CN109880649A - A kind of desulfurizing agent, sulfur method and filter - Google Patents
A kind of desulfurizing agent, sulfur method and filter Download PDFInfo
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- CN109880649A CN109880649A CN201910173441.4A CN201910173441A CN109880649A CN 109880649 A CN109880649 A CN 109880649A CN 201910173441 A CN201910173441 A CN 201910173441A CN 109880649 A CN109880649 A CN 109880649A
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Abstract
The present invention provides a kind of desulfurizing agent, sulfur method and filter, the desulfurizing agent includes: Ternary copper comprising copper oxide, cuprous oxide and copper；And modified activated carbon.After sulphur-containing burning oil passes through Ternary copper, be modified activated carbon adsorption.The advantage of the invention is that, Ternary copper can be effectively improved thiophene, alkylthrophene, dibenzothiophenes and 4, the adsorption activity and selectivity of the low activities sulfide such as 6- dimethyl Dibenzothiophene, to improve cocoanut active charcoal to the adsorbance of such compound, and then improve the desulfurization effect of sulphur-containing burning oil；Desulfurization is carried out in 100ppm gasoline below, diesel oil to sulfur content using desulfurizing agent provided by the present invention, desulfurization degree can reach 90% or more.
Description
Technical field
The present invention relates to technical field of desulfurization, and in particular to a kind of desulfurizing agent, sulfur method and filter.
Background technique
Currently, social modernization's progress faster, the consumption of fuel oil for vehicles is growing day by day.It is produced by the burning of sulphur-containing burning oil
Raw environmental pollution is well known the harm of human health, thus the environmental regulation of country is increasingly strict.Exploitation is high
Economical fuel oil depth and ultra-deep desulfurization technology are imitated, the fuel oil quality standard for reaching low-sulfur as early as possible has great importance.
Containing there are many sulfide in fuel oil, wherein the electron cloud of alcohol ethers sulfide and benzothiophene (BT) because of sulphur atom
Density is larger, active higher and easy removing；For thiophene (T), alkylthrophene (Cn-T), dibenzothiophenes (DBT) and 4,
The low sulfur-containing compound removing of 6- dimethyl Dibenzothiophene (4,6-DMDBT) isoreactivity is then more difficult.
In numerous deep desulfurization of fuel oil technique, operating condition, lower that absorption method deep desulfurization of fuel oil is mitigated by it
Desulphurization cost and be considered as a kind of there is stronger competitiveness and wide to the advantages that special selectivity of complicated sulfur-containing compound
The ultra-deep desulfurization technology of wealthy market prospects.But the removal effect of absorption method desulfurization sulfur-containing compound lower for activity still has
Wait further strengthen.
Summary of the invention
The purpose of the present invention is to provide a kind of desulfurizing agent, sulfur method and filters, traditional in the prior art to solve
Absorption method desulfurization for the lower sulfur-containing compound of activity removal effect difference problem.
To achieve the above object, a kind of desulfurizing agent provided by the invention, the desulfurizing agent includes following components:
Ternary copper, the Ternary copper include copper oxide, cuprous oxide and copper；And
Modified activated carbon.
Optionally, the mass ratio of the Ternary copper and the modified activated carbon is 1:2-5.
Optionally, in the Ternary copper, the mass percentage content of each component is as follows:
Cuprous oxide is 15-40%；
Copper is 45-80%；
Copper oxide is 1-17%.
Optionally, load has metal component on the modified activated carbon.
Optionally, the micropore size range on the modified activated carbon is 0.536-1.290nm.
Optionally, the modified activated carbon is modified cocoanut active charcoal.
Optionally, the modified cocoanut active charcoal uses obtains following preparation method: by cocoanut active charcoal through oxidant oxygen
Change laggard row metal ion load, then roasting obtains the modified cocoanut active charcoal under protective gas atmosphere.
In addition, to achieve the above object, a kind of sulfur method provided by the invention uses above-mentioned desulfurizing agent to sulfur-bearing
Fuel oil carries out desulfurization, after the sulphur-containing burning oil and the Ternary copper are acted on the activity to improve sulfide, then through the modification
Activated carbon adsorption desulfurization.
Optionally, the time that the sulfurous fuels oil is reacted with the Ternary copper and the modified activated carbon is 1-5min.
In addition, to achieve the above object, a kind of desulfurizing filter provided by the invention, including shell, the shell have
One inner cavity is provided with an oil inlet and an oil outlet in communication with the inner cavity respectively, the interior intracavitary alternating on the shell
Ground is provided at least a ternary layers of copper and modified active carbon layer, wherein being ternary layers of copper close to oil inlet setting, leans on
The nearly oil outlet setting is modified active layer of charcoal.
Compared with prior art, the desulfurizing agent comprising Ternary copper, sulfur method and filter of the invention have following excellent
Point:
Ternary copper can be effectively improved thiophene, alkylthrophene, dibenzothiophenes and 4,6- dimethyl Dibenzothiophene etc.
The adsorption activity and selectivity of low activity sulfide, to improve cocoanut active charcoal to the adsorbance of such compound, Jin Ergai
The desulfurization effect of kind sulphur-containing burning oil；Using desulfurizing agent provided by the present invention to sulphur sulfur-bearing in 100ppm gasoline below, diesel oil
Desulfurization is carried out, desulfurization degree can reach 90% or more；
Ternary copper, deoxidation in reaction process, in the surface shape of Ternary copper are produced using the reduction reaction of cupric oxide powder
At a large amount of micropores, its catalytic action is further enhanced, facilitates the adsorptive selectivity for improving low activity sulfide and absorption is lived
Property；
It is provided by the invention containing sulfur catalyst after use can activating and regenerating, be used repeatedly, to reduce user
Use cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the desulfurizing filter that one embodiment of the invention provides；
Fig. 2 be another embodiment of the present invention provides desulfurizing filter structural schematic diagram；
Fig. 3 be another embodiment of the present invention provides desulfurizing filter structural schematic diagram.
[the reference numerals are as follows]:
100- filter；
110- shell；
120- oil inlet；
130- oil outlet；
140- desulfurizing agent；
141- ternary layers of copper, 142- modified active layer of charcoal；
150- separation layer.
Specific embodiment
To keep the purpose of the present invention, advantages and features clearer, below in conjunction with attached drawing to it is proposed by the present invention include three
The various embodiments of the desulfurizing agent of first copper, sulfur method and filter are described in further detail.It should be noted that attached drawing is adopted
With very simplified form and using non-accurate ratio, only to facilitate, lucidly aid in illustrating the embodiment of the present invention
Purpose.
As used in the specification and the appended claims, singular "a", "an" and "the" includes
Plural reference, in addition in addition non-content explicitly points out.As used in the specification and the appended claims, term "or"
Usually carried out with including the meaning of "and/or" using, in addition in addition non-content explicitly points out.It is same or similar in attached drawing
Appended drawing reference represent the same or similar component.
Sulfur method provided by the present invention is primarily directed to sulphur-containing burning oil desulfurization, such as diesel oil, gasoline, especially to containing
Sulfur content 100ppm fuel oil below desulfurization effect it is further preferred that.
Fig. 1 show filter 100 used in inventive desulfurization method, includes shell 110 in filter 100, described
Shell 110 has an inner cavity, is provided with an oil inlet 120 and an oil outlet in communication with the inner cavity on the shell 110
130, the interior intracavitary alternating is filled with ternary layers of copper 141 and modified active layer of charcoal 142.Ternary copper and modified activated carbon are combined,
Constitute the desulfurizing agent of sulfur-containing compound in removing fuel oil.
In one embodiment, shell 110 uses draw ratio for the steel cylindrical tube of 20:1, and oil inlet 120 is arranged in shell
The other end of shell 110 is arranged in one end of body 110, oil outlet 130；Ternary layers of copper 141 is arranged close to oil inlet 120, modified
Active carbon layer 142 is arranged close to oil outlet 130, is additionally provided between ternary layers of copper 141 and modified active layer of charcoal 142 by stainless
The separation layer 150 that steel strainer is constituted.Separation layer 150 is not only used to separate ternary layers of copper 141 and modified active layer of charcoal 142, also uses
To support ternary layers of copper 141.In this way, be vertically arranged when filter 100, and when oil inlet 120 is located at upper end, avoid Ternary copper because
Gravity and sink.According to actual needs, ternary layers of copper 141 and the mass ratio of modified active layer of charcoal 142 are adjusted in the range of 1:2-5
It is whole.
Sulphur-containing burning oil enters after filter 1 from oil inlet 130 to flow out from oil outlet 130 again.Fuel oil is passing through ternary layers of copper
During 141, Ternary copper improves such as thiophene (T), alkylthrophene (Cn-T), dibenzothiophenes (DBT) and 4,6- bis-
The adsorption activity and selection activity of the sulfur-containing compounds such as methyldibenzothiophene (4,6-DMDBT), make it pass through modified active
It can be adsorbed when layer of charcoal 142 and be separated with fuel oil.During actual treatment, every 1g desulfurizing agent be can act on about
The sulfur content of 2300-3000g is in 100ppm fuel oil below.
It should be appreciated that the present invention is not intended to limit the concrete shape and size of the shell 110 of filter 100.Other real
It applies in example, filter 100 can also use the shell 110 of U-shaped structure or other forms as shown in Figure 2.
In addition, the present invention is to the ternary layers of copper 141 filled in filter 100 and the specific number of plies of modified active layer of charcoal 142
Also there is no limit.For example, ternary layers of copper 141 and modified active layer of charcoal 142 are disposed as two in filter 1 shown in Fig. 3
Layer, and ternary layers of copper 141 and modified active layer of charcoal 142 are arranged alternately, adjacent ternary layers of copper 141 and modified cocoanut active charcoal
Separation layer 150 is provided between layer 142.As long as in fact, guaranteeing that two kinds of component numbers of plies of desulfurizing agent 140 are identical and alternately set
Set, and be provided that ternary layers of copper 141 close to oil inlet 120, close to the setting of oil outlet 130 be modified active layer of charcoal 142 i.e.
It can.
The ingredient of Ternary copper used in the embodiment of the present invention includes copper oxide, cuprous oxide and copper.As one kind
Selection, cuprous oxide mass percent are 15-40%；The mass fraction of copper is 45-80%；The mass percent of copper oxide is 1-
17%.
In Ternary copper, the mass percentage of cuprous oxide can for 15%, 17%, 20%, 21%, 24%, 28%,
29%, 33%, 38% or 40% etc.；The mass percentage of copper can for 45%, 50%, 55%, 60%, 63%, 66%,
70%, 73%, 78% or 80% etc.；The mass percentage of copper oxide can for 1%, 2%, 3%, 5%, 8%, 9%, 13%,
15% or 17% etc..
There are many preparation methods of Ternary copper, for example, referring to method disclosed in CN1072870, is reduced into using mantoquita
After copper powder, then cuprous oxide and copper oxide are generated under the effect of the oxygen；Referring to application No. is disclosed in 201610331008.5
Method occurs comproportionation reaction by copper powder and copper oxide and produces Ternary copper；Or reduction reaction is carried out by copper oxide and produces three
First copper etc..It is of course also possible to directly adopt commercially available ternary copper products.It should be appreciated that when using distinct methods preparation Ternary copper
May because of raw material difference and cause in final product containing other micro substances.
Preferably, when being used as desulphurization catalyst, particle surface is preferably used to be formed with the Ternary copper of micropore.Such as
This, catalyst has relatively large specific surface area, is capable of increasing its contact surface with sulphur-containing burning oil, improves catalytic effect.
Different preparation conditions can obtain the different Ternary copper of constituent content.
Another component of the modified activated carbon as desulfurizing agent, effect are absorption sulfur-containing compounds.Modified activated carbon can be with
Commercial product is directlyed adopt, can also be prepared using following methods:
(1) magnesium oxide/absorbent charcoal: active carbon is added in oxidizing agent solution, controlled at 30-60 DEG C, oscillation, then
It is washed with deionized, is dried again after suction filtration to get oxidation modification active carbon is arrived；
(2) equi-volume impregnating carried metal component: by modified activated carbon incipient impregnation in metal salt solution, room temperature
Lower standing makes metal component be carried on modified active carbon surface；There is the modified activated carbon of metal component dry load again, and
Protective gas, such as N2It roasts under atmosphere, is finally sieved.
The content of metal of modified activated carbon can be changed by regulating and controlling the concentration of maceration extract.It is appropriate in dipping process
Improving temperature can be improved pickling efficiency.
In some embodiments of the invention, oxidizing agent solution is nitric acid solution, and maceration extract uses iron nitrate solution, finally
Obtain the modified activated carbon that load has iron oxide.It is appreciated that oxidizing agent solution can also be that hydrogenperoxide steam generator, sulfuric acid are molten
Liquid, hydrochloric acid solution, chloroazotic acid etc..In further embodiments, when using other metal salt solutions as maceration extract, obtaining load has
The modified activated carbon of respective metal component obtains the modified of loaded copper oxide and lives for example, by using copper nitrate solution as maceration extract
Property charcoal；Using cerous nitrate solution as maceration extract, the modified activated carbon etc. that load has cerium oxide is obtained.
Further study show that when modified activated carbon using cocoanut active charcoal as raw material, and modified coconut husk obtained
The particle size of active carbon is in 40 mesh between 20 mesh, and surface micropore size range is in 0.536-1.290nm, by modified coconut husk
Active carbon is filled in filter 100, and porosity is suitble to passing through for sulphur-containing burning oil, and has biggish absorption to sulfur-containing compound
Amount.
Used desulfurizing agent in the present invention after suitably handling can activating and regenerating, to reuse,
Reduce the economic cost for the treatment of of fuels.
Activating and regenerating treatment process specifically is as follows: first using steam blowing Ternary copper, make to adhere in Ternary copper contains
Sulphur fuel oil volatilization is complete, and then Ternary copper is done in reusable heat wind.
It for volatile matter, is recycled after its condensation, obtains the high fuel oil of sulfur content through water-oil separating, subsequent can use again adds
Hydrogen doctor treatment is handled.
Modified cocoanut active charcoal also carries out activating and regenerating processing using identical method.
The desulfurization effect of sulfur method of the present invention is evaluated followed by the actual treatment to sulphur-containing burning oil.
Embodiment 1
In the present embodiment, the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:2.Wherein, copper oxide in Ternary copper
Mass percent is 1%, the mass fraction of copper is 75%, the mass fraction of cuprous oxide is 21%.Modified cocoanut active charcoal table
Face loads iron oxide, and load capacity is the 5% of cocoanut active charcoal quality.The shell 110 of filter 100 uses draw ratio for 20:1
Cylindrical steel tubes, one layer of ternary layers of copper 141 of setting and one layer of coconut activated layer of charcoal 142 of modification in shell 110.
Desulfurization process is carried out using gasoline of the above-mentioned desulfurizing filter 100 to sulfur content 95ppm, gasoline is in filter 100
The interior residence time is 5min.Gasoline sulfure content after detection processing is 5.5ppm, and desulfurization degree reaches 94.2%.
Embodiment 2
The present embodiment the difference from embodiment 1 is that: in Ternary copper, the mass percent of copper oxide is the quality of 1%, copper
Score is 56%, the mass fraction of cuprous oxide is 43%.Remaining parameter of desulfurizing agent and the parameter of desulfurization test with implementation
Example 1 is identical.Gasoline after detection processing, sulfur content 5ppm, desulfurization degree 94.7%.
Embodiment 3
The present embodiment the difference from embodiment 1 is that: in Ternary copper, the mass percent of copper oxide is the quality of 3%, copper
Percentage is 61%, the mass percent of cuprous oxide is 28%.Remaining parameter of desulfurizing agent and the parameter of desulfurization test with
Embodiment 1 is identical.Gasoline after detection processing, sulfur content 6.2ppm, desulfurization degree reach 93.4%.
Embodiment 4
In the present embodiment, the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:3.Wherein, copper oxide in Ternary copper
Mass percent is 17%, the mass fraction of copper is 40%, the mass fraction of cuprous oxide is 35%.Modified cocoanut active charcoal table
Face loads iron oxide, and load capacity is the 8% of cocoanut active charcoal quality.The shell 110 of filter 100 uses draw ratio for 20:1
Cylindrical steel tubes, one layer of ternary layers of copper 141 of setting and one layer of coconut activated layer of charcoal 142 of modification in shell 110.
Desulfurization process is carried out using gasoline of the above-mentioned desulfurizing filter 100 to sulfur content 98ppm, gasoline is in filter 100
The interior residence time is 3min.Gasoline sulfure content after detection processing is 4.3ppm, and desulfurization degree reaches 95.6%.
Embodiment 5
The present embodiment and the difference of embodiment 4 are: in Ternary copper, the mass percent of copper oxide is the matter of 16%, copper
Amount percentage is 51%, the mass percent of cuprous oxide is 26%.Remaining parameter of desulfurizing agent and the parameter of desulfurization test are equal
It is same as Example 4.Gasoline sulfure content after detection processing is 5ppm, and desulfurization degree reaches 94.8%.
Embodiment 6
The present embodiment and the difference of embodiment 4 are: in Ternary copper, the mass percent of copper oxide is the matter of 17%, copper
Amount percentage is 54%, the mass percent of cuprous oxide is 21%.Remaining parameter of desulfurizing agent and the parameter of desulfurization test are equal
It is same as Example 4.Gasoline sulfure content after detection processing is 4.5ppm, and desulfurization degree reaches 95.4%.
Embodiment 7
In the present embodiment, the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:5.Wherein, copper oxide in Ternary copper
Mass percent is 8%, the mass fraction of copper is 52%, the mass fraction of cuprous oxide is 30%.Modified cocoanut active charcoal table
Face loads iron oxide, and load capacity is the 10% of cocoanut active charcoal quality.The shell 110 of filter 100 uses draw ratio for 20:
1 cylindrical steel tubes, the one layer of ternary layers of copper 141 of interior setting of shell 110 and one layer of coconut activated layer of charcoal 142 of modification.
Desulfurization process is carried out using diesel oil of the above-mentioned filter 100 to sulfur content 95ppm, diesel oil is in filter 100
Residence time is 1min.Gasoline sulfure content after detection processing is 7.3ppm, and desulfurization degree reaches 92.3%.
Embodiment 8
The present embodiment and the difference of embodiment 7 are: the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:4.Wherein,
The mass percent of copper oxide is 12% in Ternary copper, the mass fraction of copper is 62%, the mass fraction of cuprous oxide is 22%.
Modified cocoanut active charcoal area load iron oxide, load capacity are the 9% of cocoanut active charcoal quality.
When desulfurization is tested, residence time of the diesel oil in filter 100 is 2min.Diesel oil sulfur content after detection processing is
7.3ppm, desulfurization degree reach 92.3%.
Embodiment 9
The present embodiment and the difference of embodiment 7 are: the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:4.Wherein,
The mass percent of copper oxide is 6% in Ternary copper, the mass fraction of copper is 68%, the mass fraction of cuprous oxide is 15%.
Modified cocoanut active charcoal area load cerium oxide, load capacity are the 6% of cocoanut active charcoal quality.
Desulfurization test is carried out to the diesel oil that sulfur content is 97ppm, residence time of the diesel oil in filter 100 is 2min.
Diesel oil sulfur content after detection processing is 7ppm, and desulfurization degree reaches 92.7%.
Embodiment 10
The present embodiment and the difference of embodiment 7 are: the mass ratio of Ternary copper and modified cocoanut active charcoal is 1:5.Wherein,
The mass percent of copper oxide is 13% in Ternary copper, the mass fraction of copper is 47%, the mass fraction of cuprous oxide is 33%.
Modified cocoanut active charcoal area load copper oxide, load capacity are the 7% of cocoanut active charcoal quality.
Desulfurization test is carried out to the diesel oil that sulfur content is 97ppm, residence time of the diesel oil in filter 100 is 2min.
Diesel oil sulfur content after detection processing is 9ppm, and desulfurization degree reaches 90.7%.
Although present disclosure is as above, however, it is not limited to this.Those skilled in the art can carry out the present invention each
Kind modification and variation is without departing from the spirit and scope of the present invention.In this way, if these modifications and changes of the present invention belongs to this
Within the scope of invention claim and its equivalent technologies, then the present invention is also intended to include these modifications and variations.
Claims (10)
1. a kind of desulfurizing agent, which is characterized in that the desulfurizing agent includes following components:
Ternary copper, the Ternary copper include copper oxide, cuprous oxide and copper；And
Modified activated carbon.
2. a kind of desulfurizing agent according to claim 1, which is characterized in that the matter of the Ternary copper and the modified activated carbon
Amount is than being 1:2-5.
3. a kind of desulfurizing agent according to claim 1 or 2, which is characterized in that in the Ternary copper, the quality hundred of each component
Divide as follows than content:
Cuprous oxide is 15-40%；
Copper is 45-80%；
Copper oxide is 1-17%.
4. a kind of desulfurizing agent according to claim 1 or 2, which is characterized in that load has metal on the modified activated carbon
Component.
5. a kind of desulfurizing agent according to claim 4, which is characterized in that the micropore size range on the modified activated carbon
For 0.536-1.290nm.
6. a kind of desulfurizing agent according to claim 5, which is characterized in that the modified activated carbon is that modification is coconut activated
Charcoal.
7. a kind of desulfurizing agent according to claim 6, which is characterized in that the modified cocoanut active charcoal is using following preparation
Method obtains: by cocoanut active charcoal through oxidizing laggard row metal ion load, then roasting under protective gas atmosphere
Obtain the modified cocoanut active charcoal.
8. a kind of sulfur method uses and carries out desulfurization to sulphur-containing burning oil such as the described in any item desulfurizing agents of claim 1-7,
It is characterized in that, after the sulphur-containing burning oil and the Ternary copper are acted on the activity to improve sulfide, then through the modified active
Charcoal adsorbs desulfurization.
9. a kind of sulfur method according to claim 8, which is characterized in that the sulfurous fuels oil and the Ternary copper and
The time of the modified activated carbon reaction is 1-5min.
10. a kind of desulfurizing filter, which is characterized in that including shell, the shell has an inner cavity, is provided on the shell
An oil inlet in communication with the inner cavity and an oil outlet respectively, it is described it is interior it is intracavitary be alternately arranged an at least ternary layers of copper and
Modified active carbon layer is modification close to oil outlet setting wherein being ternary layers of copper close to oil inlet setting
Active carbon layer.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104203371A (en) * | 2012-02-06 | 2014-12-10 | 环球油品公司 | Method of making supported copper adsorbents having copper at selectively determined oxidation levels |
| CN108697976A (en) * | 2015-11-10 | 2018-10-23 | 环球油品公司 | The copper adsorbent guard bed for alkynes converter |
-
2019
- 2019-03-07 CN CN201910173441.4A patent/CN109880649A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104203371A (en) * | 2012-02-06 | 2014-12-10 | 环球油品公司 | Method of making supported copper adsorbents having copper at selectively determined oxidation levels |
| CN108697976A (en) * | 2015-11-10 | 2018-10-23 | 环球油品公司 | The copper adsorbent guard bed for alkynes converter |
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Application publication date: 20190614 |