CN103191697B - Desulfurizing adsorbent Ag2O/NaY based on molecular screen and preparation method thereof - Google Patents
Desulfurizing adsorbent Ag2O/NaY based on molecular screen and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a desulfurizing adsorbent Ag2O/NaY based on a molecular screen and a preparation method thereof, belonging to the technical filed of desulfurizing adsorbents. The preparation method mainly comprises the steps of carrier pretreatment based on a urea sublimation and desublimation method; incipient impregnation of a NaY type molecular screen by using a silver salt solution and calcining of the Y type molecular screen. The desulfurizing adsorbent Ag2O/NaY based on a molecular screen has an excellent performance of dispersing the active components of carriers and therefore has an excellent adsorbent desulfurizing performance although the content of Ag2O is little; so that an excellent desulfurizing effect with lower cost can be achieved by using the desulfurizing adsorbent based on a molecular screen to remove disulfides in hydrocarbon fuel.
Description
Technical field
The present invention relates to a kind of molecular screen base adsorbent for deep desulfuration, more specifically, the present invention relates to such molecular screen base adsorbent A g for deep desulfuration
2o/NaY, it has excellent dispersive property to active component, at room temperature has the excellent ability removing disulphide, belongs to desulfuration adsorbent technical field.
Background technology
Along with the development of petro chemical industry, liquefied petroleum gas (LPG), as a kind of chemical industry base stock and New-type fuel, is more and more subject to people's attention.Normal containing H in liquefied petroleum gas (LPG)
2s, mercaptan sulfides, it can cause equipment corrosion in following process process, the poisoning and inactivation of catalyst, the SO that burning produces
xcontaminated environment, forms acid rain, all brings serious impact and destruction to ecological environment, human health and social economy.
Remove mercaptan in LPG most widely used be Mei Luokesi (Merox) technique, its principle is, adds catalyst sulfonation titanium cyanogen cobalt or poly-titanium cyanogen cobalt in sodium hydrate aqueous solution, the mercaptan in LPG and NaOH is reacted and generates sodium mercaptides; Then under the effect of catalyst with air oxidation sodium mercaptides, make it to be converted into disulphide, then different according to disulphide and NaOH density, disulphide be separated, realize alkali liquid regeneration.But in alkali dose step, disulphide and alkali lye separation difficulty, often cause disulphide to remain, cause total sulfur in LPG to exceed standard.Therefore, needed to carry out deep desulfuration removing disulphide wherein before LPG utilizes further.But, for the rarely seen report of research that disulphide removes.
A kind of conventional sulfur method is adsorption desulfurize.JP1994-306377B discloses and carries out with polyvalent metal ion the zeolite adsorbents that ion-exchange obtains, but this adsorbent only can be used for removing of mercaptan in town gas.
CN1820839A discloses a kind of adsorbent, by exchanging y-type zeolite with transition metal, obtains the desulfuration adsorbent that relative crystallinity is 45 ~ 98%.This adsorbent is mainly used in removing thiophene-type sulfide and thio-alcohol sulfide in town gas.
But LPG is different from town gas, from the alkene of LPG often containing a great deal of of refinery, alkene and sulfide are often competed and are adsorbed, and therefore need to carry out the exploitation of selective desulfurization adsorbent to the fuel gas containing alkene.And disulphide has two connected sulphur atoms, its structure and thiophene-type sulfide have very large difference, and in LPG, the sulfide of more than 80% is all exist with the form of disulphide.Therefore, be necessary to develop the deep desulfurization absorbent for disulphide.
The selective absorption of known sulfide occurs in the active sites of adsorbent, the impact that the size receptor 1 activity position of adsorption capacity is how many, and therefore improving active component content is on the sorbent the main path improving adsorption capacity.But the too much active component of load easily causes active component to reunite, even block carrier duct, cause adsorption capacity to decline, active component is not fully utilized.Therefore the key improving adsorbent capacity is to promote the dispersion of active component in adsorbent duct.
Summary of the invention
The object of the present invention is to provide a kind of method, by urea sublimating and condensing pretreatment NaY molecular sieve, first urea is evenly distributed in molecular sieve pore passage, and then the desulphurizing activated component of load, again by the method removing urea of calcining, namely obtained can have good desulfuration selectivity and excellent desulfurization performance at ambient temperature.
A kind of Ag of the present invention
2o/NaY desulfuration adsorbent, its desulfuration adsorbent is made up of starting material and carrier, and described starting material is active A g
+nitrate, described carrier is through the pretreated faujasite-type NaY molecular sieve of urea.
A kind of desulfuration adsorbent Ag based on molecular sieve of the present invention
2the preparation method of O/NaY, comprises the following steps:
(A) the former powder of the NaY molecular sieve roasting 4h under 500-600 DEG C (preferably 550 DEG C) will having faujasite structure, naturally cools to room temperature;
(B) by the sieve particle that (A) step obtains, 40-60 object granulating carrier is made;
(C) water absorption of determination step (B) sieve particle carrier, gets the granulating carrier that (B) step obtains, dries to constant weight; Then by the carrier after oven dry, drip distilled water, limit edged vibrates, until carrier is completely moistening, and has obvious water to exist on the wall, and no longer loaded body absorption, calculates unit mass carrier institute water absorption;
(D) the granulating carrier (B) step obtained and the urea of pulverize are placed in closed container, vacuumize rear closed container, heating, distil to make urea and enter granulating carrier duct, then room temperature is down to, to make urea sublimate in carrier duct, thus be uniformly distributed in carrier duct, the quality of preferred urea is that granulating carrier obtains 1%-5%; The temperature that heating makes urea distillation enter granulating carrier duct is: 180 DEG C are carried out 12 hours.
(E) take carrier after step (D) pretreatment, and take AgNO
3, according to the water absorption of the unit mass carrier that step (C) obtains, calculate the amount of deionized water that alleged carrier needs, take the deionized water of respective amount and and AgNO
3wiring solution-forming; Carrier after the pretreatment taken is placed in container vacuumize, the AgNO simultaneously will configured
3solution is added drop-wise on carrier, and dropping limit, limit vibrates, until all dropwised by solution; Then by seal of vessel, flood under being placed in room temperature; The preferred 12h of dip time; Preferred AgNO
3consumption for making Ag in final products
2the content of O is 1-10wt%.
(F) step (E) load there is AgNO
3naY molecular sieve dry after take out, then put into Muffle furnace roasting, to remove urea, and impel the conversion of active component presoma, gained is Ag
2o/NaY desulfuration adsorbent.In Muffle furnace, roasting is preferred: roasting 2-4h under air, under 500-550 DEG C (more preferably 550 DEG C).
Thinking of the present invention: known metal ion is short of electricity daughter, has the ability obtaining electronics, can regard lewis acid as, and in urea, nitrogen-atoms, containing lone pair electrons, has electron donation, can regard lewis base as.In the outer surface that the pretreatment of urea sublimating and condensing makes urea be uniformly distributed in molecular sieve carrier and duct, due to the electrostatic interaction between metal ion and lone pair electrons, impel metal ion to be also uniformly distributed in carrier outer surface and duct, thus make active component also having higher dispersiveness compared with during heavy load amount.
The advantage of high-efficiency desulfurization adsorbent of the present invention: silver oxide has excellent disulphide adsorption capacity, the present invention with faujasite-type NaY molecular sieve for carrier, after the pretreatment of urea sublimating and condensing, adopt the method for incipient impregnation that silver oxide active component is highly dispersed in carrier surfaces externally and internally.Adopt urea pretreatment, active component is covered in carrier surfaces externally and internally monolayer, be conducive to the dispersiveness and the utilization ratio that improve silver oxide active component.The advantage of which is that disulphide is only absorbed in surface oxidation silver active sites, can not affect carrier framework structure, thus improve service life.
The active component of molecular screen base adsorbent to load for desulfurization of the present invention has more excellent dispersive property, thus has more excellent adsorption desulfurize performance, although the Ag wherein comprised
2o is a small amount of.Therefore, during the disulphide utilizing molecular screen base desulfuration adsorbent of the present invention to remove in hydrocarbon fuel, excellent desulfurized effect can be reached at lower cost.This adsorbent mainly for molecular structure different from thiophene-type sulfide containing the disulphide of two sulphur atoms.
The invention has the beneficial effects as follows: namely this desulfuration adsorbent at room temperature has excellent desulfurization performance, avoiding in sweetening process because heating the energy consumption consumption caused; This desulfuration adsorbent can reduce the reunion of active component, has excellent dispersive property to silver oxide active component; This desulfuration adsorbent has good desulfuration selectivity, namely still has good desulfurized effect when there being alkene to exist; Compared with desulfuration adsorbent prepared by this desulfuration adsorbent and conventional ion-exchange, improve the utilization rate of silver, adsorption activity position is distributed in carrier surface, on the skeleton structure of carrier almost without affecting.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of NaY molecular sieve.
Fig. 2 is urea pretreated carrier load difference amount Ag in embodiment 2
2the XRD collection of illustrative plates of O gained adsorbent.
Fig. 3 be carrier through urea pretreatment with without the different amount Ag of urea pretreatment load
2the working sulfur capacity contrast of O gained adsorbent.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail, but the present invention is not limited to following examples.
The present invention proposes Ag
2o/NaY desulfuration adsorbent and preparation method thereof.Adopt the NaY molecular sieve with faujasite structure as carrier; In order to make Ag
2o has higher activity and adopts AgNO
3as starting material.The preparation method of desulfurizing agent adopts equi-volume impregnating, by starting material AgNO
3load is on carrier NaY.The pretreatment of urea sublimating and condensing is carried out to carrier, makes Ag
2o has good distribution on NaY carrier, and from change AgNO
3use amount set about, reach and change Ag on carrier NaY
2the object of the load capacity of O, thus make desulfurizing agent reach best desulfurized effect and minimum cost.
Ag of the present invention
2o/NaY regenerating desulfurization adsorbent, its desulfuration adsorbent is made up of starting material and carrier, and described starting material is active A g
+nitrate, described carrier is through the pretreated faujasite-type NaY molecular sieve of urea.
Ag of the present invention
2the preparation method of O/NaY regenerating desulfurization adsorbent, comprises the following steps:
(A) by former for NaY molecular sieve powder roasting 4h under 550 ° of C, room temperature is progressively cooled to;
(B) by the sieve particle that (A) step obtains, 40-60 object particle is made;
(C) water absorption of carrier is measured.Get the granulating carrier that a certain amount of (B) step obtains, dry under 110 ° of C to constant weight, then take the carrier after a certain amount of oven dry; drip distilled water, limit edged vibrates, until carrier is completely moistening; and have obvious water to exist on the wall, no longer loaded body absorption.Record unit mass carrier institute water absorption.
(D) the granulating carrier a certain amount of (B) step obtained and the urea of pulverize are placed in closed container; vacuumize rear closed container; in 180 ° of C baking ovens, process 12h enter carrier duct to make urea distil; then slowly room temperature is down to; to make urea sublimate in carrier duct, thus be uniformly distributed in carrier duct.
(E) take carrier after a certain amount of pretreatment, take the Ag into vehicle weight 5%
2the AgNO that O is corresponding
3, according to the water absorption of unit mass carrier, calculate the amount of deionized water that alleged carrier needs, take the deionized water of respective amount and and AgNO
3wiring solution-forming;
(F) carrier is placed in container to vacuumize, the AgNO simultaneously will configured
3solution is added drop-wise on carrier, and dropping limit, limit vibrates, until all dropwised by solution; Then by seal of vessel, flood 12h under being placed in room temperature, make AgNO
3be carried on NaY molecular sieve carrier equably;
(G) load there is AgNO
3naY molecular sieve dry under 110 ° of C after take out, then put into roasting 2h under Muffle furnace 500 ° of C, to remove urea, and impel the conversion of active component presoma.Gained is Ag
2o/NaY desulfuration adsorbent.
Fixed bed reactors are utilized to evaluate the desulfurization performance of adsorbent.The desulfuration adsorbent active component high degree of dispersion prepared by the method, has excellent desulfurization performance to disulphide.Under room temperature, air speed is 1h
-1time, Ag
2o/NaY desulfurizing agent working sulfur capacity in the model solution of sulfur-bearing 1000ppmw can reach 90.2mg S/g adsorbent.
Embodiment
In the present invention, adopting the method for absorption, with DMDS (DMDS) for removing object, measuring the adsorption capacity of desulfuration adsorbent.Sulfur content is by being equipped with the gas chromatographic detection of pulsive flame photometric detector (PFPD).The present invention utilizes fixed bed reactors to carry out the desulphurizing activated evaluation of adsorbent, and the model solution of sulfur-bearing 1000ppmw is passed through 3.00g sample of sorbent with certain air speed, is measured the sulfur content in exit by PFPD simultaneously.
Desulfurization performance evaluation experimental model solution used composition is as shown in table 1:
Table 1 model solution composition
Herein, by beginning when exit detects sulphur, namely think to reach and penetrate critical point.The working sulfur capacity of adsorbent is calculated as follows:
Embodiment 1:
(A) take 10gNaY molecular sieve, in Muffle furnace, roasting 4h under 550 ° of C, progressively cools to room temperature, is then pressed into 40-60 object particle; As shown in Figure 1, it is 541.1m that NaY molecular sieve carrier measures its specific area by BET method to the XRD figure of NaY molecular sieve
2/ g.
(B) carrier in a certain amount of (A) is taken, dry in 110 ° of C baking ovens to constant weight, take 1g40-60 object NaY molecular sieve carrier granular, slowly drip deionized water wherein, limit edged vibrates gently, until carrier is completely moistening, and obvious water is had to exist on the wall, no longer loaded body absorption.The water absorption recording unit mass carrier is: 1.52g water/g carrier.
(C) 40-60 object NaY molecular sieve carrier granular 5g is taken, urea together with 1g pulverize is placed in closed container and vacuumizes, then closed container, is placed in 180 ° of C baking ovens and is incubated 12h, then naturally cool to room temperature, carry out urea distillation, pretreatment of sublimating.
(D) starting material AgNO is taken
30.513g, obtains desulfurizing agent with 7.60g deionized water dissolving and prepares solution, then it is slowly dripped on the pretreated NaY molecular sieve carrier vacuumized of urea, limit edged vibration, solution dropwises rear stopping and vacuumizing, closed container, and floods 12h under being placed in room temperature.
(E) taking-up after being dried under 110 ° of C by products therefrom in (D), then puts into roasting 2h under Muffle furnace 500 ° of C, naturally cools to room temperature, obtain desulfuration adsorbent A.
Comparative example 1:
Adopt the method for embodiment 1, save urea pre-treatment step wherein, obtained without the pretreated adsorbent B of urea.
Under room temperature, air speed is 1h
-1time, desulfurization performance evaluation is carried out to adsorbent A and adsorbent B.Desulfurized effect is as shown in table 2:
Table 2 carrier is through urea pretreatment and the desulfurization performance without urea pretreatment gained adsorbent
As shown in Table 2, the desulfuration adsorbent that carrier obtains through urea pretreatment, the desulfuration adsorbent that its working sulfur capacity obtains without urea pretreatment higher than carrier.In the present invention, urea enters microporous molecular sieve inside with gas phase and sublimates after heating sublimation, uniform basic center is formed at carrier surfaces externally and internally, acid metal ion is guided to be dispersed in carrier surfaces externally and internally, compared with time unprocessed with carrier, active component has better dispersiveness.
Embodiment 2:
Adopt the method for embodiment 1, take starting material AgNO respectively
30.00g, 0.073g, 0.220g, 0.367g, 0.513g, 0.733g, obtain desulfurizing agent with 7.60g deionized water dissolving respectively and prepare solution, then carries out incipient impregnation to through the pretreated NaY molecular sieve carrier of urea respectively, dry, roasting, is cooled to room temperature, obtains Ag
2o content is respectively desulfuration adsorbent A1, B1, C1, D1, E1, F1 of 0wt.%, 1wt.%, 3wt.%, 5wt.%, 7wt.%, 10wt.%.
The X ray diffracting spectrum of obtained adsorbent as shown in Figure 2.The XRD spectra of obtained adsorbent is substantially identical with the NaY molecular sieve of non-modified, illustrate dipping and roasting process in, the structure of molecular sieve is still retained well, modified adsorbent still retains the distinctive pore passage structure of NaY molecular sieve, and not generating new crystalline phase or solid solution with carrier function, active component exists with Monolayer Dispersion form at molecular sieve surface.
Comparative example 2:
Adopt the method identical with embodiment 2 and proportioning, carrier uses without the pretreated NaY molecular sieve of urea, obtained Ag
2o content is respectively desulfuration adsorbent A2, B2, C2, D2, E2, F2 of 0wt.%, 1wt.%, 3wt.%, 5wt.%, 7wt.%, 10wt.%.
Under room temperature, air speed is 1h
-1time, desulfurization performance evaluation is carried out to the serial desulfurizing agent of embodiment 2 and comparative example 2.
Table 3 load different content Ag
2the desulfurization performance of adsorbent after O
With Ag in adsorbent
2o percentage composition is abscissa, and the working sulfur capacity of adsorbent is ordinate, and the data according to table 3 are mapped, and see Fig. 3.Shown in figure, the working sulfur capacity of comparative example 2 and embodiment 2 gained adsorbent is because of Ag
2o constituent content is different and different.Comparative example 2 and comparative example 2 gained catalyst, work as Ag
2o constituent content increases to 5wt.% from 0wt.%, and the working sulfur capacity of adsorbent all increases.But work as Ag
2o content, more than after 5wt.%, continues to increase Ag
2o content, the working sulfur capacity of comparative example 2 gained adsorbent E2 and F2 declines on the contrary to some extent, and this is due to too much Ag
2o easily forms cluster, even blocks caused by carrier duct.And for embodiment 2 gained adsorbent E1 and F1, diminish though the increase amplitude of working sulfur capacity has, but still in increase tendency, this just well illustrates that carrier is provided with better dispersive property to active component after urea pretreatment, thus makes adsorbent be provided with higher absorption Sulfur capacity.
Claims (9)
1. the desulfuration adsorbent Ag based on molecular sieve
2the preparation method of O/NaY, is characterized in that,
Comprise the following steps:
(A) the former powder of the NaY molecular sieve roasting 4h at 500-600 DEG C will having faujasite structure, naturally cools to room temperature;
(B) by the sieve particle that (A) step obtains, 40-60 object granulating carrier is made;
(C) water absorption of determination step (B) sieve particle carrier, gets the granulating carrier that (B) step obtains, dries to constant weight; Then by the carrier after oven dry, drip distilled water, limit edged vibrates, until carrier is completely moistening, and has obvious water to exist on the wall, and no longer loaded body absorption, calculates unit mass carrier institute water absorption;
(D) the granulating carrier (B) step obtained and the urea of pulverize are placed in closed container, vacuumize rear closed container, heating, distil to make urea and enter granulating carrier duct, then room temperature is down to, to make urea sublimate in carrier duct, thus be uniformly distributed in carrier duct;
(E) take carrier after step (D) pretreatment, and take AgNO
3, according to the water absorption of the unit mass carrier that step (C) obtains, calculate the amount of deionized water that alleged carrier needs, take the deionized water of respective amount and and AgNO
3wiring solution-forming; Carrier after the pretreatment taken is placed in container vacuumize, the AgNO simultaneously will configured
3solution is added drop-wise on carrier, and dropping limit, limit vibrates, until all dropwised by solution; Then by seal of vessel, flood under being placed in room temperature;
(F) step (E) load there is AgNO
3naY molecular sieve dry after take out, then put into Muffle furnace roasting, to remove urea, and impel the conversion of active component presoma, gained is Ag
2o/NaY desulfuration adsorbent.
2. according to the method for claim 1, it is characterized in that, the temperature of step (A) is 550 DEG C.
3. according to the method for claim 1, it is characterized in that, the quality of step (D) urea is the 1%-5% of granulating carrier.
4. according to the method for claim 1, it is characterized in that, the temperature that step (D) Urea makes urea distillation enter granulating carrier duct is: 180 DEG C are carried out 12 hours.
5. according to the method for claim 1, it is characterized in that, the preferred 12h of step (E) dip time;
6. according to the method for claim 1, it is characterized in that, step (E) AgNO
3consumption for making Ag in final products
2the content of O is 1-10wt%.
7. according to the method for claim 1, it is characterized in that, roasting condition in Muffle furnace: roasting 2-4h under air, at 500-550 DEG C.
8. according to the method for claim 1, it is characterized in that, roasting condition in Muffle furnace: roasting 2h under air, at 500 DEG C.
9. according to claim 1-8 either method prepared by the desulfuration adsorbent Ag based on molecular sieve
2o/NaY.
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| CN104014301A (en) * | 2014-06-20 | 2014-09-03 | 南通三创机械制造有限公司 | Organic sulfide removal agent |
| CN105664659A (en) * | 2016-02-15 | 2016-06-15 | 中国石油大学(北京) | Method for continuous adsorption and removal of carbonyl sulfide and dimethyl disulfide in carbon 4 left after etherification reaction |
| CN106390910B (en) * | 2016-12-02 | 2018-08-31 | 中国工程物理研究院核物理与化学研究所 | A kind of preparation method and applications of difunctional Ag2O/ niobic acids composite adsorbing material |
| CN110813313B (en) * | 2019-11-11 | 2022-03-04 | 安徽理工大学 | Silver oxide/layered double-metal hydroxide compound and preparation and application thereof |
| CN110723741B (en) * | 2019-11-20 | 2021-04-23 | 泰州清润环保科技有限公司 | Green preparation method of AgY molecular sieve for adsorption desulfurization |
| CN111592769A (en) * | 2020-04-17 | 2020-08-28 | 上杭鑫昌龙实业有限公司 | OPGW hydrogen absorption optical fiber filling paste and production process thereof |
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| CN1511629A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院大连化学物理研究所 | Molecular sieve adsorbent for deep sulfide removing and preparation and use |
| CN101259428A (en) * | 2008-04-24 | 2008-09-10 | 福州大学 | Preparation of catalyst for processing industrial wastewater and using method thereof |
| CN101367033A (en) * | 2007-08-15 | 2009-02-18 | 中国石油化工股份有限公司 | Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent |
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| CN1511629A (en) * | 2002-12-30 | 2004-07-14 | 中国科学院大连化学物理研究所 | Molecular sieve adsorbent for deep sulfide removing and preparation and use |
| CN101367033A (en) * | 2007-08-15 | 2009-02-18 | 中国石油化工股份有限公司 | Preparation method for Cu(I)-Y molecular sieve adsorption desulphurizing agent |
| CN101259428A (en) * | 2008-04-24 | 2008-09-10 | 福州大学 | Preparation of catalyst for processing industrial wastewater and using method thereof |
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