CN105621658B - A kind of Application way of sulfur transfer additive and FCC catalyst production fine powder and waste water - Google Patents
A kind of Application way of sulfur transfer additive and FCC catalyst production fine powder and waste water Download PDFInfo
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Abstract
The invention discloses a kind of sulfur transfer additive and the Application way of FCC catalyst production fine powder and waste water, FCC catalyst production waste water is first carried out solid-liquid pre-separation processing by this method, pre-separation clear liquid and pre-separation heavy phase and/or sediment are obtained, pre-separation heavy phase and/or sediment are sent into the colloid generating kettle of production FCC catalyst after levigate processing；The production waste water for pre-processing clear liquid and sulfur transfer additive is mixed, after adding sulfur transfer additive fine powder, control ph, two-stage separating treatment, obtained separation clear liquid is sent into reuse in sulfur transfer additive production process, and obtained heavy phase and/or sediment are sent into after levigate processing in the colloid generating kettle of production sulfur transfer additive.The present invention can be reused the rare earth element and solid particulate matter dissolved in auxiliary agent fine powder and waste water, not only recycle resource, but also reduce environmental pollution.
Description
Technical field
The present invention relates to a kind of sulfur transfer additive and the Application way of FCC catalyst production fine powder and waste water.
Background technology
During fluid catalytic cracking (FCC), the Rapid contact in riser carries out catalytic cracking to feedstock oil with catalyst
Reaction, reacts the coke laydown of generation and its inactivation is caused to catalyst, the catalyst of green coke inactivation enters regeneration after stripping
Device carries out coke burning regeneration.In regenerative process, the selective oxidation of sulfur containing compounds in particular being deposited in coke generates SOx, is discharged with regenerated flue gas
Environmental pollution is caused into air.
The use of flue gas SOx transferring assistants (also referred to as sulfur transferring assistant or sulfur transfer additive) is control FCC apparatus regenerated flue gas SOx
The technical measures of discharge.Its action principle is to trap what is generated in flue gas by metal active constituent in a regenerator
SOx, forms stable metal sulfate, then enters riser reactor, under reducing atmosphere, metal sulfate with regenerator
It is reduced, with H2S-shaped formula enters in gaseous product, is recycled by sulfur recovery facility.Sulfur transfer additive with respect to wet scrubbing etc. other
Flue gas SOx treatment technologies are excellent with operating flexible and convenient, being not required to plant modification and equipment investment and not producing secondary pollution etc.
Point, common concern and application are obtained in refinery.Therefore, sulfur transfer additive has become the important auxiliary agent kind of catalyst plant.
The chemical composition of sulfur transfer additive has significant difference with FCC catalyst, in the prior art disclosed sulfur transfer additive composition
And preparation method thereof can be found in US4497902, US4768235, CN1485132A, CN100425339C, CN101185829A etc..
For example, sulfur transfer additive disclosed in CN1485132A is using the oxide of the cerium of 2-30 weight % as active component, with 70-98 weight %
Composition containing magnesium aluminate spinel be carrier, also contain 0-15 weight %, preferably 0.5- in the composition containing magnesium aluminate spinel
The rare earth element in addition to Ce of 10 weight % and the V of 0-10 weight %, preferably 0.5-5 weight %2O5.Rare earth element is especially
CeO2It is the important active component of sulfur transfer additive, is carried on using the dipping method (excessive to impregnate) of maceration extract volume excess
On carrier, relatively isometric saturation dipping method can improve CeO2Scattered uniformity, improves the sulphur transfer efficiency of auxiliary agent.But
The method excessively impregnated can produce a large amount of filtrate waste water, and the method production sulphur provided by CN1485132A, CN100425339C turns
Agent is moved, rare earth element ce is loaded in the microspheroidal support after spray-dried shaping and roasting using the method excessively impregnated,
Since Ce generally can not be completely by carrier adsorption, the Ce not being fully utilized causes CeO in filtrate waste water with filtrate discharge2Contain
Sometimes up to 20 g/l of amount.In addition, in filter process, a small amount of builder granule be particularly some fine graineds can pass through filter cloth into
Enter in waste water, also result in containing 5-25 g/l of solid particulate matter in waste water, thus waste water is thick suspended in mud color in appearance
Liquid.
Because sulfur transfer additive contains the metal component of a variety of FCC catalysts easy to pollute, its production waste water cannot be back to use FCC and urge
In agent production.Even if by waste water recycling to sulfur transfer additive itself production procedure, if without processing direct-on-line circulation profit
With there is also problems with：(1) rare earth maceration extract is prepared if be back to, wherein fine particle and the rare earth flocculation contained
Precipitation constantly accumulation, causes filter cloth mesh gradually to block, filter efficiency is greatly reduced；(2) if be back to use during plastic,
When colloid is sprayed and is shaped, contained solid particulate matter not only spray drying tower atomizer easy to wear, but also with colloid adhesion
Cause builder granule sphericity poor, influence abrasion resistance properties.Recycled due to online there are problem, thus sulfur transfer additive is given birth to
Waste water of the outer row containing rare earth and builder granule thing is needed during production, not only causes resources loss, but also after being mixed with other waste water
Cause sewage disposal difficulty to increase, easily lead to problem of environmental pollution.
Although sulfur transferring assistant production waste water needs to pay special attention to because of the reason such as its rare earth element and fine particle content height,
But actually it is that oil refining catalyst factory largely produces a part in waste water.As well known to the researcher of this area, FCC catalysis
Agent is the most important catalizer variety of oil refining catalyst factory, and substantial amounts of exchange washing water is equally produced in FCC catalyst production
And other sewage.Wherein, the exchange washing water dosage maximum washed during sodium is exchanged for catalyst, it is filtered to consolidate with catalyst
A large amount of filtrates are produced after liquid separation.These filtrate waste water are in acidity, except containing sodium ion, ammonia nitrogen and solid particle beyond the region of objective existence, also containing
There is the rare earth element being lost in from catalyst, although its concentration is relatively low, be lost in since washing water consumption is larger, thus with filtrate
Rare earth resources total amount is higher.Due to that, dissolved with the sodium ion to the toxic effect of FCC catalyst, can not be recycled to be used in washings
In Cracking catalyst production.To reduce the consumption of water in Catalyst Production, sewage discharge is reduced, the prior art mainly adopts filter
The method that liquid waste water is segmented reuse step by step, for molecular sieve production or catalyst cake elution.But due to containing in filtrate waste water
Sodium ion, rare earth ion, solid particulate matter and other impurity etc., may be to molecular sieve and catalyst prod quality during reuse
Have some impact on.Therefore, if having new processing and can shunt portion filtrate waste water using technology, waste water can on the one hand be reduced
Outer row, on the other hand, the use ratio of fresh water is improved in molecular sieve and Catalyst Production, is conducive to stable prod matter
Amount.
In addition, in sulfur transfer additive production process, it is similar with conventional FCC catalyst production process, produced in spray-drying process
First portion fine powder, these fine powders are easily less easily entrained by effusion and cause loss of material or granular material discharged pollution, thus need in life
The different phase of production flow is recycled using modes such as cyclone separators.Fine powder before fired can be back to use in colloid generating kettle to be beaten again
Slurry is scattered or feeds back to roaster, but the fine powder reuse after roaster is there are some problems, if being back to use plastic
During, then, can be to spray drying tower atomizer and auxiliary agent sphericity and wear-resisting such as the solid particulate matter in above-mentioned waste water
Damage performance adversely affects；Directly it is blended into catalyst or Additives Products, then product fine powder content may be caused to exceed matter
Figureofmerit requirement.
The above-mentioned prior art (US4497902, US4768235, CN1485132A, CN100425339C,
CN101185829A) although in disclose composition of a variety of different sulfur transfer additives and preparation method thereof, be not directed to auxiliary agent fine powder
And the reuse problem of production waste water, especially it is not directed to that auxiliary agent fine powder and waste water are carried out at the same time to handle to recycle online to realize
The problem of.
CN203392959U discloses a kind of separator of dead catalyst in flue gas desulfurization waste-water, mainly for separating of
Dead catalyst in FCC regenerated flue gas wet scrubbing device waste water.Waste water enters cyclone hydraulic separators, and top catalyst content is low
Thin liquid is recycled back into chilling tower, and laggard dewaterer is mixed with flocculant in the material after bottom is concentrated rich in catalyst granules
Separated.The separator is mainly used for removing the spent catalyst particles in regenerated flue gas wet scrubbing device, the production of sewage
Raw process, component characteristic and sulfur transfer additive and FCC catalyst production waste water has significant difference.And solid-liquid separation efficiency is not high enough,
Need the materials such as additional flocculating agents.
CN100429157C discloses the high-concentration ammonia nitrogen waste water treatment method produced in a kind of oil refining catalyst production, main
Want step to include adjusting pH value of waste water, the suspended matter in waste water and the sial ion and its chemical combination of dissolving are removed through separation of solid and liquid
Thing；Calcium ion generation calcium sulfate precipitation is added, the acidic materials in waste water are reduced through separation of solid and liquid；Add carbanion generation
Precipitation of calcium carbonate, the calcium ion in waste water is removed through separation of solid and liquid；Then through stripping deamination and biochemical treatment, waste water is made to reach state
Family's discharge standard.The goal of the invention of this method is, is combined by the methods of chemical precipitation and stripping ammonia nitrogen removal to catalyst
Wastewater purification is produced, makes discharged wastewater met the national standard.But the processing method primarily focuses on removal of ammonia and nitrogen, suspended particulate substance etc.
Aspect, needs the materials such as additional flocculating agents, chemical precipitation agent, and operation is relative complex, and does not consider the reuse of contained rare earth resources.
Currently, as the requirement to catalyst plant stabilized product quality, energy-saving and emission-reduction etc. is continuously improved, enterprise is urgent
Need to further improve the processing of production fine powder and waste water and using technical merit, thus be necessary that developing more effective sulphur turns
Move agent and the recycle utilization of FCC catalyst production fine powder and waste water.
The content of the invention
, should the object of the present invention is to provide a kind of sulfur transfer additive and the Application way of FCC catalyst production fine powder and waste water
Method is by using the pretreatment of containing wastewater from catalyst pre-separation, auxiliary agent fine powder to composite waste, two-stage separation of solid and liquid and separation weight
The levigate processing of phase and/or sediment, can be back to use online by fine powder and with the rare earth element and solid particulate matter discharged in waste water
In production procedure, and product quality and production procedure are not adversely affected.
To achieve these goals, the present invention provides a kind of profit of sulfur transfer additive and FCC catalyst production fine powder and waste water
With method, this method includes：FCC catalyst production waste water is first subjected to solid-liquid pre-separation processing, pre-separation clear liquid is obtained and contains
The pre-separation heavy phase and/or sediment of solid particulate matter；The pre-separation heavy phase and/or sediment are subjected to levigate processing, obtained pre-
Separate levigate processing heavy phase and/or sediment, the average grain of solid particulate matter in processing heavy phase that the pre-separation is levigate and/or sediment
Footpath is less than 4.5 microns；The levigate processing heavy phase of the pre-separation and/or sediment are sent to reuse in FCC catalyst colloid generating kettle；With body
Product meter, 1 part of sulfur transfer additive production waste water is mixed with 0.2-5 parts of the pre-separation clear liquid, sulfur transfer additive is obtained and FCC is urged
Agent mixture manufacturing waste water；Using sulfur transfer additive fine powder as helping sedimentation agent to be added in the mixture manufacturing waste water, mixed
Suspension；On the basis of the volume of the mixture manufacturing waste water, the addition of the sulfur transfer additive fine powder is 1-15 g/l；Will
The pH value of the mixing suspension is controlled in 2-6；The mixing suspension that the pH value is 2-6 is subjected to level-one solid-liquid separation treatment,
Obtain level-one clear liquid and level-one heavy phase and/or sediment containing solid particulate matter；The level-one clear liquid is subjected to two level separation of solid and liquid
Processing, obtains two level clear liquid and two level heavy phase and/or sediment containing solid particulate matter；Then the two level clear liquid is conveyed again
Recycled into the production process of sulfur transfer additive, by the two level heavy phase and/or sediment and the level-one heavy phase and/or
Levigate processing is carried out after sediment mixing, obtains the levigate processing heavy phase of sulfur transfer additive and/or sediment, the levigate processing of sulfur transfer additive
The average grain diameter of solid particulate matter is less than 4.5 microns in heavy phase and/or sediment；By the sulfur transfer additive it is levigate processing heavy phase and/
Or sediment is sent to reuse in the auxiliary agent colloid generating kettle in sulfur transfer additive production process.
Preferably, wherein, the pH value of the FCC catalyst production waste water is 3.5-5, contains the 0.2- in terms of oxide weight
1.5 g/l of rare earth element, with 0.5-10 g/l of solid particulate matter of dry basis；Wherein, in terms of oxide weight, institute
The content for stating Ce in FCC catalyst production waste water is not less than the 20% of whole rare earth element contents.
Preferably, wherein, the pH value of sulfur transfer additive production waste water is 5-8, containing 1-20 grams in terms of oxide weight/
The rare earth element risen, with 2-25 g/l of solid particulate matter of dry basis.
Preferably, wherein, the sulfur transfer additive fine powder is the fine powder produced in sulfur transfer additive production process, which puts down
Equal particle diameter is 2-20 microns.
Preferably, wherein, first by the sulfur transfer additive fine powder 450-800 DEG C roast 0.5-4 it is small when after be re-used as helping it is heavy
Depressant prescription is added in sulfur transfer additive and FCC catalyst the mixture manufacturing waste water.
Preferably, wherein, the pH value of the mixing suspension is controlled in 3-5.
Preferably, wherein, the pH value of the mixing suspension is controlled by adding hydrochloric acid.
Preferably, wherein, the solid-liquid pre-separation is carried out by using subsider, filter or cyclone hydraulic separators and is handled
And/or level-one solid-liquid separation treatment.
Preferably, wherein, the two level solid-liquid separation treatment is carried out by using centrifugal separator.
Preferably, wherein, the two level clear liquid is transported to rare earth material-compound tank in sulfur transfer additive production process, auxiliary agent into
Recycled in glue kettle and/or carrier impregnation tank.
Preferably, wherein, the FCC catalyst fine powder, molecule are first added in the pre-separation heavy phase and/or sediment
At least one of sieve, aluminium oxide and kaolin, obtain pre-separation mixing heavy phase and/or sediment；The pre-separation is mixed into weight
Mutually and/or sediment carries out levigate processing, obtains the levigate processing mixing heavy phase of pre-separation and/or sediment, the levigate place of pre-separation
The average grain diameter of solid particulate matter is less than 4.5 microns in reason mixing heavy phase and/or sediment；By the levigate processing mixing of the pre-separation
Heavy phase and/or sediment are sent to reuse in FCC catalyst colloid generating kettle；Wherein, with dry basis, the pre-separation heavy phase and/or
The weight of sediment is the 0.1~10 of the weight of at least one of FCC catalyst fine powder, molecular sieve, aluminium oxide and the kaolin
Times.
Preferably, wherein, added after the two level heavy phase and/or sediment are mixed with the level-one heavy phase and/or sediment
Sulfur transfer additive fine powder and/or aluminium oxide, obtain sulfur transfer additive mixing heavy phase and/or sediment；Then sulfur transfer additive is mixed into heavy phase
And/or after sediment carries out levigate processing, obtain the levigate processing mixing heavy phase of sulfur transfer additive and/or sediment, the sulfur transfer additive mill
The average grain diameter of solid particulate matter is less than 4.5 microns in thin processing mixing heavy phase and/or sediment；By the levigate place of the sulfur transfer additive
Reason mixing heavy phase and/or sediment are sent to reuse in sulfur transfer additive colloid generating kettle；Wherein, with dry basis, the two level heavy phase and/
Or sediment and the level-one heavy phase and/or the gross weight of sediment be the sulfur transfer additive fine powder and/or alumina weight 0.1~
10 times.
Preferably, wherein, carried out using the levigate processing unit of at least one of cutter, ball mill and sand mill described in
Levigate processing, the time of levigate processing is 5-60 minutes.
Preferably, wherein, the FCC catalyst fine powder is the fine powder produced in FCC catalyst production process, the fine powder
Average grain diameter is 2-20 microns.
The Application way of sulfur transfer additive and FCC catalyst production fine powder and waste water provided by the invention, FCC catalyst production
Waste water is mixed with sulfur transfer additive production waste water after solid-liquid pre-separation, before separating treatment is carried out to composite waste, turned using sulphur
The fine powder that produces is moved in prepared by agent as helping sedimentation agent to pre-process waste water, the auxiliary agent fine powder for being used as helping sedimentation agent to
Fired processing before being added in waste water, with reference to acid control pH is added, can significantly reduce waste water solid separating difficulty, then pass through two
Fine particle in level separation of solid and liquid efficient removal waste water, realizes that the online recycling of waste water rare earth elements utilizes.Since sulphur turns
Move in agent composition and contain substantial amounts of alkaline-earth metal and heavy metal, thus, the sodium ion in FCC catalyst production waste water is back to sulphur
The performance of sulfur transfer additive will not be adversely affected in transfer agent production.Catalyst production waste water pre-separation obtains pre-
Heavy phase and/or sediment are separated, other catalyst fines can be added, after levigate processing, FCC catalyst colloid generating kettle is transported to and returns
With.In addition the separation heavy phase and/or sediment based on solid particulate matter that composite waste is obtained through two-stage separation of solid and liquid, can add
Auxiliary agent fine powder, after levigate processing, be transported to auxiliary agent colloid generating kettle reuse.The wastewater recycling method is not to product quality
Adversely affected with production procedure particularly filter filter efficiency.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Attached drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the flow according to a kind of circulation utilization method of the sulfur transfer additive production waste water of embodiment of the present invention
Schematic diagram.
Embodiment
The embodiment of the present invention is described in detail below in conjunction with attached drawing.It should be appreciated that this place is retouched
The embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The present invention provides a kind of Application way of sulfur transfer additive and FCC catalyst production fine powder and waste water, and this method includes：
FCC catalyst production waste water is first subjected to solid-liquid pre-separation processing, obtains pre-separation clear liquid and the pre-separation containing solid particulate matter
Heavy phase and/or sediment；The pre-separation heavy phase and/or sediment are subjected to levigate processing, obtain the levigate processing heavy phase of pre-separation and/
Or sediment, the pre-separation is levigate to handle the average grain diameter of solid particulate matter in heavy phase and/or sediment less than 4.5 microns；By institute
State the levigate processing heavy phase of pre-separation and/or sediment is sent to reuse in FCC catalyst colloid generating kettle；By volume, 1 part of sulphur is shifted
Agent production waste water is mixed with 0.2-5 parts of the pre-separation clear liquid, obtains sulfur transfer additive and FCC catalyst mixture manufacturing waste water；
Using sulfur transfer additive fine powder as helping sedimentation agent to be added in the mixture manufacturing waste water, mixing suspension is obtained；With the mixing
On the basis of the volume for producing waste water, the addition of the sulfur transfer additive fine powder is 1-15 g/l；By the pH of the mixing suspension
Value control is in 2-6；The mixing suspension that the pH value is 2-6 is subjected to level-one solid-liquid separation treatment, obtains level-one clear liquid and containing solid
The level-one heavy phase and/or sediment of body particulate matter；By the level-one clear liquid carry out two level solid-liquid separation treatment, obtain two level clear liquid and
Two level heavy phase and/or sediment containing solid particulate matter；Then the two level clear liquid is transported to the production of sulfur transfer additive again
Recycled, carried out after the two level heavy phase and/or sediment are mixed with the level-one heavy phase and/or sediment levigate in journey
Processing, obtains the levigate processing heavy phase of sulfur transfer additive and/or sediment, and the sulfur transfer additive is levigate to be handled in heavy phase and/or sediment admittedly
The average grain diameter of body particulate matter is less than 4.5 microns；The levigate processing heavy phase of the sulfur transfer additive and/or sediment are sent to sulfur transfer additive
Reuse in auxiliary agent colloid generating kettle in production process.
The FCC catalyst that FCC catalyst production waste water of the present invention can come from FCC catalyst production process exchanges
The filtrate of the filtered generation of slurries or a part for filtrate are washed, the other processes that can be from FCC catalyst production are produced
Raw waste water, this is well known to those skilled in the art.Wherein, the pH value of the FCC catalyst production waste water can be 3.5-
5, with oxide (RE2O3) weight meter rare earth element total content can be 0.2-1.5 g/l, with the solid of dry basis
The content of particulate matter can be 0.5-10 g/l, and the average grain diameter of solid particulate matter can be 3-8 microns, with oxide
(RE2O3) weight meter, the content of Ce is not less than the 20% of whole rare earth element contents in FCC catalyst production waste water.It is described
The zwitterions such as sodium ion, ammonium ion, chlorion can also be contained in waste water.
The preparation method of sulfur transfer additive be usually first using as carrier material containing magnesium hydroxide, magnesia, aluminium oxide, viscous
It by spray drying forming is the carrier microballoons particle similar to catalytic cracking catalyst after plastic that soil, which is waited in colloid generating kettle, will be carried
Body microsphere particle carries out calcination process, then by impregnating the active component of the main rare earth element such as including cerium in impregnating autoclave
Load on carrier, be then dried.According to the present invention, the sulfur transfer additive production waste water can be that sulfur transfer additive produced
All waste water produced in journey, such as waste water caused by dipping, wherein, the pH value of the waste water is about in 5-8 or so, generally
Containing with oxide (RE2O3) 1-20 g/l of weight meter rare earth element, the rare earth element in the waste water, such as Ce can be with
Exist with ionic state, can also exist with sediment state, and also contain the solid particle with 2-25 g/l of dry basis
Thing, the average grain diameter of the solid particulate matter have the composition same or like with sulfur transfer additive in 3-8 microns.
According to the present invention, based on wastewater volume, the sulfur transfer additive production waste water is with FCC catalyst production waste water is divided in advance
It can be not less than 0.2 from the pre-separation clear liquid mixed proportion obtained after processing:1, it is preferably 0.2:1-5:1, more preferably
0.5:1-5:1。
According to the present invention it is possible to using sulfur transfer additive fine powder as helping, sedimentation agent is added to sulfur transfer additive and FCC catalyst mixes
In symphysis production waste water, waste water is pre-processed.The sulfur transfer additive fine powder can come from the finished product of sulfur transfer additive production process
Collector unit, for example, can come from the fines collection unit of airstream drying tower, can be from spray drying tower, finished product bag
The fine powder that charging hopper etc. is collected, is preferred from the fine powder of airstream drying tower, finished product packing feed bin etc. collection.The sulphur transfer
The average grain diameter of agent fine powder can be preferably 5-15 microns in 2-20 microns.The sulfur transfer additive fine powder can be first
450-800 DEG C roast 0.5-4 it is small when, more preferably 550-750 DEG C roast 1-2 it is small when after be re-used as helping sedimentation agent to be added to sulphur
In transfer agent and FCC catalyst mixture manufacturing waste water.On the basis of the volume of the production waste water, the sulfur transfer additive fine powder
Addition is 1-15 g/l, is preferably 2-10 g/l.
According to the present invention, in order to be conducive to follow-up separation of solid and liquid, will can add described in the sulfur transfer additive fine powder
The pH value for the mixing suspension that mixture manufacturing waste water obtains is controlled in 2-6, is preferably controlled in 3-5, the acid used in control ph does not have
There is special limitation, preferably using hydrochloric acid.
According to the present invention, the solid-liquid pre-separation processing, separator used in firsts and seconds solid-liquid separation treatment
It is well-known to those skilled in the art, for example, can be carried out by using subsider, filter or cyclone hydraulic separators described solid
Liquid pretreatment separation and/or level-one solid-liquid separation treatment.Preferably, the solid-liquid can be carried out by filter-press type filter in advance to divide
From processing, the pressure of the filter-press type filter is generally in 0.2-1.0MPa, preferably 0.4-0.8MPa.Filter-press type mistake can be passed through
Filter or cyclone hydraulic separators carry out the level-one solid-liquid separation treatment, further, it is preferable to described in being carried out using cyclone hydraulic separators
Level-one solid-liquid separation treatment, the inlet pressure of cyclone hydraulic separators is 0.1-0.5MPa, is preferably 0.2-0.4MPa, underflow and overflow
Volume flow ratio can be controlled 1:5-1:20, it is preferably 1:8-1:15.Described in being carried out by using centrifugal separator
Two level solid-liquid separation treatment, the centrifugal separator are preferably supercentrifuge, more preferably tubular-bowl centrifuge, centrifugation
The rotating speed of machine particularly tube centrifuge can be 10000-50000rpm, be preferably 12000-20000rpm, the tubular type from
Scheming can be separate unit or is operated in parallel using more.A kind of embodiment according to the present invention, through cyclone hydraulic separators into
After row level-one separation of solid and liquid, overflow port clear liquid can mutually deliver into tubular type centrifugal separator and carry out two level separation of solid and liquid, into one
Step removing fine particle, the separation heavy phase and/or sediment of centrifuge can be discharged by slag-drip opening interval, solid particle in clear liquid phase
In general thing mean concentration is less than 0.8g/L, preferably shorter than 0.2g/L, sees the solution substantially clarified in appearance.
It will be appreciated by persons skilled in the art that according to the present invention it is possible to by the rare earth element in the two level clear liquid
Further recycled and be enriched with, still, the two level clear liquid is preferably transported to the production process of sulfur transfer additive by the present invention
It is middle to be recycled online, not only facilitate but also the fresh water magnitude of recruitment and rare earth inventory of sulfur transfer additive production can be reduced.
The whereabouts that line recycles includes, but are not limited to：It is transported in rare earth material-compound tank, for preparing earth solution；It is back to use auxiliary agent
In colloid generating kettle, it is beaten for colloidal dispersions；It is recycled back to the part as maceration extract in carrier impregnation tank；Wherein it is preferred that follow
A part in loopback carrier impregnation tank as maceration extract.
According to the present invention, FCC catalyst production waste water carry out pre-separation heavy phase that solid-liquid pre-separation handles and/
Or sediment, can with FCC catalyst fine powder mix after, carry out levigate processing, obtained pre-separation is levigate processing mixing heavy phase and/
Or sediment is sent into reuse in the colloid generating kettle of FCC catalyst production process, based on butt, for the mixing heavy phase of plastic and/or heavy
Slag accounts for 1 weight %-20 weight % of every kettle inventory butt gross weight, is preferably 5 weight %-10 weights %.Pre-separation is levigate, and processing mixing is heavy
Mutually and/or in sediment the average grain diameter of solid particulate matter is less than 4.5 microns, preferably smaller than 3 microns.The pre-separation heavy phase and/
Or sediment and the catalyst fines that are added are by dry basis, mixed proportion 0.1-10:1, it is preferably 0.5-5:1.Wherein,
The FCC catalyst fine powder is the fine powder produced in FCC catalyst production process, can come from FCC catalyst production process
Any fines collection unit, for example, can come from the fines collection unit of airstream drying tower, can be from spray drying tower
The fine powder that place, roaster, finished product packing feed bin etc. are collected, preferably carrys out spray drying tower, divides from airstream drying tower etc. whirlwind
The fine powder collected from device, the average grain diameter of the fine powder can be 2-20 microns.The catalyst fines can also be part or all of
Replace with least one of molecular sieve, aluminium oxide and kaolin.
A kind of embodiment according to the present invention, first can add institute in the pre-separation heavy phase and/or sediment
At least one of FCC catalyst fine powder, molecular sieve, aluminium oxide and kaolin are stated, pre-separation mixing heavy phase is obtained and/or sinks
Slag；The pre-separation is mixed into heavy phase and/or sediment and carries out levigate processing, obtain the levigate processing mixing heavy phase of pre-separation and/or
Sediment, the levigate processing of pre-separation mixes the average grain diameter of solid particulate matter in heavy phase and/or sediment less than 4.5 microns, excellent
Choosing is less than 3 microns；The levigate processing mixing heavy phase of the pre-separation and/or sediment can be sent in FCC catalyst colloid generating kettle and returned
With；Wherein, with dry basis, the weight of the pre-separation heavy phase and/or sediment can be the FCC catalyst fine powder, point
0.1-10 times of the weight of at least one of son sieve, aluminium oxide and kaolin.
According to the present invention, it will be appreciated by persons skilled in the art that can be by the two level heavy phase and/or sediment and institute
Levigate processing is carried out after stating level-one heavy phase and/or sediment mixing, obtains the levigate processing heavy phase of sulfur transfer additive and/or sediment, it is described
The average grain diameter of solid particulate matter is less than 4.5 microns, preferably smaller than 3 microns in heavy phase that sulfur transfer additive is levigate and/or sediment；Then
The levigate processing heavy phase of the sulfur transfer additive and/or sediment can be sent in the colloid generating kettle of sulfur transfer additive production and carry out circulation profit
With based on butt, mixing heavy phase and/or sediment for plastic account for 1 heavy %-10 weights % of every kettle inventory butt gross weight, excellent
Elect 4 weight %-8 weights % as.Further, in order to rationally utilize sulfur transfer additive production finished product collector unit collected by sulphur transfer
Sulfur transfer additive fine powder, can be added in the level-one heavy phase and/or sediment and the two level heavy phase and/or sediment by agent fine powder
Carry out being sent to after levigate processing in the colloid generating kettle of sulfur transfer additive production together and recycled.Wherein, with dry basis, institute
State the sulfur transfer additive fine powder of level-one heavy phase and/or sediment and the two level heavy phase and/or the gross weight of sediment and addition
Weight ratio can be 1:10-10:1, it is preferably 1:5-5:1, the sulfur transfer additive fine powder can also be partly or totally replaced with oxygen
Change aluminium, preferably replace with boehmite.
A kind of embodiment according to the present invention, can be by the two level heavy phase and/or sediment and the level-one weight
Sulfur transfer additive fine powder and/or aluminium oxide mutually and/or after sediment mixing are added, obtains sulfur transfer additive mixing heavy phase and/or sediment；So
After sulfur transfer additive can be mixed after heavy phase and/or sediment carry out levigate processing, obtain the levigate processing mixing heavy phase of sulfur transfer additive
And/or sediment, the average grain diameter that the levigate processing of sulfur transfer additive mixes solid particulate matter in heavy phase and/or sediment are less than 4.5
Micron, preferably smaller than 3 microns；The levigate processing mixing heavy phase of the sulfur transfer additive and/or sediment can be sent to sulfur transfer additive life
Reuse in the colloid generating kettle of production process；Wherein, with dry basis, the two level heavy phase and/or sediment and the level-one heavy phase and/
Or the gross weight of sediment can be 0.1~10 times of the sulfur transfer additive fine powder and/or alumina weight.
According to the present invention, it will be appreciated by persons skilled in the art that can use in cutter, sand mill and ball mill
At least one levigate processing unit carry out the levigate processing, levigate processing time can be 5-60 minutes, it is preferred to use ball
Grinding machine carries out levigate processing, can also use industrial other levigate processing methods, and the present invention is not restricted.Wherein, it is described
It is well-known to those skilled in the art to carry out levigate processing using ball mill, and the slurry solid content of levigate processing can be
10%-40%, the time of levigate processing can be 5-60 minutes.
The method of the present invention will be described further by embodiment below, but the present invention is not limited thereto.
The instrument and equipment is routine instrument device in prior art unless otherwise instructed, but does not therefore limit this hair
It is bright.
Sulfur transfer additive production and wastewater treatment are limited in Sinopec catalyst in all embodiment and comparative example experiments
Carried out on the existing Conventional catalytic cracking Catalyst Plant of company.Wherein, used sulfur transfer additive produces efflux wastewater
Average composition is：CeO2Content is 12.5g/L, and solid particulate matter content 10.3g/L, average grain diameter is 5.65 μm, wastewater pH
It is worth for 6.5.Catalyst exchanges to exist in washing filtrate waste water containing 0.8 g/l of rare earth element, 5.5 g/l of average grain diameter
5.36 μm of solid particulate matter, the pH value of the waste water is 4.5.Under the basic operating mode of existing efflux wastewater operation, belt filter
Machine filtering rate is usually in 2.2-2.5m3/ h, cake moisture is in 33-38%.Sulfur transfer additive fine powder is derived from airstream drying tower rotation
Wind separator, 10.2 μm of average grain diameter, above-mentioned fine powder, which is directly added into waste water, in the embodiment of the present invention is used as helping sedimentation agent, or warp
Added after 650 DEG C of roasting 1.5h in waste water and be used as helping sedimentation agent.For the auxiliary agent fine powder with heavy phase and/or sediment mixed grinding not
Calcination process is carried out again.FCC catalyst fine powder comes from spray drying tower cyclone separator, and average grain diameter is 11.5 μm, with press filtration
Without calcination process before filter residue mixed grinding obtained by machine pre-separation.Sulfur transfer additive is adopted with FCC catalyst straight tube abrasion index
(Yang Cuiding, Gu Kanying, Wu Wenhui volume Petrochemical Engineering Analysis method Beijing is measured with RIPP 29-90 methods：Science Press,
1990).Sulfur transfer additive abrasion index qualification index is≤4.5, and FCC catalyst straight tube abrasion index qualification index is≤3.0.It is useless
The average grain diameter of solid particulate matter is measured (the Nephelometric Determination solids in suspension particles such as Zheng Bo using nephelometry in water
The research of concentration, petroleum refining and chemical industry, 2011,41 (10):78-81), the average grain diameter of fine powder uses laser particle size analyzer
It is measured by ASTM D4464 methods.
Embodiment 1
This example demonstrates that the circulation profit of sulfur transferring assistant of the present invention and FCC catalyst production fine powder and composite waste
Use method.
Catalyst production waste water carries out solid-liquid pre-separation, operating pressure 0.7MPa using filter press, and filtrate is continuously discharged, and filters
Slag interval discharging.By volume flowmeter, the mixed proportion of filter press filtrate and sulfur transfer additive production waste water is 1:1.
Sulfur transfer additive fine powders of the 4g after 650 DEG C roast 1.5h is added into every liter of composite waste, is stirred, uses hydrochloric acid
PH value is adjusted to 4.Waste water suspension is pumped into cyclone hydraulic separators, inlet pressure 0.35MPa, underflow and overflow volume flow-rate ratio 1:
8.Overflow outlet clear liquid is mutually transported to tube centrifuge entrance, centrifuge speed 15000rpm, solid phase sediment at interval of 1 it is small when
Remove once, clear liquid phase particle content is 0.15g/L.
Clear liquid is transported in carrier impregnation tank, for sulphur transfer vector excess dip loading rare earth.Per reuse 1m3Clear liquid
Can be while equivalent fresh water be substituted, it is 6.65kg to reduce rare earth inventory.After continuous reuse 8h, filtering rate is kept substantially
In 2.4m3/ h, cake moisture 35.5%, with being arranged outside waste water before reuse under operation operating mode quite.Show waste water through the present invention
It is back to after the method processing during carrier impregnation, while realizing that rare earth element recycles online, not to filter
Filter efficiency is produced and significantly affected.
After the containing wastewater from catalyst filter cake that filter press obtains is drawn off, by butt weight ratio 1:2 mix with the fine powder that it is possible to additionally incorporate,
Into ball mill grinding, grinding solid content is 32%, and milling time 25min, solid particle average grain diameter reaches 2.25 microns.Grind
Slurry after mill is back in catalyst colloid generating kettle, and by dry basis, reuse slurry accounts for the 8% of every kettle material total amount.Continuously
After reuse 8h, finished catalyst straight tube abrasion index is 1.6.
After cyclone hydraulic separators heavy phase and tube centrifuge sludge collection, by dry basis, add and heavy phase and sediment
Middle solid identical weight (1:1) auxiliary agent fine powder, into ball mill grinding, grinding solid content is 35%, milling time 30min,
After grinding, solid particle average grain diameter reaches 2.48 microns.Slurry after grinding is transported to reuse in batches in auxiliary agent colloid generating kettle.Press
Dry basis, the inventory of reuse slurry account for the 5% of every kettle material butt total amount.After continuous reuse 8h, auxiliary agent finished-product straight pipe
Abrasion index is 3.3.Show the separating obtained solid particulate matter of waste water and fine powder mixture material, plastic is back to after ground processing
Process, does not adversely affect auxiliary agent abrasion resistance properties.
Embodiment 2
This example demonstrates that the circulation profit of sulfur transferring assistant of the present invention and FCC catalyst production fine powder and composite waste
Use method.
Catalyst production waste water carries out solid-liquid pre-separation, operating pressure 0.7MPa using filter press, and filtrate is continuously discharged, and filters
Slag interval discharging.By volume flowmeter, the mixed proportion of filter press filtrate and sulfur transfer additive production waste water is 1:1.
Sulfur transfer additive fine powders of the 4g without calcination process is added into every liter of composite waste, is stirred, is adjusted with hydrochloric acid
PH value is to 4.Waste water suspension is pumped into cyclone hydraulic separators, inlet pressure 0.35MPa, underflow and overflow volume flow-rate ratio 1:8.Overflow
Flow export clear liquid is mutually transported to tube centrifuge entrance, centrifuge speed 15000rpm, and solid phase sediment is removed at interval of 50min
Once, clear liquid phase particle content is 0.55g/L.
Clear liquid is transported in carrier impregnation tank, for sulphur transfer vector excess dip loading rare earth.Per reuse 1m3Clear liquid
Can be while equivalent fresh water be substituted, it is 6.65kg to reduce rare earth inventory.After continuous reuse 8h, filtering rate is kept substantially
In 2.3m3/ h, cake moisture 36.2%, with being arranged outside waste water before reuse under operation operating mode quite.Show waste water through the present invention
It is back to after the method processing during carrier impregnation, while realizing that rare earth element recycles online, filter can be made
Filter efficiency and cake moisture are substantially remained in the range of nominal situation.
After the containing wastewater from catalyst filter cake that filter press obtains is drawn off, by butt weight ratio 1:0.8 mixes with the fine powder that it is possible to additionally incorporate
Close, into ball mill grinding, grinding solid content is 30%, and milling time 20min, it is micro- that solid particle average grain diameter reaches 2.42
Rice.Slurry after grinding is back in catalyst colloid generating kettle, and by dry basis, reuse slurry accounts for the 5% of every kettle material total amount.
After continuous reuse 8h, finished catalyst straight tube abrasion index is 1.8.
After cyclone hydraulic separators heavy phase and tube centrifuge sludge collection, by dry basis, add and heavy phase and sediment
Middle solid identical weight (1:1.5) auxiliary agent fine powder, into ball mill grinding, grinding solid content is 35%, and milling time is
30min, after grinding, solid particle average grain diameter reaches 2.75 microns.Slurry after grinding is transported in auxiliary agent colloid generating kettle in batches
Reuse.By dry basis, the inventory of reuse slurry accounts for the 5% of every kettle material butt total amount.After continuous reuse 8h, auxiliary agent into
Product straight tube abrasion index is 3.6.Show the separating obtained solid particulate matter of waste water and fine powder mixture material, reuse after ground processing
In plastic process, auxiliary agent abrasion resistance properties are not adversely affected.
Comparative example 1
This comparative example be used for illustrate composite waste without processing direct reuse in sulfur transfer additive carrier impregnation process to production
The influence of flow.
By volume flowmeter, the mixed proportion of sulfur transfer additive production waste water and catalyst production waste water is 1:1.Will be without place
The waste water of reason is delivered directly in carrier impregnation tank, for sulphur transfer vector excess dip loading rare earth.Per reuse 1m3Clear liquid is same
While sample alternative equivalent fresh water, it is 6.65kg to reduce rare earth inventory.After continuous reuse 8h, filtering rate is reduced to
1.7m3/ h, cake moisture bring up to 40.4%.Show to soak the undressed direct reuse of waste water containing rare earth element in carrier
During stain, although equivalent fresh water can be substituted equally, rare earth inventory is reduced, to filter filter efficiency and cake moisture
Generation significantly affects.
Comparative example 2
This comparative example is used to illustrate clear liquid reuse influence to production procedure of the composite waste only after two-stage separation of solid and liquid.
After the obtained heavy phase of separation of solid and liquid at different levels and/or sediment, with catalyst or the blending of auxiliary agent fine powder, as long as by
Sufficient levigate processing, can be back to use in FCC catalyst or sulfur transfer additive production procedure by proper proportion, without to product
Abrasion index causes significantly to adversely affect.Thus need to pay close attention to during fine powder and cycling utilization of wastewater is still separation
Influence of the clear liquid to filter efficiency.
Solid-liquid pre-separation is carried out to catalyst production waste water with reference to 1 the method for embodiment, and will be produced with sulfur transfer additive
Waste water presses 1:1 ratio mixing.But add sulfur transfer additive fine powder not into composite waste, also adjusted without pH value.But will be mixed
Close waste water and be pumped directly into cyclone hydraulic separators, inlet pressure 0.35MPa, underflow and overflow volume flow-rate ratio 1:8.Overflow outlet is clear
Liquid phase is transported to tube centrifuge entrance, centrifuge speed 15000rpm, solid phase sediment at interval of 0.5 it is small when remove once,
Clear liquid phase particle content is 1.09g/L.Clear liquid is transported in carrier impregnation tank, for sulphur transfer vector excess dip loading
Rare earth.Per reuse 1m3Clear liquid can be while equivalent fresh water be substituted, and it is 6.65kg to reduce rare earth inventory.Continuous reuse 8h
Afterwards, filtering rate is reduced to 2.1m3/ h, cake moisture 38.5%.With respect to embodiment 2, the centrifuge scarfing cinder week of comparative example 2
Phase significantly shortens, and solid-liquid separation effect is deteriorated, although equivalent fresh water can be substituted equally, rare earth inventory is reduced, to filter
Filter efficiency and cake moisture, which produce, significantly to be influenced.
Comparative example 3
This comparative example is used to illustrate that fine powder and composite waste are prepared to production without processing direct reuse in sulfur transfer additive colloid
Quality and the influence of production procedure.
By volume flowmeter, the mixed proportion of sulfur transfer additive production waste water and catalyst production waste water is 1:1.It is mixed to every liter
Close and 5g sulfur transfer additive fine powders are added in waste water, be delivered directly in auxiliary agent colloid generating kettle, plastic is beaten for sulphur transfer vector.By dry
Base weight gauge, often reuse material proportion is 4% in kettle material.After continuous reuse 8h, filtering rate is reduced to 2.1m3/ h,
Cake moisture brings up to 38.5%, and auxiliary agent finished-product straight pipe abrasion index is 5.2.Show undressed fine powder and waste water is straight
Take back for during plastic, although rare earth and raw material inventory can be reduced, to filter filter efficiency, cake moisture and
Auxiliary agent abrasion resistance properties, which produce significant adverse, to be influenced.
Claims (12)
1. a kind of sulfur transfer additive and the Application way of FCC catalyst production fine powder and waste water, this method include：First FCC is catalyzed
Agent production waste water carries out solid-liquid pre-separation processing, obtains pre-separation clear liquid and pre-separation heavy phase containing solid particulate matter and/or heavy
Slag；The pre-separation heavy phase and/or sediment are subjected to levigate processing, obtain the levigate processing heavy phase of pre-separation and/or sediment, it is described
The average grain diameter of solid particulate matter is less than 4.5 microns in processing heavy phase that pre-separation is levigate and/or sediment；The pre-separation is levigate
Processing heavy phase and/or sediment are sent to reuse in FCC catalyst colloid generating kettle；By volume, by 1 part of sulfur transfer additive production waste water with
0.2-5 parts of pre-separation clear liquid mixing, obtains sulfur transfer additive and FCC catalyst mixture manufacturing waste water；Sulfur transfer additive is thin
Powder obtains mixing suspension as helping sedimentation agent to be added in the mixture manufacturing waste water；With the body of the mixture manufacturing waste water
On the basis of product, the addition of the sulfur transfer additive fine powder is 1-15 g/l；The pH value of the mixing suspension is controlled in 2-6；
By the pH value be 2-6 mixing suspension carry out level-one solid-liquid separation treatment, obtain level-one clear liquid and containing solid particulate matter one
Level heavy phase and/or sediment；The level-one clear liquid is subjected to two level solid-liquid separation treatment, two level clear liquid is obtained and contains solid particle
The two level heavy phase and/or sediment of thing；Then the two level clear liquid is transported in the production process of sulfur transfer additive again and is circulated
Utilize, carry out levigate processing after the two level heavy phase and/or sediment are mixed with the level-one heavy phase and/or sediment, obtain sulphur
Processing heavy phase and/or sediment that transfer agent is levigate, solid particulate matter is flat in processing heavy phase that the sulfur transfer additive is levigate and/or sediment
Equal particle diameter is less than 4.5 microns；The levigate processing heavy phase of the sulfur transfer additive and/or sediment are sent in sulfur transfer additive production process
Reuse in auxiliary agent colloid generating kettle；The pH value of the FCC catalyst production waste water is 3.5-5, contains the 0.2-1.5 in terms of oxide weight
G/l rare earth element, with 0.5-10 g/l of solid particulate matter of dry basis；Wherein, it is described in terms of oxide weight
The content of Ce is not less than the 20% of whole rare earth element contents in FCC catalyst production waste water；The sulfur transfer additive produces waste water
PH value be 5-8, containing 1-20 g/l in terms of oxide weight of rare earth element, with 2-25 g/l of solid of dry basis
Particulate matter.
2. the method according to claim 1, wherein, the sulfur transfer additive fine powder be produced in sulfur transfer additive production process it is thin
Powder, the average grain diameter of the fine powder is 2-20 microns.
3. the method according to claim 1, wherein, first by the sulfur transfer additive fine powder 450-800 DEG C roast 0.5-4 it is small when after
It is re-used as helping sedimentation agent to be added in sulfur transfer additive and FCC catalyst the mixture manufacturing waste water.
4. the method according to claim 1, wherein, the pH value of the mixing suspension is controlled in 3-5.
5. the method according to claim 1, wherein, the pH value of the mixing suspension is controlled by adding hydrochloric acid.
6. the method according to claim 1, wherein, the solid-liquid is carried out by using subsider, filter or cyclone hydraulic separators
Pre-separation processing and/or level-one solid-liquid separation treatment.
7. according to the method for claim 1 or 6, wherein, carried out by using centrifugal separator at the two level separation of solid and liquid
Reason.
8. the method according to claim 1, wherein, the rare earth that the two level clear liquid is transported in sulfur transfer additive production process is matched somebody with somebody
Recycled in batch can, auxiliary agent colloid generating kettle and/or carrier impregnation tank.
9. the method according to claim 1, wherein, first the FCC catalyst is added in the pre-separation heavy phase and/or sediment
At least one of fine powder, molecular sieve, aluminium oxide and kaolin, obtain pre-separation mixing heavy phase and/or sediment；By described pre- point
Levigate processing is carried out from mixing heavy phase and/or sediment, levigate handle of pre-separation is obtained and mixes heavy phase and/or sediment, described pre- point
Average grain diameter from solid particulate matter in levigate processing mixing heavy phase and/or sediment is less than 4.5 microns；The pre-separation is levigate
Processing mixing heavy phase and/or sediment are sent to reuse in FCC catalyst colloid generating kettle；Wherein, with dry basis, the pre-separation weight
Phase and/or the weight of sediment are the weight of at least one of FCC catalyst fine powder, molecular sieve, aluminium oxide and the kaolin
0.1~10 times.
10. the method according to claim 1, wherein, by the two level heavy phase and/or sediment and the level-one heavy phase and/or sink
Sulfur transfer additive fine powder and/or aluminium oxide are added after slag mixing, obtains sulfur transfer additive mixing heavy phase and/or sediment；Then sulphur is turned
After moving agent mixing heavy phase and/or the levigate processing of sediment progress, the levigate processing mixing heavy phase of sulfur transfer additive and/or sediment, institute are obtained
The average grain diameter for stating solid particulate matter in the levigate processing mixing heavy phase of sulfur transfer additive and/or sediment is less than 4.5 microns；By the sulphur
Processing mixing heavy phase that transfer agent is levigate and/or sediment are sent to reuse in sulfur transfer additive colloid generating kettle；Wherein, with dry basis, institute
It is the sulfur transfer additive fine powder and/or oxidation to state two level heavy phase and/or sediment and the level-one heavy phase and/or the gross weight of sediment
0.1~10 times of aluminium weight.
11. according to the method for claim 1,9 or 10, wherein, ground using at least one of cutter, ball mill and sand mill
Thin processing unit carries out the levigate processing, and the time of levigate processing is 5-60 minutes.
12. method according to claim 9, wherein, the FCC catalyst fine powder is produced in FCC catalyst production process
Fine powder, the average grain diameter of the fine powder is 2-20 microns.
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