CN106984264A - The method that harmless treatment prepares atlapulgite is carried out to spent FCC catalyst - Google Patents
The method that harmless treatment prepares atlapulgite is carried out to spent FCC catalyst Download PDFInfo
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- CN106984264A CN106984264A CN201710222482.9A CN201710222482A CN106984264A CN 106984264 A CN106984264 A CN 106984264A CN 201710222482 A CN201710222482 A CN 201710222482A CN 106984264 A CN106984264 A CN 106984264A
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- fcc catalyst
- spent fcc
- atlapulgite
- leaching
- liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The method that harmless treatment prepares atlapulgite is carried out to spent FCC catalyst the present invention relates to a kind of, is comprised the following steps that：(1) activation and leaching of spent FCC catalyst；(2) solid- liquid separation I, leaching liquid is separated with leaching slag；(3) processing of leaching liquid, extracts metal or compound, and devil liquor recovery is used for the activation of next group spent FCC catalyst；(4) washing of spent FCC catalyst leaching slag；(5) solid- liquid separation II, cleaning solution is separated with washed-residue, and cleaning solution reclaims the activation for next group spent FCC catalyst or the washing of leaching slag；(6) spent FCC catalyst washed-residue is prepared into atlapulgite.The present invention realizes innoxious, the recycling of spent FCC catalyst, and whole preparation process does not produce any waste liquid, waste residue, belongs to green circulatory industrial production technology.
Description
Technical field
The invention belongs to discard the technical field that industrial chemicals is recycled, and in particular to a kind of spent FCC catalyst is recycled
Method, more particularly to a kind of the harmless treatment method for preparing atlapulgite is carried out to spent FCC catalyst.
Background technology
FCC catalyst is the most important catalyst of oil plant, and amount is big.Total consumption in the annual whole nation is more than 90,000 tons, every year
Produce nearly 80,000 tons of spent FCC catalysts.Spent FCC catalyst surface attachment derives from the various metals in raw material and Petroleum Refining Additives
Element, such as comes from nickel, the vanadium of catalytically cracked material, comes from antimony and tin of catalytic cracking passivator etc..Therefore useless FCC catalysis
Agent has different degrees of pollution to soil and water body environment, has been included in the dangerous solid waste of state control discharge.Country
Preventing and treating to solid waste pollution environment, is carried out and reduces the yield and harmfulness of solid waste, fully rationally given up using solid
The principle of thing and harmlessness disposing solid waste, promotes clean manufacturing and recycling economy development.
The untreated spent FCC catalyst of major oil plants was largely landfilled in the past.In recent years, environmental administration improves place
Reason standard, increase supervision.National policy and environmental requirement are not met with land-fill method disposal hazardous waste, should be paid
Hazardous waste charges for disposing pollutants.Have Magneto separate at present to the processing of spent FCC catalyst, catalyst plant is reclaimed, then demetalization regeneration or
Person's crystallization again, also have been reported that spent FCC catalyst is used to paving the way, to be added to cement medium.And spent FCC catalyst is carried out harmless
There is not been reported for the regeneration of the activation process production high-performance atlapulgite of change.
After catalyst inactivation to the processing of dead catalyst and can regeneration, be not only directly connected to industrial warp
Ji benefit, is more related to the environmental issue of human kind sustainable development.Processing and regeneration, certainly using the regeneration that effects a permanent cure as
It is good.
Atlapulgite main chemical compositions are silica, alundum (Al2O3) and water, also containing iron, magnesium, calcium, sodium, potassium etc.
Element.Catalytic cracking catalyst is a kind of solid acid catalyst of good thermal stability.From initial natural clay, synthesizing Si-Al
All it is the solid-acid material based on alumina silicate to molecular sieve catalyst.The main body of spent FCC catalyst chemical composition is
SiO2And Al2O3, it is consistent with atlapulgite main chemical compositions.Spent FCC catalyst typically contains the boiling of 10%~25% mass fraction
Stone, with larger specific surface area and pore volume, with the potential quality as good adsorption agent.Moreover, composition FCC catalyst
I.e. the carrier of matrix catalyst, is typically the unbodied aluminosilicate of catalytic activity, natural activity carclazyte, semi-synthetic
Kaolin etc., thus it is feasible to carry out innoxious activation process to spent FCC catalyst to produce high-performance atlapulgite.
Atlapulgite is to use clay（Mainly bentonite）For raw material, the activation process through peracid, then rinse through water, dry
The adsorbent being made, outward appearance is off-white powder, and odorless is tasteless, and nontoxic, absorption property is very strong, can adsorb coloring matter, organic
Material.Atlapulgite is big because of specific surface area, high adsorption capacity, and decolorizing efficiency is high；Activity degree is low, not with grease and other chemicals
Chemical action occurs for matter；Fast for the liquid decoloration rate of filtration, raffinate rate is low, such as eats oil decolorization, sugaring and decolourizes；After decolouring
Liquid-transparent is limpid, stay in grade, free from extraneous odour, not color reversion, does not return acid；Product after use, can be carried out by proper treatment
It is secondary to utilize, do not result in the series of products such as environmental pollution advantage and be widely used in adsorbent, granular carclazyte, NCR
With in developer.
The content of the invention
The side that harmless treatment prepares atlapulgite is carried out to spent FCC catalyst it is an object of the invention to provide a kind of
Method, fully rationally using the dangerous solid waste of simultaneously harmlessness disposing oil plant, to turn waste into wealth, eliminate the dirt to environment
Dye, promotes clean manufacturing and recycling economy development.
To achieve the above object, technical solution of the invention is：It is a kind of that harmless treatment is carried out to spent FCC catalyst
The method for preparing atlapulgite, is comprised the following steps that：
(1) activation and leaching of spent FCC catalyst：Spent FCC catalyst is mixed with acid solution, in certain temperature, pressure and stirred
Mix under velocity conditions, activate spent FCC catalyst and leach the rare earth in spent FCC catalyst and heavy metal；
(2) solid- liquid separation I：Leaching liquid is separated with leaching slag；
(3) processing of leaching liquid：Leaching liquid is purified, is enriched with being separated, metal or compound are produced out from solution, is given up
Liquid reclaims the activation for next group spent FCC catalyst；
(4) washing of spent FCC catalyst leaching slag：Leaching slag is washed with clear water or cleaning solution, is repeated 2~8 times, until washing
The pH value of liquid is washed between 4~6；
(5) solid- liquid separation II：Cleaning solution is separated with washed-residue, cleaning solution is reclaimed for next group spent FCC catalyst
Activation or leaching slag washing；
(6) spent FCC catalyst washed-residue is prepared into atlapulgite：Washed-residue is dehydrated under certain temperature, pressure condition, ground
Mill, is made atlapulgite.
The acid solution mixed with spent FCC catalyst is sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, oxalic acid, citric acid, tartaric acid
In one kind or any several formed with water mixed preparing；Further, the sour mass fraction is 0.1% ~ 50%；More enter
One step, the solid-to-liquid ratio that spent FCC catalyst is mixed with the acid is 1: (1 ~ 10).
The temperature of activation and the leaching of the spent FCC catalyst is 10 ~ 150 DEG C, and pressure is 0.01 ~ 0.9MPa, stirring speed
Spend for 0 ~ 3000rpm, the time is 1 ~ 48h.
The method of the solid- liquid separation is sedimentation, filtering, press filtration and one kind in centrifugation or any several cooperations
With.
Purification, enrichment and the separation method of the leaching liquid are chemical precipitation, hydrolysis, displacement, solvent extraction, ion friendship
Change, one kind in membrane separation technique or any several cooperations are used；Further, it is described that metal or change are produced out from solution
The method of compound is electrolysis, chemical precipitation, evaporative crystallization, chemical displacement method, one kind in pressurization hydrogen reduction method or any several
Plant to coordinate and use.
The method of the washed-residue dehydration is in gravity dehydration, centrifugal dehydration, filtering means dehydration, filter-press dehydration and drying and dehydrating
One kind or it is any it is several coordinate use, the temperature of dehydration is 10 ~ 150 DEG C, pressure is -1 ~ 4Mpa.
The present invention realizes innoxious, the recycling of spent FCC catalyst, and whole preparation process does not produce any
Waste liquid, waste residue, belong to green circulatory industrial production technology.According to the present invention provide it is a kind of to spent FCC catalyst carry out it is harmless
Change processing prepares atlapulgite product prepared by the method for atlapulgite, according to country chemical industry standard HG/T 2569-2007
Detected, testing result indices comply fully with requirement of the national standard to atlapulgite.
Classification, model and the code name of the atlapulgite of table 1
The requirement of the atlapulgite of table 2 and spent FCC catalyst prepare atlapulgite testing result
Embodiment：
A part of specific embodiment is set forth below, and the present invention will be described, it is necessary to it is pointed out here that be specific examples below
It is served only for that the invention will be further described, does not represent limiting the scope of the invention.Other people make according to the present invention
Some it is nonessential modification and adjustment still fall within protection scope of the present invention.
Embodiment 1
(1) activation and leaching of spent FCC catalyst：By the sulfuric acid of spent FCC catalyst and mass fraction 25% according to solid-to-liquid ratio 1:4
Mixing, under the conditions of 115 DEG C, 0.2MPa and mixing speed 300rpm, activates spent FCC catalyst and leaches in spent FCC catalyst
Rare earth and heavy metal, duration 4h；
(2) solid- liquid separation I：Leaching liquid is separated with leaching slag with the method for filtering；
(3) processing of leaching liquid：Leaching liquid is purified, be enriched with and separated with chemical precipitation and solvent-extracted method, is used
Chemical precipitation and evaporative crystallization method produce out metal or compound from solution, and devil liquor recovery is used for next group spent FCC catalyst
Activation；
(4) washing of spent FCC catalyst leaching slag：Leaching slag is washed with clear water or cleaning solution, is repeated 5 times, until washing
The pH value of liquid is between 4~6；
(5) solid- liquid separation II：Cleaning solution is separated with washed-residue with the method for filtering, cleaning solution is reclaimed for next group
The activation of spent FCC catalyst or the washing of leaching slag；
(6) spent FCC catalyst washed-residue is prepared into atlapulgite：By washed-residue under the conditions of 120 DEG C, 0.1Mpa drying and dehydrating,
Half an hour is ground, atlapulgite is made.
Embodiment 2
(1) activation and leaching of spent FCC catalyst：By the nitric acid of spent FCC catalyst and mass fraction 35% according to solid-to-liquid ratio 1:5
Mixing, under the conditions of 95 DEG C, 0.1MPa and mixing speed 1000rpm, activates spent FCC catalyst and leaches in spent FCC catalyst
Rare earth and heavy metal, duration 6h；
(2) solid- liquid separation I：Leaching liquid is separated with leaching slag with the method for centrifugation；
(3) processing of leaching liquid：Leaching liquid is purified, be enriched with and separated with the method for solvent extraction and ion exchange, is used
Electrolysis and chemical precipitation method produce out metal or compound from solution, and devil liquor recovery is used for next group spent FCC catalyst
Activation；
(4) washing of spent FCC catalyst leaching slag：Leaching slag is washed with clear water or cleaning solution, is repeated 4 times, until washing
The pH value of liquid is between 4~6；
(5) solid- liquid separation II：Cleaning solution is separated with washed-residue with the method for sedimentation, cleaning solution is reclaimed for next group
The activation of spent FCC catalyst or the washing of leaching slag；
(6) spent FCC catalyst washed-residue is prepared into atlapulgite：By washed-residue under the conditions of 110 DEG C, 0.1Mpa drying and dehydrating,
Half an hour is ground, atlapulgite is made.
Embodiment 3
(1) activation and leaching of spent FCC catalyst：By spent FCC catalyst and the sulfuric acid of mass fraction 25%, the hydrochloric acid of mass fraction 35%
With saturated oxalic acid volume ratio 4:4:1 nitration mixture is according to solid-to-liquid ratio 1:3 mixing, it is living in 25 DEG C, 0.5MPa and under conditions of not stirring
Change spent FCC catalyst and leach the rare earth in spent FCC catalyst and heavy metal, duration 24h；
(2) solid- liquid separation I：Leaching liquid is separated with leaching slag with the method for press filtration；
(3) processing of leaching liquid：Leaching liquid is purified with the method for solvent extraction, ion exchange and membrane separation technique, it is rich
Collect with separating, metal or compound, devil liquor recovery are produced out from solution with electrolysis, chemical precipitation method and pressurization hydrogen reduction method
Activation for next group spent FCC catalyst；
(4) washing of spent FCC catalyst leaching slag：Leaching slag is washed with clear water or cleaning solution, is repeated 6 times, until washing
The pH value of liquid is between 4~6；
(5) solid- liquid separation II：Cleaning solution is separated with washed-residue with the method for press filtration, cleaning solution is reclaimed for next group
The activation of spent FCC catalyst or the washing of leaching slag；
(6) spent FCC catalyst washed-residue is prepared into atlapulgite：By washed-residue centrifugal dehydration under the conditions of 25 DEG C, 0.1Mpa, connect
The filter-press dehydration under the conditions of 25 DEG C, 0.4Mpa, finally the drying and dehydrating under the conditions of 115 DEG C, 0.1Mpa, ground one hour, system
Obtain atlapulgite.
Claims (6)
1. a kind of carry out the method that harmless treatment prepares atlapulgite to spent FCC catalyst, it is characterised in that specific steps are such as
Under：
(1) activation and leaching of spent FCC catalyst：Spent FCC catalyst is mixed with acid solution, in certain temperature, pressure and stirred
Mix under velocity conditions, activate spent FCC catalyst and leach the rare earth in spent FCC catalyst and heavy metal；
(2) solid- liquid separation I：Leaching liquid is separated with leaching slag；
(3) processing of leaching liquid：Leaching liquid is purified, is enriched with being separated, metal or compound are produced out from solution, is given up
Liquid reclaims the activation for next group spent FCC catalyst；
(4) washing of spent FCC catalyst leaching slag：Leaching slag is washed with clear water or cleaning solution, is repeated 2~8 times, until washing
The pH value of liquid is washed between 4~6；
(5) solid- liquid separation II：Cleaning solution is separated with washed-residue, cleaning solution is reclaimed for next group spent FCC catalyst
Activation or leaching slag washing；
(6) spent FCC catalyst washed-residue is prepared into atlapulgite：Washed-residue is dehydrated under certain temperature, pressure condition, ground
Mill, is made atlapulgite.
2. according to claim 1 carry out the method that harmless treatment prepares atlapulgite, its feature to spent FCC catalyst
It is the acid solution mixed with spent FCC catalyst in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, oxalic acid, citric acid, tartaric acid
It is a kind of or any several formed with water mixed preparing；Further, the sour mass fraction is 0.1% ~ 50%；Further
Ground, the solid-to-liquid ratio that spent FCC catalyst is mixed with the acid is 1: (1 ~ 10).
3. according to claim 1 carry out the method that harmless treatment prepares atlapulgite, its feature to spent FCC catalyst
The temperature for being activation and the leaching of the spent FCC catalyst is 10 ~ 150 DEG C, and pressure is 0.01 ~ 0.9MPa, and mixing speed is 0
~ 3000rpm, the time is 1 ~ 48h.
4. according to claim 1 carry out the method that harmless treatment prepares atlapulgite, its feature to spent FCC catalyst
It is sedimentation, filtering, press filtration and one kind in centrifugation or any several cooperation utilizations to be the method for the solid- liquid separation.
5. according to claim 1 carry out the method that harmless treatment prepares atlapulgite, its feature to spent FCC catalyst
The purification, enrichment and separation method for being the leaching liquid are chemical precipitation, hydrolysis, displacement, solvent extraction, ion exchange, film
One kind or any several cooperations in isolation technics are used；Further, it is described that metal or compound are produced out from solution
Method be electrolysis, chemical precipitation, evaporative crystallization, chemical displacement method, one kind in pressurization hydrogen reduction method or any several match somebody with somebody
Close and use.
6. according to claim 1 carry out the method that harmless treatment prepares atlapulgite, its feature to spent FCC catalyst
The method for being the washed-residue dehydration is one in gravity dehydration, centrifugal dehydration, filtering means dehydration, filter-press dehydration and drying and dehydrating
Kind or it is any it is several coordinate use, the temperature of dehydration is 10 ~ 150 DEG C, pressure is -1 ~ 4Mpa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187762A (en) * | 2018-01-02 | 2018-06-22 | 上海炼升化工股份有限公司 | A kind of regeneration method of equilibrium catalyst for catalytic cracking process |
| CN109482222A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of denitrating catalyst and preparation method thereof |
| CN112275262A (en) * | 2020-11-16 | 2021-01-29 | 中国石油化工股份有限公司 | Refinery anhydrous liquid ammonia decolorant and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109482222A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of denitrating catalyst and preparation method thereof |
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| CN108187762A (en) * | 2018-01-02 | 2018-06-22 | 上海炼升化工股份有限公司 | A kind of regeneration method of equilibrium catalyst for catalytic cracking process |
| CN112275262A (en) * | 2020-11-16 | 2021-01-29 | 中国石油化工股份有限公司 | Refinery anhydrous liquid ammonia decolorant and preparation method thereof |
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Application publication date: 20170728 |