CN101884897B - Method for reacting gas and solid particles - Google Patents
Method for reacting gas and solid particles Download PDFInfo
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- CN101884897B CN101884897B CN2009101804517A CN200910180451A CN101884897B CN 101884897 B CN101884897 B CN 101884897B CN 2009101804517 A CN2009101804517 A CN 2009101804517A CN 200910180451 A CN200910180451 A CN 200910180451A CN 101884897 B CN101884897 B CN 101884897B
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a method for reacting gas and solid particles, which comprises the step of contacting the gas with the solid particles. The contact is performed in reaction equipment, and the reaction equipment comprises a reaction kettle, a feed inlet and a gas outlet. The interior of the reaction kettle also comprises a stirrer; and a gas-solid separator is arranged on the gas outlet. The pore diameter and the porosity of the pores contained in the gas-solid separator guarantee that the gas can pass the pores and the solid particle cannot pass the pores. A stirring rod of the stirrer extends out of the reaction kettle, and the contacting position of the stirring rod and the reaction kettle is sealed, so that the reaction kettle does not communicate with the outside. The solid particles and the gas or substances capable of generating gas are added into the reaction kettle through the feed inlet, and the solid particles and the gas or the gas generated by the substances capable of generating gas contact to perform the reaction of the gas and the solid particles under the stirring of the stirrer. The contact reaction of the gas and the solid particles is more uniform and the phenomenon that the solid particles are coalesced into dense blocks is avoided. Therefore, the method for reacting the gas and the solid particles can lower the labor intensity and reduce the environmental pollution, obviously reduces the production cost, and is easy for large-scale industrial application.
Description
The application be submitted on March 31st, 2004, application number is 200410029864.2, denomination of invention is divided an application for " method that a kind of gas and solid particle react " application for a patent for invention.
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; Said contact is carried out in a consersion unit; Said consersion unit is made up of a reaction tube (or being called agitated reactor) and an air inlet and a gas outlet of being positioned at the reaction tube two ends, and said 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 agitated reactor; Fill with fillers such as porcelain ring or quartz materials at two; Enrich to guarantee that solid particle is filled, be present in the stage casing of 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 through the solid particle bed time.Unreacted gas is discharged through the gas outlet with the waste gas that reaction generates.
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, be prone to 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, be prone to 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 decision of itself 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 like 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 agitated 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 from consersion unit, draw off 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, be prone to 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 like this, very big as the consumption that carries gas and reactive material that carries reactive material; Contain unreacted gas and the waste gas that reaction produces, 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 that said contact is carried out, wherein in a consersion unit; Said consersion unit comprises 1, one charging aperture 2 of an agitated reactor and a gas outlet 3, wherein; Also comprise an agitator 4 in the inside of agitated 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 through and solid particle can not pass through, the puddler of agitator 4 stretches out outside the agitated reactor 1; It is local airtight that puddler contacts with agitated reactor 1, and agitated reactor 1 is not in communication with the outside; The material of solid particle and gas or ability process gas is joined in the agitated reactor 1 through charging aperture 2, and under the stirring of agitator 4, said solid particle contacts with the gas that said gas maybe can generate the material generation of gas.。
Because comprise a stirring in the said consersion unit of method provided by the invention, solid particle under agitation evenly rolls; 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; Be prone to cause hot-spot or cold excessively shortcoming; Also make gas and solid particle haptoreaction more even, therefore, can obtain character solid particulate product more uniformly.Particularly, when solid particle is superfine powder or the nano-scale particle of diameter below 5 microns, 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, have 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 agitated 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 quantitatively add the material that maybe can form the gas that reacts with solid particle with the gas of solid particle reaction according to the consumption of solid particle, and; Need not 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 said consersion unit of method provided by the invention can leave gas and solids effectively; Waste gas after guaranteeing to react can be discharged; Even and particle diameter is less than 1 micron, even 0.3 micron solid particle from then on pipeline discharge, avoided the loss of solid particle; Reduced dust pollution, input-output ratio is improved.
Description of drawings
Accompanying drawing 1-8 is the sketch map of the said consersion unit of method provided by the invention;
Accompanying drawing 9-10 is a spiral ribbon agitator sketch map in the said consersion unit of method provided by the invention;
Accompanying drawing 11 is agitated reactor rip cutting sketch mapes of the said 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 3 is discharged with gas-solid separator 5 through the gas outlet.
The present invention has many concrete embodiments, is wherein representative example below.
First specific embodiment of the present invention is as shown in Figure 1.Said consersion unit comprises 1, one charging aperture 2 of an agitated reactor and a gas outlet 3, also has an agitator 4 in the inside of agitated 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 through and solid particle can not pass through, the puddler of agitator 4 stretches out outside the agitated reactor 1; It is local airtight that puddler contacts with agitated reactor 1, and agitated 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, 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 not reacting by heating still 1 make the said gasification substance that can generate with the gas of solid particle reaction, reaction under agitation to reaction temperature.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset agitated reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 2nd specific embodiments of the present invention is as shown in Figure 2.Said consersion unit comprises all members of first specific embodiment, in addition, also comprises an air inlet 6.Said air inlet 6 can be positioned at the optional position of agitated reactor 1, and under the preferable case, charging aperture 2 and gas outlet 3 are positioned at the top of agitated reactor 1, and air inlet 6 is positioned at the bottom of agitated 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, agitator 4 is airtight with charging aperture 2 and gas outlet 3.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 agitated reactor 1; The heating or not reacting by heating still 1 to reaction temperature; Make the said gasification substance that can generate the gas that reacts with solid particle, reaction under agitation.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset agitated reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 3rd specific embodiments of the present invention is as shown in Figure 3.Said 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 agitated reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of agitated reactor 1 still.The effect of said gas distributor is that gas can be got in the agitated reactor 1 continuously equably, simultaneously, guarantees that solid particle does not get 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, agitator 4 is airtight with charging aperture 2.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 agitated reactor 1; The heating or not reacting by heating still 1 to reaction temperature; Can generate material with the gas of solid particle reaction after gasification with the gas of solid particle reaction or said,, get into agitated reactor 1 equably and under agitation react with solid particle through the distributional effects of gas distributor 9.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.Gas-solid separator 5 can be discharged gas, and solid can not be discharged.Upset agitated reactor 1 is opened charging aperture 2, draws off reacted solid from charging aperture 2.
The 4th concrete embodiment of the present invention is as shown in Figure 4.Said 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 agitated reactor 1, and discharging opening 7 is positioned at the bottom of agitated reactor 1.Discharging opening 7 is used for drawing off reacted solid particle.Discharging opening 7 has been arranged, and the agitated 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, 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 not reacting by heating still 1 make the said gasification substance that can generate with the gas of solid particle reaction, reaction under agitation to reaction temperature.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.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 concrete embodiment of the present invention is as shown in Figure 5.Said 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 makes the solid particle can not be through in the pipeline that aperture gets into discharging opening 7 links to each other, at the bottom of the still of the upper surface of dish 8 and agitated reactor 1 in one plane or be higher than the plane that belongs at the bottom of agitated reactor 1 still.Said dish 8 guarantees that solid particle does not get 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, 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 not reacting by heating still 1 make the said gasification substance that can generate with the gas of solid particle reaction, reaction under agitation to reaction temperature.Because the existence of dish 8, in the course of reaction, solid particle can not get into the pipeline that links to each other with discharging opening.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.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 6th concrete embodiment of the present invention is as shown in Figure 6.Said 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 agitated reactor 1, and air inlet 6 and discharging opening 7 are positioned at the bottom of agitated 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 agitated reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of agitated 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 makes the solid particle can not be through in the pipeline that aperture gets into discharging opening 7 links to each other, at the bottom of the still of the upper surface of dish 8 and agitated reactor 1 in one plane or be higher than the plane that belongs at the bottom of agitated reactor 1 still.Said distributor 9 plays the effect of gas distributor, and gas can be got in the agitated reactor 1 continuously equably, simultaneously, guarantees that solid particle does not get in the pipeline that links to each other with air inlet 6.Said dish 8 guarantees that solid particle does not get 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; Agitator 4 adds gas with the solid particle reaction from air inlet 6 and maybe can generate the material with the gas of solid particle reaction, and pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the agitated reactor 1; The heating or not reacting by heating still 1 to reaction temperature; Can generate material with the gas of solid particle reaction after gasification with the gas of solid particle reaction or said,, get into agitated reactor 1 equably and under agitation react with solid particle through the distributional effects of distributor 9.Because the existence of dish 8, in the course of reaction, solid particle can not get into the pipeline that links to each other with discharging opening.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out Gas Recovery.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 concrete embodiment of the present invention is as shown in Figure 7.Said 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 agitated reactor 1; Air inlet 6 communicates with agitated reactor 1 through 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 agitated reactor 1 of gas distributor 9 in one plane or be higher than the plane at place at the bottom of agitated reactor 1 still.Said gas distributor 9; Both played the effect of gas distributor, gas can evenly be got in the agitated reactor 1, guaranteed again that solid particle did not get 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; Agitator 4 adds gas with the solid particle reaction from air inlet 6 and maybe can generate the material with the gas of solid particle reaction, and pressure air inlet 6 is airtight or that keep air inlet 6 places is not less than the pressure in the agitated reactor 1; The heating or not reacting by heating still 1 to reaction temperature; Can generate material with the gas of solid particle reaction after gasification with the gas of solid particle reaction or said,, get into agitated reactor 1 equably and under agitation react with solid particle through the distributional effects of gas distributor 9.Because the existence of gas distributor 9, in the course of reaction, solid particle can not get into the pipeline that links to each other with discharging opening.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.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 concrete embodiment of the present invention is as shown in Figure 8.Said consersion unit comprises the 7th all members of the specific embodiment; In addition; At agitated reactor 1 outside electrical heating cover 10 in addition, comprise the interface 12 of a connection Pressure gauge 11 and the recess 14 of at least one heat supply galvanic couple 13 insertion on the top of agitated reactor 1, recess 14 is not communicated with agitated 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.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 agitated reactor 1; Start the power supply of electrical heating cover 10, agitated reactor 1 is heated to required temperature, can generate material with the gas of solid particle reaction after gasification with the gas of solid particle reaction or said; Through the distributional effects of gas distributor 9, get into agitated reactor 1 equably and under agitation react with solid particle.Pressure and temperature in the agitated 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 get into the pipeline that links to each other with discharging opening.Reaction is closed agitator 4 after accomplishing, and stops to stir, and cools off or does not cool off, and opens gas outlet 3, and waste gas is discharged, and carries out waste gas and reclaims.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, said agitated reactor 1 can be a shape arbitrarily, is oval-shaped column, coniform, square like cylindric, spherical, cross section, cuboid or other irregular shape.For solid particle is mixed more evenly and easy-unloading, under the preferable case, said agitated reactor 1 is the cylindric of following band cone cylindric, spherical, coniform or shown in figure 11.
Agitated reactor 1 can adopt various material preparations according to the kind of gas that reacts and solid.Like various metal materials, nonmetallic materials and alloy material, particularly stainless steel, the alloy of the alloy of the alloy of aluminium, aluminium alloy, iron, cast iron, iron content, titanium, titaniferous, copper, cupric, the alloy that contains chromium, nickeliferous alloy, pottery etc.
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 agitated reactor 1.Said 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 the support bar 17 that links to each other with 16, 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 of horizontal plane is the 10-70 degree, preferred 20-60 degree.The width of ribbon changes in very significantly according to the size of agitated 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 the agitator that in industry, uses; 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 agitated reactor 1, and for fear of the collision of recess 14 with agitator 4, the stirring of said agitator 4 can be divided into shown in figure 10 at least 2 sections with 16, and stir between the band at 2 sections the position of recess 14.Adopt such agitator, when direction is rotated, easily material is risen to the top from the bottom of agitated reactor 1 at agitator; Solid particle can successfully prolong the stirring band and slide, and stirs, and makes gas and solid particle even contact; Avoid material to form the hole, center, lean on wall to form the phenomenon in duricrust district, can solve the solid material defective slow, the mass transfer difference of conducting heat better; 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, said gas-solid separator is a kind of porous material, the bore dia of said porous material contained hole and porosity guarantee gas can through and solid particle can not pass through.The bore dia of said porous material and porosity design according to the solid particle size of the reaction of participating in gas and solid particle; As when the solid particle diameter is the 0.1-5 micron; The bore dia of said porous material contained hole is the 1-40 micron; Preferred 5-20 micron, porosity is 5-60%, is preferably 10-40%.Said 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 agitated reactor 1 agitated reactor 1 can only be in communication with the outside through gas-solid separator 5; This can be through covering gas-solid separator 5 on the gas outlet 3 of agitated reactor 1, and airtight the reaching of part that gas-solid separator 5 is contacted with agitated reactor 1.
Said 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 of participating in reaction, and when being the 0.1-5 micron like 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 makes the solid particle can not be through in the pipeline that aperture gets into discharging opening 7 links to each other on the dish 8; The size of aperture is decided according to the size of the solid particle of participating in reaction; When being the 0.1-5 micron like 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.
A kind of heater that described electrical heating cover 10 just can adopt, said heating jacket can be used the mode of heating of any equivalence, as adopts direct naked light heating, and modes such as water-bath heating, oil bath heating replace.
The material of the gas of ability generation and solid particle reaction refers to the solid or the liquid of the gas that any ability generation and solid particle react.When the material that can generate the gas that reacts with solid particle is solid, can join in the agitated reactor 1 with said 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 agitated reactor 1 with said solid particle from charging aperture 2, also can and preferably join the agitated 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.Superfine powder solid particle and the nanoscale solids particle and the gas that are particularly suitable for particle diameter and are below 5 microns react.
Following instance will further specify the present invention.
This instance is explained the said consersion unit of method provided by the invention.
Using thickness is that 3 millimeters the industrial trade mark is processed equipment as shown in Figure 8 as the stainless steel of NiCr18Ti.Away from the port of agitated reactor 1 valve has been installed at charging aperture 2, gas outlet 3, air inlet 6 and discharging opening 7.
Wherein, the kettle of agitated 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-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 processed 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 agitated reactor 1 adopts the spiral shell button airtight.
This instance is explained the said consersion unit of method provided by the invention.
Using thickness is that 3 millimeters the industrial trade mark is prepared equipment as shown in Figure 1 as the steel alloy of 0Cr18Ni10Ti.Agitated 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 processed.The position of gas-solid separator 5 and agitated reactor contact adopts that flange is airtight to be connected.
This instance is explained the said consersion unit of method provided by the invention.
Using thickness is that 4 millimeters the industrial trade mark is prepared equipment as shown in Figure 8 as the steel alloy of 0Cr18Ni9.Away from the port of agitated reactor 1 valve has been installed at charging aperture 2, gas outlet 3, air inlet 6 and discharging opening 7.
Wherein, the kettle of agitated reactor 1 is the cylinder of the cone of band down shown in figure 11, 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.
Agitator 4 is 2 segmentation spiral ribbon agitators shown in Figure 10.Puddler 15, stir be with 16 and support bar 17 all process with stainless steel.12 millimeters of puddler 15 diameters, said spiral begins from the bottom of puddler 15, and the height of top spiral is 100 millimeters; Diameter is 90 millimeters, and the height of bottom hurricane band is 215 millimeters, and the distance between 2 hurricane bands is 10 millimeters; Wherein, the height of the bottom spiral that the agitated reactor cone is above is 140 millimeters, and diameter is 90 millimeters; In the agitated 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 agitated reactor 1; The length that puddler 15 stretches out agitated reactor 1 exterior portions is 20 millimeters; Puddler 15 links to each other with motor; Stirring is 30 degree with the angle of 16 plane and horizontal plane, and the width that stirs with 16 is 10 millimeters, 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 agitated reactor contact adopts that flange is airtight to be connected.
This instance is explained the said consersion unit of method provided by the invention.
Except that agitator 4 for climbing the formula agitator, other material equipment is all identical with instance 1.When the said formula agitator 4 of climbing when rotating, stirring band, to rotate formed columniform diameter be 90 millimeters.
This instance is explained method provided by the invention.
From the charging aperture 2 of instance 1 said consersion unit, be 99% powdery rare earth Y zeolite (lattice constant 2.468 nanometers, sodium oxide content 4.5 weight % with 800 gram (butt weight) solid contents; 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 agitated 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 agitated 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 agitated reactor 1 top also is 280 ℃); Constant temperature feeds SiCl from air inlet 6
4Liquid 130 grams, SiCl
4Gasification is also passed through gas distributor 9 entering agitated reactors 1, reacts with Rare Earth Y.Agitated reactor 1 internal pressure maintains 4 kilograms per centimeter basically
2, agitated 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 wash solids products,, get 790 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 1020 ℃; Rare earth oxide content is 14.5 weight %, and 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.
This instance is explained method provided by the invention.
From the charging aperture 2 of instance 2 said consersion units, be 99% powdery rare earth sodium Y zeolite (lattice constant 2.470 nanometers, sodium oxide content 5 weight % with 1000 gram (butt weight) solid contents; 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 agitated 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 agitated reactor 1 is immersed temperature, reacts 5 hours, and agitated 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 agitated reactor 1, upset agitated reactor 1 is opened charging aperture 2, and solid product is drawn off.With 20 times of deionized water wash solids products,, get 990 gram Y type zeolites containing rare-earth and high content of silicon 120 ℃ of oven dry to solid product; Its lattice constant is 2.456 nanometers, sodium oxide content 0.45 weight %, and lattice avalanche temperature is 1010 ℃; Rare earth oxide content is 12.5 weight %, and 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 %.
This instance is explained method provided by the invention.
Charging aperture 2 from instance 3 said 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 ℃, and 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 agitated 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
4The liquid gasification, and through gas distributor 9 entering agitated reactors 1, react with the NaY zeolite.Agitated reactor 1 internal pressure maintains 6 kilograms per centimeter basically
2, agitated 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 wash solids 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 %.
This instance is explained method provided by the invention.
From the charging aperture 2 of instance 4 said consersion units, be 99.1% powdery rare earth Y zeolite (lattice constant 2.468 nanometers, sodium oxide content 4.5 weight % with 600 gram (butt weight) solid contents; 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 agitated 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 agitated 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 agitated reactor 1 top also is 250 ℃); Constant temperature feeds SiCl from air inlet 6
4Liquid 140 grams, SiCl
4The liquid gasification, and through gas distributor 9 entering agitated reactors 1, react with Rare Earth Y.Agitated reactor 1 internal pressure maintains 6 kilograms per centimeter basically
2, agitated 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 wash solids 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 comprise gas are contacted with solid particle that said contact is carried out in a consersion unit; Said consersion unit comprises an agitated reactor (1), a charging aperture (2) and a gas outlet (3), wherein; Also comprise an agitator (4) in the inside of agitated 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 through and solid particle can not pass through, the puddler of agitator (4) stretches out outside the agitated reactor (1); It is local airtight that puddler contacts with agitated reactor (1), and agitated reactor (1) is not in communication with the outside; The material of solid particle and gas or ability process gas is joined in the agitated reactor (1) through charging aperture (2), and under the stirring of agitator (4), said solid particle contacts with the gas that said gas maybe can generate the material generation of gas; It is characterized in that said agitator (4) is the spiral ribbon agitator, this agitator comprises a puddler (15); Stir the support bar (17) of being with (16) and two ends to link to each other with puddler (15) and stirring band (16); Stirring band (16) is the axle center with puddler (15), spiral escalation or decline, and stirring the plane of band (16) and the angle of horizontal plane is the 10-70 degree; Wherein, the stirring band (16) of said agitator (4) is divided at least 2 sections.
2. method according to claim 1 is characterized in that, stirring the plane of band (16) and the angle of horizontal plane is the 20-60 degree.
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Citations (5)
| 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 |
| CN1378562A (en) * | 1999-10-06 | 2002-11-06 | 巴塞尔聚烯烃有限公司 | Gas phase polymerization method |
| CN1448211A (en) * | 2002-03-29 | 2003-10-15 | 中国石油化工股份有限公司 | Gas-solid reactor |
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- 2004-03-31 CN CN2009101804517A patent/CN101884897B/en not_active Expired - Lifetime
Patent Citations (5)
| 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 |
| CN1378562A (en) * | 1999-10-06 | 2002-11-06 | 巴塞尔聚烯烃有限公司 | Gas phase polymerization method |
| CN1448211A (en) * | 2002-03-29 | 2003-10-15 | 中国石油化工股份有限公司 | Gas-solid reactor |
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