wayward, reaction temperature is inhomogeneous, easily cause hot-spot or cold excessively shortcoming, also make gas and solid particle haptoreaction more even, therefore, can obtain the more uniform solid particulate product of character.Particularly, when solid particle be diameter below 5 microns superfine powder or during nano-scale particle, adopt method provided by the invention, solid material can be well tumble mixed up and down, avoided the phenomenon that is agglomerated into the compact massive thing between the solid particle.
When adopting method provided by the invention to carry out the reaction of gas and solid particle, has only a kind of solid particle, do not need filler, therefore, save separating of solid particle and filler, made the complete closed conveying of solid particle and draw off to become from reactor automatically to be more prone to, can reduce labour intensity, reduce environmental pollution and work personnel and the chance that the superfine powder material with corrosivity and penetrating odor contacts, be easy to carry out large-scale industrial application.
Adopt method provided by the invention when carrying out the reaction of gas and solid particle, can carry out in confined conditions, on the one hand, in confined conditions, can make full use of the characteristic that gaseous material is easy to spread and the characterization of adsorption of solid particle, make gas and solid even contact, and gaseous material is diffused in the solid lattice, carry out sufficient adsorption/desorption reaction, improve the quality of products.On the other hand, can be according to the consumption of solid particle, quantitatively add the material that maybe can form the gas that reacts with solid particle with the gas of solid particle reaction, and, do not need to use and carry gas, thereby reduced the loss and the discharging of reacting gas material, reduced pollution, reduced production cost significantly.
The gas-solid separator that install the gas outlet of the described consersion unit of method provided by the invention can separate gas effectively with solid, waste gas after guaranteeing to react can be discharged, even and particle diameter is less than 1 micron, 0.3 micron solid particle pipeline discharge from then on even, avoided the loss of solid particle, reduced dust pollution, input-output ratio is improved.
Description of drawings
Accompanying drawing 1-8 is the schematic diagram of the described consersion unit of method provided by the invention;
Accompanying drawing 9-10 is a spiral ribbon agitator schematic diagram in the described consersion unit of method provided by the invention;
Accompanying drawing 11 is reactor rip cutting schematic diagrames of the described consersion unit of method provided by the invention.
The specific embodiment
According to method provided by the invention, under the preferable case, the waste gas that reaction generates through the gas outlet 3 and gas-solid separator 5 discharge.
The present invention has many concrete embodiments, is wherein representative example below.
First specific embodiment of the present invention as shown in Figure 1.Described consersion unit comprises a reactor 1, a charging aperture 2 and a gas outlet 3, also has an agitator 4 in the inside of reactor 1, wherein, a gas-solid separator 5 is installed on the gas outlet 3, the bore dia of gas-solid separator 5 contained holes and porosity guarantee gas can by and solid particle can not pass through, the puddler of agitator 4 stretches out outside the reactor 1, it is local airtight that puddler contacts with reactor 1, and reactor 1 is not in communication with the outside.
When carrying out the reaction of gas and solid particle, from charging aperture 2 solid particle of packing into, start agitator 4, and the gas of adding and solid particle reaction maybe can generate the material with the gas of solid particle reaction, charging aperture 2 and gas outlet 3 is airtight.Heating or do not heat reactor 1 to reaction temperature makes the described gasification substance that can generate with the gas of solid particle reaction, reaction under agitation.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 2nd specific embodiments of the present invention as shown in Figure 2.Described consersion unit comprises all members of first specific embodiment, in addition, also comprises an air inlet 6.Described air inlet 6 can be positioned at the optional position of reactor 1, and under the preferable case, charging aperture 2 and gas outlet 3 are positioned at the top of reactor 1, and air inlet 6 is positioned at the bottom of reactor 1.Air inlet 6 is used for adding the material that the gas with the solid particle reaction maybe can gasify.Air inlet 6 has been arranged, and the material that gas maybe can generate with the gas of solid particle reaction adds from air inlet 6, and charging aperture 2 is used for adding solid particle specially, operates easier.
When carrying out the reaction of gas and solid particle, from charging aperture 2 solid particle of packing into, start agitator 4, charging aperture 2 and gas outlet 3 is airtight.Add the material that maybe can generate the gas that reacts with solid particle with the gas of solid particle reaction from air inlet 6, pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the reactor 1, the heating or do not heat reactor 1 to reaction temperature, make the described gasification substance that can generate the gas that reacts with solid particle, reaction under agitation.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 3rd specific embodiments of the present invention as shown in Figure 3.Described consersion unit comprises the 2nd all members of the specific embodiment, and, a gas distributor 9 is housed on the top of air inlet 6, at the bottom of the still of the top and reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of reactor 1 still.The effect of described gas distributor is that gas can be entered in the reactor 1 continuously equably, simultaneously, guarantees that solid particle does not enter in the pipeline that links to each other with air inlet 6.
When carrying out the reaction of gas and solid particle, from charging aperture 2 solid particle of packing into that charging aperture 2 and gas outlet 3 is airtight, start agitator 4, charging aperture 2 is airtight.Add the material that maybe can generate the gas that reacts with solid particle with the gas of solid particle reaction from air inlet 6, pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the reactor 1, the heating or do not heat reactor 1 to reaction temperature, generate the material of the gas that reacts with solid particle after gasification with the gas or the described energy of solid particle reaction, by the distributional effects of gas distributor 9, enter reactor 1 equably and under agitation react with solid particle.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 4th specific embodiment of the present invention as shown in Figure 4.Described consersion unit comprises all members of first specific embodiment, in addition, also comprises a discharging opening 7.Charging aperture 2 and gas outlet 3 are positioned at the top of reactor 1, and discharging opening 7 is positioned at the bottom of reactor 1.Discharging opening 7 is used for drawing off reacted solid particle.Discharging opening 7 has been arranged, and the reactor 1 that can overturn just can easily draw off reacted solid particle, operates easier.
When carrying out the reaction of gas and solid particle, gas outlet 3 and discharging opening 7 is airtight, from charging aperture 2 solid particle of packing into, start agitator 4, and the gas of adding and solid particle reaction maybe can generate the material with the gas of solid particle reaction, and charging aperture 2 is airtight.Heating or do not heat reactor 1 to reaction temperature makes the described gasification substance that can generate with the gas of solid particle reaction, reaction under agitation.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Open discharging opening 7, draw off reacted solid from discharging opening 7.
The 5th specific embodiment of the present invention as shown in Figure 5.Described consersion unit comprises the 4th all members of the specific embodiment, in addition, the dish 8 that can dismantle is housed on the top of discharging opening 7, can have also on this dish 8 and can not have a plurality of apertures, the size of aperture can not enter in the pipeline that links to each other with discharging opening 7 solid particle by aperture, at the bottom of the still of the upper surface of dish 8 and reactor 1 in one plane or be higher than the plane at place at the bottom of reactor 1 still.Described dish 8 guarantees that solid particle does not enter in the pipeline that links to each other with discharging opening 7, avoids part solid particle and gas reaction insufficient, thereby the situation of loss part solid particle takes place.
When carrying out the reaction of gas and solid particle, gas outlet 3 and discharging opening 7 is airtight, from charging aperture 2 solid particle of packing into, start agitator 4, and the gas of adding and solid particle reaction maybe can generate the material with the gas of solid particle reaction, and charging aperture 2 is airtight.Heating or do not heat reactor 1 to reaction temperature makes the described gasification substance that can generate with the gas of solid particle reaction, reaction under agitation.Because the existence of dish 8, in the course of reaction, solid particle can not enter the pipeline that links to each other with discharging opening.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Open discharging opening 7 and unload dish 8, draw off reacted solid from discharging opening 7.
Embodiment 6
The 6th specific embodiment of the present invention as shown in Figure 6.Described consersion unit comprises all members of first specific embodiment, comprises an air inlet 6 and discharging opening 7 in addition; Charging aperture 2 and gas outlet 3 are positioned at the top of reactor 1, and air inlet 6 and discharging opening 7 are positioned at the bottom of reactor 1.A gas distributor 9 is housed on the top of air inlet 6, at the bottom of the still of the top and reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of reactor 1 still; A dismountable dish 8 is housed on the top of discharging opening 7, can be with or without a plurality of apertures on this dish 8, the size of aperture can not enter in the pipeline that links to each other with discharging opening 7 solid particle by aperture, at the bottom of the still of the upper surface of dish 8 and reactor 1 in one plane or be higher than the plane at place at the bottom of reactor 1 still.Described distributor 9 plays the effect of gas distributor, and gas can be entered in the reactor 1 continuously equably, simultaneously, guarantees that solid particle does not enter in the pipeline that links to each other with air inlet 6.Described dish 8 guarantees that solid particle does not enter in the pipeline that links to each other with discharging opening 7, avoids part solid particle and gas reaction insufficient, thereby the situation of loss part solid particle takes place.
When carrying out the reaction of gas and solid particle, gas outlet 3 and discharging opening 7 is airtight, from charging aperture 2 solid particle of packing into, charging aperture 2 is airtight, start agitator 4, add the material that maybe can generate the gas that reacts with solid particle with the gas of solid particle reaction from air inlet 6, pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the reactor 1, the heating or do not heat reactor 1 to reaction temperature, generate the material of the gas that reacts with solid particle after gasification with the gas or the described energy of solid particle reaction, by the distributional effects of distributor 9, enter reactor 1 equably and under agitation react with solid particle.Because the existence of dish 8, in the course of reaction, solid particle can not enter the pipeline that links to each other with discharging opening.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Open discharging opening 7 and unload dish 8, draw off reacted solid from discharging opening 7.
The 7th specific embodiment of the present invention as shown in Figure 7.Described consersion unit comprises all members of first specific embodiment, comprises an air inlet 6 and discharging opening 7 in addition; Discharging opening 7 is positioned at the bottom of reactor 1, air inlet 6 communicates with reactor 1 by discharging opening 7, a dismountable gas distributor 9 is equipped with on the top of discharging opening 7, at the bottom of the still of the top and reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of reactor 1 still.Described gas distributor 9, both played the effect of gas distributor, gas can evenly be entered in the reactor 1, guaranteed again that solid particle did not enter in the pipeline that links to each other with discharging opening 7, avoid part solid particle and gas reaction insufficient, thereby the situation of loss part solid particle take place.
When carrying out the reaction of gas and solid particle, gas outlet 3 and discharging opening 7 is airtight, from charging aperture 2 solid particle of packing into, charging aperture 2 is airtight, start agitator 4, add the material that maybe can generate the gas that reacts with solid particle with the gas of solid particle reaction from air inlet 6, pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the reactor 1, the heating or do not heat reactor 1 to reaction temperature, generate the material of the gas that reacts with solid particle after gasification with the gas or the described energy of solid particle reaction, by the distributional effects of gas distributor 9, enter reactor 1 equably and under agitation react with solid particle.Because the existence of gas distributor 9, in the course of reaction, solid particle can not enter the pipeline that links to each other with discharging opening.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Open discharging opening 7 and unload gas distributor 9, draw off reacted solid from discharging opening 7.
The 8th specific embodiment of the present invention as shown in Figure 8.Described consersion unit comprises the 7th all members of the specific embodiment, in addition, at reactor 1 outside electrical heating cover 10 in addition, comprise the interface 12 of a connection Pressure gauge 11 and the recess 14 that at least one heat supply galvanic couple 13 inserts on the top of reactor 1, recess 14 is not communicated with reactor 1, thermocouple 13 is connected with the instrument of displays temperature, with the temperature in the Indicator Reaction still 1.
When carrying out the reaction of gas and solid particle, gas outlet 3 and discharging opening 7 is airtight, from charging aperture 2 solid particle of packing into, that charging aperture 2 is airtight.Start agitator 4, add the material that maybe can generate the gas that reacts with solid particle with the gas of solid particle reaction from air inlet 6, pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the reactor 1, start the power supply of electrical heating cover 10, reactor 1 is heated to required temperature, generate the material of the gas that reacts with solid particle after gasification with the gas or the described energy of solid particle reaction, by the distributional effects of gas distributor 9, enter reactor 1 equably and under agitation react with solid particle.Pressure and temperature in the reactor 1 is read with the instrument that links to each other with the thermocouple that inserts recess 14 from Pressure gauge 11 respectively.Because the existence of gas distributor 9, in the course of reaction, solid particle can not enter the pipeline that links to each other with discharging opening.After reaction is finished, close agitator 4, stop to stir, cool off or do not cool off, open gas outlet 3, waste gas is discharged, carry out waste gas and reclaim.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Open discharging opening 7 and unload gas distributor 9, draw off reacted solid from discharging opening 7.
According to method provided by the invention, described reactor 1 can be a shape arbitrarily, is oval-shaped column, coniform, square as cylindric, spherical, cross section, cuboid or other irregular shape.For solid particle is mixed more evenly and easy-unloading, under the preferable case, described reactor 1 is cylindric, spherical, coniform or following band cone as shown in figure 11 cylindric.
The position of agitator 4 should be able to mixing solids, solid particle is evenly rolled and flows, and do not contact with the wall of reactor 1.Described agitator 4 can be conventional agitator, as climbs formula agitator, blade mixer, spiral ribbon agitator, gate stirrer, circular tank bracket agitator etc.
Preferred agitator 4 is a spiral ribbon agitator as shown in Figure 9.This agitator comprises a puddler 15, stirring is with 16 with two ends and puddler 15 and stir with 16 support bars that link to each other 17, and stirring is with 16 to be the axle center with puddler 15, spiral escalation or decline, stirring the plane of band and the angle α of horizontal plane is the 10-70 degree, preferred 20-50 degree.The width of ribbon changes in very significantly according to the size of reactor 1 and the amount of solid particle, and in general, the width of ribbon is a 0.005-1 rice, is preferably 0.01-0.5 rice.The pitch that stirs the spiral of band formation can in very large range change, such as the used agitator of laboratory small-scale test, its pitch can be as small as several millimeters, and at the agitator of industrial use, its pitch can be up to several meters, in general, the pitch that stirs the spiral of band formation is 0.005-2 rice, is preferably 0.01-1 rice.
The recess 14 that inserts thermocouple 13 need extend near the axle center of reactor 1, and for fear of the collision of recess 14 with agitator 4, the stirring of described agitator 4 is with 16 at least 2 sections of can be divided into as shown in figure 10, and stir between the band at 2 sections the position of recess 14.Adopt such agitator, at agitator when direction is rotated, easily material is risen to the top from the bottom of reactor 1, solid particle can successfully prolong and stirs band and slide, and stirs, make gas and solid particle even contact, avoid material to form the hole, center, form the phenomenon in duricrust district, can solve the solid material defective slow, the mass transfer difference of conducting heat better by wall, avoid hot-spot, be suitable for the heat release and the endothermic reaction.During the agitator counter-rotating, produce a kind of downward thrust, help discharging.
Gas-solid separator 5 is that any one can see through gas, and can not see through the material of solid particle.Usually, described gas-solid separator is a kind of porous material, the bore dia of described porous material contained hole and porosity guarantee gas can by and solid particle can not pass through.The bore dia of described porous material and porosity design according to the solid particle size of the reaction that participates in gas and solid particle, as when the solid particle diameter is the 0.1-5 micron, the bore dia of described porous material contained hole is the 1-40 micron, preferred 5-20 micron, porosity is 5-60%, is preferably 10-40%.Described porous material can be ceramic material, cement material, glass fiber material, Refrasil, the synthetic expanding material of polytetrafluoroethylene fibre material, fluoropolymer and glass fibre, contains the stainless steel agglomerated material of Cr, Ni, Ti and/or Mo.Gas-solid separator 5 guarantees that with being connected of reactor 1 reactor 1 can only be in communication with the outside by gas-solid separator 5, this can be by covering gas-solid separator 5 on the gas outlet 3 of reactor 1, and airtight the reaching of part that gas-solid separator 5 is contacted with reactor 1.
Described gas distributor 9 can be existing all gases distributor, a kind of as in dish type gas distributor, tubular gas distributor, spirally coiled gas distributor, cylindrical gas distributor, the spheroid gas distributor, these gas distributors are conventionally known to one of skill in the art.With the dish type gas distributor is example, and the dish type gas distributor is a dish, and a plurality of apertures are arranged on the dish, and the size of aperture makes solid particle can not pass through aperture, and gas can pass through aperture smoothly.The size of aperture decide according to the size of the solid particle that participates in reaction, and when being the 0.1-5 micron as the diameter of solid particle, the diameter of the aperture on the dish is the 1-6 millimeter, preferably the 2-5 millimeter.
The size of aperture can not enter in the pipeline that links to each other with discharging opening 7 solid particle by aperture on the dish 8, the size of aperture is decided according to the size of the solid particle that participates in reaction, when being the 0.1-5 micron as the diameter of solid particle, the diameter of the aperture on the dish is the 1-6 millimeter, preferred 2-5 millimeter.
The method of airtight each opening can adopt various existing methods, and these methods are conventionally known to one of skill in the art.As adopt the welding airtight, bonding airtight, the spiral shell button is airtight, packing is airtight, the flange packing ring is airtight or mounted valve is airtight.
Described electrical heating cover 10 a kind of heaters that just can adopt, described heating jacket can be used the mode of heating of equivalence arbitrarily, as adopts direct naked light heating, and modes such as water-bath heating, oil bath heating replace.
The material of the gas of energy generation and solid particle reaction refers to the solid or the liquid of the gas that any energy generation and solid particle react.When the material that can generate the gas that reacts with solid particle is solid, can join in the reactor 1 with described solid particle from charging aperture 2.When the material that can generate the gas that reacts with solid particle is liquid, can join in the reactor 1 with described solid particle from charging aperture 2, also can and preferably join the reactor from air inlet 6.Under the preferable case, the material that can generate the gas that reacts with solid particle refers to generate the liquid of the gas that reacts with solid particle.
Method provided by the invention is adapted to the reaction of various solid particles and gas.Being particularly suitable for particle diameter and being superfine powder solid particle below 5 microns and nanoscale solids particle and gas reacts.
Following example will the present invention will be further described.
Example 1
This example illustrates the described consersion unit of method provided by the invention.
With thickness is that 3 millimeters the industrial trade mark is that the stainless steel of NiCr18Ti is made equipment as shown in Figure 8.Away from the port of reactor 1 valve has been installed at charging aperture 2, gas outlet 3, air inlet 6 and discharging opening 7.
Wherein, the kettle of reactor 1 is cylindrical, and the kettle interior diameter is 100 millimeters, and is high 290 millimeters, and the diameter of charging aperture 2 is 30 millimeters, and the diameter of gas outlet 3 is 6 millimeters, and the diameter of air inlet 6 is 6 millimeters, and the diameter of discharging opening 7 is 30 millimeters.
Gas distributor 9 is the dish type distributor of 30 millimeters of diameters, and 50 diameters that evenly distributed on it are 2 millimeters aperture.
Gas-solid separator 5 is that thickness is 3 millimeters, cross-sectional diameter is 15 millimeters, the industry trade mark is that material (manufacturing of Beijing Satellite Manufacturing Factory of the China Aerospace group) porosity that the stainless steel powder powder material sintering of 1Cr18Ni9Ti is made is 30%, and the bore dia of contained hole is the 10-20 micron.Gas-solid separator 5 covers on the gas outlet 3, and the position that gas-solid separator 5 contacts with reactor 1 adopts the spiral shell button airtight.
Example 2
This example illustrates the described consersion unit of method provided by the invention.
With thickness is that 3 millimeters the industrial trade mark is that the steel alloy of 0Cr18Ni10Ti is prepared equipment as shown in Figure 1.Reactor 1 is that a diameter is 200 millimeters a spherical.
The diameter of charging aperture 2 is 30 millimeters, the diameter of gas outlet 3 is 6 millimeters, and gas-solid separator 5 is that thickness is 2 millimeters, and cross-sectional diameter is 10 millimeters, porosity is 25%, and the bore dia of contained hole is the disk (Beijing nonferrous metallurgy institute system) that the Ti alloy sintering of 5-10 micron is made.The position of gas-solid separator 5 and reactor contact adopts that flange is airtight to be connected.
Example 3
This example illustrates the described consersion unit of method provided by the invention.
With thickness is that 4 millimeters the industrial trade mark is that the steel alloy of 0Cr18Ni9 is prepared equipment as shown in Figure 8.Away from the port of reactor 1 valve has been installed at charging aperture 2, gas outlet 3, air inlet 6 and discharging opening 7.
Wherein, the kettle of reactor 1 is a cylinder of being with cone as shown in figure 11 down, and the cylinder interior diameter is 100 millimeters, and is high 290 millimeters, and cone top interior diameter is 100 millimeters, and the bottom interior diameter is 30 millimeters, 80 millimeters of height.The diameter of charging aperture 2 is 30 millimeters, and the diameter of gas outlet 3 is 6 millimeters, and the diameter of air inlet 6 is 6 millimeters, and the diameter of discharging opening 7 is 30 millimeters.
Gas distributor 9 is the dish type distributor of 30 millimeters of diameters, and 80 diameters that evenly distributed on it are 2 millimeters aperture.
Agitator 4 is 2 segmentation spiral ribbon agitators shown in Figure 10.Puddler 15, stir be with 16 and support bar 17 all make with stainless steel.12 millimeters of puddler 15 diameters, described spiral is from the bottom of puddler 15, and the height of top spiral is 100 millimeters, and diameter is 90 millimeters, the height of bottom hurricane band is 215 millimeters, distance between 2 hurricane bands is 10 millimeters, and wherein, the height of the bottom spiral that the reactor cone is above is 140 millimeters, diameter is 90 millimeters, in the reactor cone, the height of bottom spiral is 75 millimeters, and the diameter of spiral is decremented to 20 millimeters along the awl wall from 90 millimeters equably.The upper and lower spiral is with 16 to be connected puddler 15 and stirring with 4 with 8 support bars that are uneven in length 17 respectively equidistantly, makes to stir to be with 16 to fix.5 millimeters of the bottoms of puddler 15 apart from the bottom of reactor 1, the length that puddler 15 stretches out reactor 1 outer part is 20 millimeters, puddler 15 links to each other with motor, stirring is 30 degree with the angle α of 16 plane and horizontal plane, stirring is 10 millimeters with 16 width, and total pitch number of top spiral and bottom spiral is 15.
Gas-solid separator 5 is that thickness is 0.86 millimeter fluoropolymer and glass fibre synthetic material (Shanghai Co., Ltd of U.S. GORE-TEX FILTRATION PRODUCT company product).This gas-solid separator can 100% filters 0.4 micron solid particle, and 90-95% filters the solid particle of 0.2-0.3 micron, and 70-80% filters 0.1 micron solid particle.The position of gas-solid separator 5 and reactor contact adopts that flange is airtight to be connected.
Example 4
This example illustrates the described consersion unit of method provided by the invention.
Except that agitator 4 for climbing the formula agitator, other material equipment is all identical with example 1.When the described formula agitator 4 of climbing when rotating, stirring band, to rotate formed columniform diameter be 90 millimeters.
Example 5
This example illustrates method provided by the invention.
Charging aperture 2 from example 1 described consersion unit, with 800 gram (butt weight) solid contents is 99% powdery rare earth Y zeolite (lattice constant 2.468 nanometers, sodium oxide content 4.5 weight %, 985 ℃ of lattice avalanche temperature, rare earth oxide content 19 weight %, wherein, lanthana content is 4.9 weight %, cerium oxide content is 9.7 weight %, and other rare earth oxide content is 4.4 weight %, and the particle diameter of powdery rare earth Y zeolite is the 0.3-1 micron) join in the reactor 1.Close the valve of charging aperture 2 and gas outlet 3.Turn on agitator 4, mixing speed are 100 rev/mins.Open the power supply of electrical heating cover 10, elevate the temperature to be positioned at reactor 1 in the middle of the SR74 type intelligent temperature control instrument displays temperature that links to each other of thermocouple 13 be 280 ℃ (at this moment, the SR74 type intelligent temperature control instrument displays temperature that links to each other with the thermocouple 13 that is positioned at reactor 1 top also is 280 ℃), constant temperature feeds SiCl from air inlet 6
4Liquid 130 grams, SiCl
4Gasification also enters reactor 1 by gas distributor 9, reacts with Rare Earth Y.Reactor 1 internal pressure maintains 4 kilograms per centimeter substantially
2, reactor 1 internal pressure is read from Pressure gauge 11.React after 5 hours, close the power supply of electrical heating cover 10, be cooled to room temperature.Slowly open exhaust outlet 3, waste gas is slowly discharged from gas-solid separator 5.Open discharging opening 7 and lay down gas distributor 9,, discharge solid product smoothly agitator 4 counter-rotatings.With 20 times of deionized water washing solid products to solid product, 120 ℃ of oven dry, get 790 gram Y type zeolites containing rare-earth and high content of silicon, its lattice constant 2.445 nanometers, sodium oxide content 0.32 weight %, lattice avalanche temperature is 1020 ℃, and rare earth oxide content is 14.5 weight %, wherein, lanthana content is 3.8 weight %, cerium oxide content is 7.4 weight %, and other rare earth oxide content is 3.3 weight %), the solid yield is 98.8 weight %.Wherein, lattice constant adopts X-ray diffraction method to measure, and lattice avalanche temperature adopts Differential scanning calorimetry to measure, and rare earth oxide content adopts x-ray fluorescence spectrometry, and sodium oxide content adopts colorimetric method for determining.
Example 6
This example illustrates method provided by the invention.
Charging aperture 2 from example 2 described consersion units, with 1000 gram (butt weight) solid contents is 99% powdery rare earth sodium Y zeolite (lattice constant 2.470 nanometers, sodium oxide content 5 weight %, 986 ℃ of lattice avalanche temperature, rare earth oxide content 14 weight %, wherein, lanthana content is 4.16 weight %, cerium oxide content is 8.16 weight %, and other rare earth oxide content is 1.68 weight %, and the particle diameter of powdery rare earth sodium Y zeolite is the 0.5-1.5 micron) and 180 gram SiCl
4Liquid joins in the reactor 1.With airtight charging aperture 2 of the spiral shell button that is lined with teflon gasket and gas outlet 3.Turn on agitator 4, mixing speed are 180 rev/mins.It is in 180 ℃ the oil bath that reactor 1 is immersed temperature, reacts 5 hours, and reactor 1 is taken out from oil bath, is cooled to room temperature, slowly opens gas outlet 3, combustion gas.Dry the greasy dirt on the reactor 1, upset reactor 1 is opened charging aperture 2, and solid product is drawn off.With 20 times of deionized water washing solid products to solid product, 120 ℃ of oven dry, get 990 gram Y type zeolites containing rare-earth and high content of silicon, its lattice constant is 2.456 nanometers, sodium oxide content 0.45 weight %, lattice avalanche temperature is 1010 ℃, and rare earth oxide content is 12.5 weight %, wherein, lanthana content is 3.25 weight %, cerium oxide content is 6.38 weight %, and other rare earth oxide content is 2.87 weight %), the solid yield is 99 weight %.
Example 7
This example illustrates method provided by the invention.
Charging aperture 2 from example 3 described consersion units, with 600 gram (butt weight) solid contents is 99% powdery NaY zeolite (lattice constant 2.470 nanometers, sodium oxide content 15.5 weight %, lattice avalanche temperature is 985 ℃, degree of crystallinity is decided to be 100%, and the particle diameter of powdery NaY zeolite is the 0.4-1 micron) join in the reactor 1.Close the valve of charging aperture 2 and gas outlet 3.Turn on agitator 4, mixing speed are 80 rev/mins.Open the power supply of electrical heating cover 10, elevate the temperature to the SR74 type intelligent temperature control instrument displays temperature that links to each other with thermocouple 13 be 300 ℃, constant temperature is from air inlet 6 feeding SiCl
4Liquid 110 grams, SiCl
4Liquid gasifies, and enters reactor 1 by gas distributor 9, reacts with the NaY zeolite.Reactor 1 internal pressure maintains 6 kilograms per centimeter substantially
2, reactor 1 internal pressure is read from Pressure gauge 11.React after 5 hours, close the power supply of electrical heating cover 10, be cooled to 100 ℃.Slowly open exhaust outlet 3, waste gas is slowly discharged from gas-solid separator 5.Open discharging opening 7 and lay down gas distributor 9,, discharge solid product smoothly agitator 4 counter-rotatings.With 20 times of deionized water washing solid products,, get 690 gram Y-type high-Si zeolites 120 ℃ of oven dry to solid product, its lattice constant is 2.445 nanometers, sodium oxide content 0.4 weight %, and lattice avalanche temperature is 1010 ℃, degree of crystallinity reservation degree is 90%, and the solid yield is 99 weight %.
Example 8
This example illustrates method provided by the invention.
Charging aperture 2 from example 4 described consersion units, with 600 gram (butt weight) solid contents is 99.1% powdery rare earth Y zeolite (lattice constant 2.468 nanometers, sodium oxide content 4.5 weight %, 985 ℃ of lattice avalanche temperature, rare earth oxide content 18 weight %, wherein, lanthana content is 4.9 weight %, cerium oxide content is 9.6 weight %, and other rare earth oxide content is 3.5 weight %, and the particle diameter of powdery rare earth Y zeolite is the 0.3-1 micron) join in the reactor 1.Close the valve of charging aperture 2 and gas outlet 3.Turn on agitator 4, mixing speed are 90 rev/mins.Open the power supply of electrical heating cover 10, elevate the temperature to be positioned at reactor 1 in the middle of the SR74 type intelligent temperature control instrument displays temperature that links to each other of thermocouple 13 be 250 ℃ (at this moment, the SR74 type intelligent temperature control instrument displays temperature that links to each other with the thermocouple 13 that is positioned at reactor 1 top also is 250 ℃), constant temperature feeds SiCl from air inlet 6
4Liquid 140 grams, SiCl
4Liquid gasifies, and enters reactor 1 by gas distributor 9, reacts with Rare Earth Y.Reactor 1 internal pressure maintains 6 kilograms per centimeter substantially
2, reactor 1 internal pressure is read from Pressure gauge 11.React after 4 hours, close the power supply of electrical heating cover 10, be cooled to room temperature.Slowly open exhaust outlet 3, waste gas is slowly discharged from gas-solid separator 5.Open discharging opening 7 and lay down gas distributor 9,, discharge solid product smoothly agitator 4 counter-rotatings.With 20 times of deionized water washing solid products,, get 590 gram Y type zeolites containing rare-earth and high content of silicon 120 ℃ of oven dry to solid product.Its lattice constant 2.445 nanometers, sodium oxide content 0.32 weight %, lattice avalanche temperature is 1003 ℃, rare earth oxide content is 14.8 weight %, wherein, lanthana content is 3.5 weight %, and cerium oxide content is 7.4 weight %, other rare earth oxide content is 3.9 weight %), the solid yield is 98.3 weight %.
Claims (2)
1. the method for gas and solid particle reaction, this method comprises gas is contacted with solid particle, described contact is carried out in a consersion unit, described consersion unit comprises a reactor (1), a charging aperture (2) and a gas outlet (3), wherein, also comprise an agitator (4) in the inside of reactor (1), a gas-solid separator (5) is installed on the gas outlet (3), the bore dia of gas-solid separator (5) contained hole and porosity guarantee gas can by and solid particle can not pass through, the puddler of agitator (4) stretches out outside the reactor (1), and it is local airtight that puddler contacts with reactor (1), and reactor (1) is not in communication with the outside; The material of solid particle and gas or energy process gas is joined in the reactor (1) through charging aperture (2), under the stirring of agitator (4), described solid particle contacts with the gas that described gas maybe can generate the material generation of gas, it is characterized in that described consersion unit also comprises an air inlet (6) and discharging opening (7); Discharging opening (7) is positioned at the bottom of reactor (1), air inlet (6) communicates with reactor (1) by discharging opening (7), a dismountable gas distributor (9) is equipped with on the top of discharging opening (7), at the bottom of the still of the top and reactor (1) of gas distributor (9) in one plane or be higher than the plane at place at the bottom of reactor (1) still, the material of described gas or energy process gas adds through air inlet (6), and reacted solid draws off through discharging opening (7).
2. method according to claim 1, it is characterized in that, at the outside electrical heating cover (10) in addition of reactor (1), also have the interface (12) of a connection Pressure gauge (11) and the recess (14) that at least one heat supply galvanic couple (13) inserts on the top of reactor (1), recess (14) is not communicated with reactor (1), thermocouple (13) is connected with the instrument of energy displays temperature, with the temperature in the Indicator Reaction still (1).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4022438A (en) * | 1974-05-13 | 1977-05-10 | Mitsubishi Kasei Kogyo Kabushiki Kaisha | Stirring apparatus |
| US4372919A (en) * | 1980-03-14 | 1983-02-08 | Nippon Oil Company, Limited | Vapor phase polymerization apparatus for olefins |
| US5182087A (en) * | 1990-04-04 | 1993-01-26 | Outokumpu Oy | Method for mixing two liquids or liquid and solid material together, and for simultaneously separating another liquid or solid from the liquid |
-
2004
- 2004-03-31 CN CN 200410029864 patent/CN1676206B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4022438A (en) * | 1974-05-13 | 1977-05-10 | Mitsubishi Kasei Kogyo Kabushiki Kaisha | Stirring apparatus |
| US4372919A (en) * | 1980-03-14 | 1983-02-08 | Nippon Oil Company, Limited | Vapor phase polymerization apparatus for olefins |
| US5182087A (en) * | 1990-04-04 | 1993-01-26 | Outokumpu Oy | Method for mixing two liquids or liquid and solid material together, and for simultaneously separating another liquid or solid from the liquid |
Non-Patent Citations (2)
| Title |
|---|
| 马振杰.1.2m3多功能搅拌反应釜的研制.化工机械26 4.1999,26(4),全文. |
| 马振杰.1.2m3多功能搅拌反应釜的研制.化工机械26 4.1999,26(4),全文. * |
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