CN107649093A - A kind of renovation process of aromatic hydrocarbon refining carclazyte - Google Patents
A kind of renovation process of aromatic hydrocarbon refining carclazyte Download PDFInfo
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- CN107649093A CN107649093A CN201610594677.1A CN201610594677A CN107649093A CN 107649093 A CN107649093 A CN 107649093A CN 201610594677 A CN201610594677 A CN 201610594677A CN 107649093 A CN107649093 A CN 107649093A
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- carclazyte
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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
- B01J20/16—Alumino-silicates
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
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Abstract
The invention discloses a kind of renovation process of aromatic hydrocarbon refining carclazyte, its renovation process is that (1) takes the aromatic hydrocarbon refining carclazyte of adsorption saturation in 120 DEG C~150 DEG C drying, 350 DEG C~850 DEG C are calcined 2~8 hours in moving air, and the moving air after roasting after the reactor burning equipped with exhaust combustion catalyst by discharging；(2) carclazyte after roasting in atmosphere is taken, is passed through the carbon dioxide for being entrained with vapor, is handled 1~9 hour at 400 DEG C~750 DEG C；(3) 1 part of the carclazyte learnt from else's experience after being entrained with the carbon dioxide treatment of vapor, 0.01~0.3 part of inorganic acid solution is added, activated 1~10 hour, 350 DEG C~850 DEG C roastings are to obtain the Regeneration Bleaching Clay in moving air.This method technical process is simple, whole process green, without noxious gas emission.The carclazyte specific surface area, pore volume and the aperture that obtain are handled by this method effectively to be recovered, and be can be recycled and are removed alkene therein in aromatic hydrocarbon refining.
Description
Technical field
The present invention relates to the renovation process after a kind of aromatic hydrocarbon refining atlapulgite adsorption saturation.
Background technology
Aromatic hydrocarbons is a kind of important large industrial chemicals and good solvent, mainly by naphtha reforming technique productions.
During aromatic hydrocarbons is produced, double centers on reforming catalyst surface can cause the generation of a small amount of accessory substance alkene, these alkene
Property it is active, not only easily forming colloid influences product quality, and the following process such as adsorbing separation that can be to aromatic hydrocarbons is brought
It is difficult.In order to obtain qualified industrial chemicals and ensure the good operation of downstream process, generally in reformation, Aromatics Extractive Project, isomery
The downstream of the devices such as change, disproportionation sets refining step by the trace amounts of olefin impurity removal in aromatic hydrocarbons.Remove the virtue after some olefin
For hydrocarbon feed liquid generally with the wherein remaining olefin(e) centent of bromine index reflection, it is defined as the milli for the bromine that 100 grams of aromatic hydrocarbons samples are consumed
Grams, need to control bromine index following for 20mgBr/ (100g) oil after general reformed arene is refined.When bromine index is higher than 20mgBr/
When (100g) is oily, olefin removal agent need to be changed.
At present, trace amounts of olefin inorganic agent generally use noble metal catalyst and Emathlite (molecular sieve) are industrially removed,
The country is mainly based on the latter.Relevant Emathlite or molecular sieve refine to be had been disclosed in many documents.For example,
ZL200910057814.8 reports the method by removing olefin of reformate in non-hydrogenation manner, and the patent uses molecular sieve and aluminum oxide
Or silica is major catalyst, the auxiliary agents such as a small amount of Cl, Br, S, F, P are added, regulation and control B acid and the catalyst after L acid show good
Good deolefination activity and life-span.ZL201010539508.0 discloses is prepared into stripe shape or ball-type Y by raw material of adobe
The method of type molecular sieve, and by the Y type molecular sieve be used for Arene removal in alkene, although the molecular sieve deolefination initial activity compared with
It is good, but the life-span is poor, influences its commercial Application.Using attapulgite clay as raw material in ZL201110092072.X, through peracidity
There is the activity of alkene in good Arene removal, but the life-span of the modified clay does not disclose in the patent after processing.
ZL201210137427.7 describes a kind of ball-type atlapulgite for being used for alkene in Arene removal, and atlapulgite service life is
1~3 year.
The problem of discarded clay treatment for adsorbing a large amount of aromatic hydrocarbon substances and olefin polymer is currently one more difficult.By
Generally in the aromatic hydrocarbon refining carclazyte containing the element such as substantial amounts of carcinogen aromatic hydrocarbons and extremely micro lead, arsenic, adsorption saturation
Occupy cultivated land and carry out buried processing.It is buried for a long time that underground water can be brought dirty although buried processing can slow down the release of pollutant
The environmental problems such as dye.Processing about discarding carclazyte has been described in some documents.For example, Chinese invention patent
CN201110446667.0 uses the discarded carclazyte of solvent processing for comprising at least two kinds of polar compounds, is carried out after extraction
Oil recovery.Similar therewith, Chinese invention patent CN201310319303.5, which is disclosed, uses a kind of non-polar solven and polarity
In the presence of ultrasonic wave, extraction solvent and spent bleaching clay are mixed as extraction solvent for solvent and both mixed solvents
Stirring is closed, the oil adsorbed in desorption, extracting spent bleaching clay, is finally washed with water, filters, dried carclazyte, making carclazyte table
Face is recovered, and activity is regenerated, and the oil of spent bleaching clay absorption is reclaimed.However, the above processing method is suitable only for absorption
The discarded carclazyte of certain grease, processing procedure need to use substantial amounts of organic solvent, and investment is high, and process is not environmentally.Aromatic hydrocarbon refining is white
Soil there is many alkylated reactions and olefinic polyreaction, simply uses solvent extraction method not in use
Properly.
The content of the invention
The present invention post-processes the problems such as difficult for the aromatic hydrocarbon refining carclazyte of adsorption saturation, there is provided a kind of aromatic hydrocarbon refining carclazyte
Renovation process.
A kind of renovation process of aromatic hydrocarbon refining carclazyte, the processing method are carried out as follows：
(1) the aromatic hydrocarbon refining carclazyte of adsorption saturation is taken 350 DEG C~850 DEG C in 120 DEG C~150 DEG C drying, moving air
Roasting 2~8 hours, the moving air after roasting after the reactor burning equipped with exhaust combustion catalyst by discharging；At tail gas
A part for reason and this technique, can reach non-pollution discharge by the whole technique of vent gas treatment
(2) carclazyte after roasting in atmosphere is taken, the carbon dioxide for being entrained with vapor is passed through, 400 DEG C~750
DEG C processing 1~9 hour；
(3) 1 part of the carclazyte learnt from else's experience after being entrained with the carbon dioxide treatment of vapor, 0.01~0.3 part of inorganic acid is added
Solution, activate 1~10 hour, 350 DEG C~850 DEG C roastings are to obtain the Regeneration Bleaching Clay in moving air.
The described carbon dioxide for being entrained with vapor, refer to the mixed gas of vapor and carbon dioxide.
The described carbon dioxide for being entrained with vapor, the wherein volume fraction of vapor are 0.5-30%.
Described inorganic acid includes one or more combinations in sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid.
Described inorganic acid mass concentration is 10%~90%.
Mass concentration after a variety of inorganic acid combinations refers to the concentration sum of each inorganic acid in system.
Described acid activation temperature is 10 DEG C~90 DEG C.
The described reactor equipped with exhaust combustion catalyst includes fixed bed, preferably fluid bed, fixed bed.
Described exhaust combustion catalyst activity component is Pt, Pd, Mn, Ce metal simple-substance or metal oxide；Catalysis
The carrier of agent includes aluminum oxide, silica, titanium oxide, carborundum.
A kind of renovation process of aromatic hydrocarbon refining carclazyte, described exhaust combustion catalyst can be selected from and industrially apply
Catalyst, such as S ü d-Chemie companies EnviCat catalyst series (including ENVICAT N2O-S) and Fushun petrochemical industry
Graduate FYP catalyst series (including FYP-1, FYP-2 etc.), but this is not limited only to, such as can also use homemade honeycomb
Pt, Pd, Mn, Ce catalyst of the alumina load of ceramic coating or homemade ceramic honey comb coating it is titania oxide supported
Pt, Pd, Mn, Ce catalyst, either silica supported Pt, Pd, Mn, Ce catalyst of homemade ceramic honey comb coating or from
Pt, Pd, Mn, Ce catalyst of the carborundum load of the ceramic honey comb coating of system.
Described exhaust combustion reaction temperature is 160 DEG C~240 DEG C, gas space velocity 4000h-1~12000h-1。
Exhaust combustion generation gas outlet of the present invention uses online gas chromatography-mass spectrum and infrared radiation detection apparatus joint-detection.
Specific surface area, pore volume and the aperture of carclazyte after the carclazyte and reprocessing of adsorption saturation of the present invention use nitrogen adsorption
Method determines.
Beneficial effect
Using the carclazyte of method provided by the invention processing aromatic hydrocarbon refining adsorption saturation, technical process is simple, whole process
Green, without noxious gas emission.Carclazyte specific surface area, pore volume and the aperture obtained by this method processing obtains effective extensive
It is multiple, it is circularly used in process for refining and removing olefin from aromatic hydrocarbon.
Embodiment
With following embodiment, the invention will be further described, but the present invention is not limited to these embodiments.
Embodiment 1：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 120 DEG C of drying, flowing
380 DEG C are calcined 8 hours in air, and the gas vent after roasting presses 4000h-1Air speed ratio load a kind of EnviCatN2O-S and urge
Agent, the organic component not sufficiently combusted in reaction removing roasting process at 160 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 0.8% is passed through, is handled 6 hours at 750 DEG C.Take and be entrained with vapor
1 part of carclazyte after carbon dioxide treatment, 0.02 part of 20% sulfuric acid is added, activated 3 hours at 40 DEG C, 400 in moving air
DEG C roasting i.e. obtain the Regeneration Bleaching Clay A.
Embodiment 2：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 150 DEG C of drying, flowing
850 DEG C are calcined 2 hours in air, and the gas vent after roasting presses 12000h-1Air speed ratio load a kind of EnviCat N2O-S
Catalyst, the organic component not sufficiently combusted in reaction removing roasting process at 240 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 20% is passed through, is handled 6 hours at 550 DEG C.Take and be entrained with the two of vapor
1 part of carclazyte after carbonoxide processing, 0.3 part of 10% nitric acid is added, is activated 1 hour at 90 DEG C, 550 DEG C of roastings in moving air
Burn and obtain the Regeneration Bleaching Clay B.
Embodiment 3：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 150 DEG C of drying, flowing
600 DEG C are calcined 2 hours in air, and the gas vent after roasting presses 8000h-1Air speed ratio load a kind of EnviCatN2O-S and urge
Agent, the organic component not sufficiently combusted in reaction removing roasting process at 200 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 30% is passed through, is handled 1 hour at 750 DEG C.Take and be entrained with the two of vapor
1 part of carclazyte after carbonoxide processing, 0.1 part of 30% phosphoric acid is added, is activated 1 hour at 75 DEG C, 650 DEG C of roastings in moving air
Burn and obtain the Regeneration Bleaching Clay C.
Embodiment 4：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 140 DEG C of drying, flowing
550 DEG C are calcined 2 hours in air, and the gas vent after roasting presses 7000h-1Air speed ratio load a kind of FYP-1 catalyst,
Organic component not sufficiently combusted in reaction removing roasting process at 220 DEG C of fixed bed.Carclazyte after being calcined in air, is passed through water
Vapor volume fraction is 15% carbon dioxide, is handled 4 hours at 680 DEG C.Take at the carbon dioxide for being entrained with vapor
1 part of carclazyte after reason, 0.2 part of 20% hydrochloric acid is added, activated 1 hour at 80 DEG C, 550 DEG C of roastings are to obtain in moving air
The Regeneration Bleaching Clay D.
Embodiment 5：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 130 DEG C of drying, flowing
580 DEG C are calcined 6 hours in air, and the gas vent after roasting presses 9000h-1Air speed ratio load a kind of homemade ball-type catalysis
(Pt contents are that 0.1%, Pd contents are that 0.15%, Mn contents are that 0.5%, Ce contents are 1.3%), at 160 DEG C of fluid bed for agent
Not sufficiently combusted organic component in reaction removing roasting process.Carclazyte after being calcined in air, is passed through vapor volume fraction
For 22% carbon dioxide, handled 3 hours at 710 DEG C.Take the carclazyte after the carbon dioxide treatment for being entrained with vapor 1
Part, 50% hydrochloric acid of 0.1 part of addition, activated 2 hours at 80 DEG C, 580 DEG C of roastings are to obtain the Regeneration Bleaching Clay E in moving air.
Embodiment 6：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 130 DEG C of drying, flowing
590 DEG C are calcined 3 hours in air, and the gas vent after roasting presses 9000h-1Air speed ratio load a kind of EnviCatN2O-S and urge
Agent, the organic component not sufficiently combusted in reaction removing roasting process at 230 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 25% is passed through, is handled 3 hours at 510 DEG C.Take and be entrained with the two of vapor
1 part of carclazyte after carbonoxide processing, adds 0.03 part 50% of sulfuric acid and 0.01 part 20% of phosphoric acid, and it is small that 5 are activated at 60 DEG C
When, in moving air 450 DEG C of roastings obtain the Regeneration Bleaching Clay F.
Embodiment 7：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 130 DEG C of drying, flowing
590 DEG C are calcined 3 hours in air, and the gas vent after roasting presses 9000h-1Air speed ratio load a kind of EnviCatN2O-S and urge
Agent, the organic component not sufficiently combusted in reaction removing roasting process at 230 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 25% is passed through, is handled 3 hours at 510 DEG C.Take and be entrained with the two of vapor
1 part of carclazyte after carbonoxide processing, adds 0.08 part 40% of sulfuric acid and 0.1 part 15% of hydrochloric acid, and it is small that 5 are activated at 60 DEG C
When, in moving air 450 DEG C of roastings obtain the Regeneration Bleaching Clay G.
Embodiment 8：
Sinopec Yangzi Petrochemical Co's aromatic hydrocarbon refining carclazyte of adsorption saturation is taken in 130 DEG C of drying, flowing
590 DEG C are calcined 3 hours in air, and the gas vent after roasting presses 9000h-1Air speed ratio load a kind of EnviCatN2O-S and urge
Agent, the organic component not sufficiently combusted in reaction removing roasting process at 230 DEG C of fixed bed.It is white after being calcined in air
Soil, the carbon dioxide that vapor volume fraction is 25% is passed through, is handled 3 hours at 510 DEG C.Take and be entrained with the two of vapor
1 part of carclazyte after carbonoxide processing, 0.1 part 30% of sulfuric acid, 0.1 part 15% of hydrochloric acid and 0.05 part 10% of phosphoric acid are added,
Activated 5 hours at 60 DEG C, 450 DEG C of roastings are to obtain the Regeneration Bleaching Clay H in moving air.
The testing result of the product of table 1.
Take the Regeneration Bleaching Clay H and the fresh carclazyte of aromatic hydrocarbon refining to be respectively charged into fixed bed reactors, be 180 in reaction temperature
DEG C, paraxylene mass space velocity is 2h-1Under conditions of, the alkene in Arene removal, 2 institutes are the results are shown in Table after reacting 100 hours
Show.
The Regeneration Bleaching Clay H of table 2 and the fresh carclazyte deolefination performance of aromatic hydrocarbon refining
Although the present invention is described in detail herein with reference to exemplary embodiment it should be appreciated that this
Invention is not limited to the embodiment.With this area common skill and it the personnel instructed herein can be obtained will appreciate that in this hair
Other changes, modification and embodiment in bright scope.Therefore, the present invention should be as one man wide with claim described below
Explain free burial ground for the destitute.
Claims (8)
- A kind of 1. renovation process of aromatic hydrocarbon refining carclazyte, it is characterised in that：Described renovation process is carried out as follows：(1) aromatic hydrocarbon refining carclazyte 350 DEG C~850 DEG C roastings 2 in 120 DEG C~150 DEG C drying, moving air of adsorption saturation are taken ~8 hours, the moving air after roasting after the reactor burning equipped with exhaust combustion catalyst by discharging；(2) carclazyte after roasting in atmosphere is taken, is passed through the carbon dioxide for being entrained with vapor, 1 is handled at 400-750 DEG C ~9 hours；(3) 1 part of the carclazyte learnt from else's experience after being entrained with the carbon dioxide treatment of vapor, 0.01~0.3 part of inorganic acid solution is added, Activation 1~10 hour, 350 DEG C~850 DEG C roastings are to obtain the Regeneration Bleaching Clay in moving air.
- 2. renovation process according to claim 1, it is characterised in that：Described inorganic acid include sulfuric acid, nitric acid, phosphoric acid, One or more combinations in hydrochloric acid.
- 3. renovation process according to claim 1, it is characterised in that：Described inorganic acid mass concentration be 10%~ 90%.
- 4. renovation process according to claim 1, it is characterised in that：The described carbon dioxide gas for being entrained with vapor The volume fraction of body, wherein vapor is 0.5-30%.
- 5. renovation process according to claim 1, it is characterised in that：Activation temperature in described step (3) is 10 DEG C ~90 DEG C.
- 6. renovation process according to claim 1, it is characterised in that：The described reactor equipped with exhaust combustion catalyst Including fixed bed, fluid bed.
- 7. renovation process according to claim 1, it is characterised in that：Described exhaust combustion catalyst activity component is Pt, Pd, Mn, Ce metal simple-substance or metal oxide, the carrier of catalyst include aluminum oxide, silica, titanium oxide, carbonization Silicon；Either use the oxidation of Pt, Pd, Mn, Ce catalyst or ceramic honey comb coating of the alumina load of ceramic honey comb coating Titanium load Pt, Pd, Mn, Ce catalyst, either silica supported Pt, Pd, Mn, Ce catalyst of ceramic honey comb coating or Pt, Pd, Mn, Ce catalyst of the carborundum load of ceramic honey comb coating.
- 8. renovation process according to claim 1, it is characterised in that：Described exhaust combustion reaction temperature be 160 DEG C~ 240 DEG C, gas space velocity 4000h-1~12000h-1。
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| CN108745275A (en) * | 2018-06-07 | 2018-11-06 | 中国科学院广州地球化学研究所 | A kind of clay mineral sill and its preparation method and application |
| CN109453755A (en) * | 2018-12-08 | 2019-03-12 | 大连福佳·大化石油化工有限公司 | Waste and old clay treatment technique and its processing system |
| CN113636580A (en) * | 2021-07-21 | 2021-11-12 | 四川金象赛瑞化工股份有限公司 | Clay recycling process |
| TWI809256B (en) * | 2019-12-10 | 2023-07-21 | 日商栗田工業股份有限公司 | Regeneration method of carbonic acid-type layered double hydroxide and acid exhaust gas treatment equipment |
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| CN109453755A (en) * | 2018-12-08 | 2019-03-12 | 大连福佳·大化石油化工有限公司 | Waste and old clay treatment technique and its processing system |
| TWI809256B (en) * | 2019-12-10 | 2023-07-21 | 日商栗田工業股份有限公司 | Regeneration method of carbonic acid-type layered double hydroxide and acid exhaust gas treatment equipment |
| CN113636580A (en) * | 2021-07-21 | 2021-11-12 | 四川金象赛瑞化工股份有限公司 | Clay recycling process |
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Application publication date: 20180202 |