CN106512923A - Desulfuration adsorbent for gasoline and preparation method and application thereof - Google Patents
Desulfuration adsorbent for gasoline and preparation method and application thereof Download PDFInfo
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- CN106512923A CN106512923A CN201611093233.6A CN201611093233A CN106512923A CN 106512923 A CN106512923 A CN 106512923A CN 201611093233 A CN201611093233 A CN 201611093233A CN 106512923 A CN106512923 A CN 106512923A
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- desulfuration adsorbent
- triethanolamine
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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
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
-
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a desulfuration adsorbent for gasoline and a preparation method and application thereof. The desulfuration adsorbent consists of the following raw materials in parts by weight: 27-35 parts of illite, 3-7 parts of strontium acetate, 13-21 parts of acrylic acid and 5-13 parts of triethanolamine. The illite is used as a raw material, after the illite is mixed with the strontium acetate and the mixture is ground, the ground mixture is then treated by the acrylic acid and the triethanolamine, then the desulfuration adsorbent is obtained, sulfur capacity is large, selectivity to sulfur is good, the desulfurization percent is high, and sulfur can be removed to be 1 ppmw. In addition, the desulfuration adsorbent is long in service life and is environment-friendly. The desulfuration adsorbent is simple in preparation process, easy to operate, easy to control, stable in performance, low in production cost and suitable for industrial production. When used for desulfurizing gasoline, the desulfuration adsorbent is gentle in process operation conditions, the process can be carried out under ordinary pressure and at low temperature, so that energy consumption is reduced, and the operation cost is also reduced.
Description
Technical field
The present invention relates to sulfur removal material technical field, specifically a kind of desulfuration adsorbent for gasoline and preparation method thereof
And application.
Background technology
Have in Chinese commodity gasoline 70% or so be from heavy oil catalytic cracking process, due to heavy oil feedstock contain it is substantial amounts of
Sulphur, nitrogen, oxygen heteroatom compound and gum asphalt, not only sulfur content is high for catalytically cracked gasoline, also containing substantial amounts of alkene group
Point, in merchantable gasoline, more than 90% sulphur comes from catalytically cracked gasoline, and this causes the sulfur content of China's gasoline will be far beyond
The sulfur content of external gasoline.Therefore, how to reduce Sulfur Content in Catalytic Cracking Gasoline is the key for reducing merchantable gasoline sulfur content.
In national five gasoline quality standard of state that will be carried out of on January 1st, 1, regulation gasoline sulfure content is not higher than 10ppm,
Explore and promote deep desulfurization of gasoline technology become petroleum refining industry in the urgent need to.
The desulfurization technology that oil refining industry is adopted is divided into hydrodesulfurization and non-hydrodesulfurization, and wherein hydrodesulfurization is present
Main desulfurization approach, but when only be down to sulfur content under 10ppm, a large amount of saturation of olefins cause octane number big
Amplitude reduction.Non-hydrodesulfurization is divided into the technologies such as absorption desulfurization, oxidation sweetening, abstraction desulfurization, biological desulphurization again, grinds at present
Study carefully absorption desulfurization technology widely, because which is carried out under conditions of normal temperature and pressure, energy consumption is low, and octane number is hardly damaged
Lose, be one of potential deep desulfuration approach.But it is not enough below desulfurizing agent generally existing of the prior art:1st, desulfurization depth
Degree is inadequate, it is difficult to sulphur is taken off to below 5ppmw;2nd, adsorbent specific surface area is relatively low, and absorption Sulfur capacity is relatively limited;3rd, sweetening process
Operating condition it is harsh and energy consumption is big, operating cost is higher;4th, sweetening process is unfriendly to environment;5th, the selectivity of desulfurizing agent
Low, the life-span is shorter.Additionally, the material such as the more employing activated carbon of existing desulfurizing agent, ZSM-5, seldom related believed using illitic
Breath.
The content of the invention
It is an object of the invention to provide a kind of desulfuration adsorbent for gasoline and its preparation method and application, to solve
The problem proposed in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of desulfuration adsorbent for gasoline, is made up of the following raw material according to weight portion:Illite 27-35 parts, second
Sour strontium 3-7 parts, acrylic acid 13-21 parts, triethanolamine 5-13 parts.
As further scheme of the invention:The desulfuration adsorbent for gasoline, by the following original according to weight portion
Material composition:Illite 29-33 parts, strontium acetate 4-6 parts, acrylic acid 15-19 parts, triethanolamine 7-11 parts.
As further scheme of the invention:The desulfuration adsorbent for gasoline, by the following original according to weight portion
Material composition:31 parts of illite, 5 parts of strontium acetate, 17 parts of acrylic acid, 9 parts of triethanolamine.
Another object of the present invention is to provide a kind of preparation method of the desulfuration adsorbent for gasoline, by following steps group
Into:
1) deionized water of 5.5 times of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its matter
The absolute ethyl alcohol mixing of 2.3 times of amount, is obtained triethanolamine solution;
2) by illite and strontium acetate mixed grinding, excessively 120 mesh sieves, acrylic acid solution is subsequently adding, 66 DEG C is warming up to simultaneously
Stir process 2.3h is sealed at such a temperature, triethanolamine solution is subsequently adding, and is warming up to 79 DEG C and is heated at such a temperature and stirs
Process 8min is mixed, then ultrasonically treated 26min at such a temperature, ultrasonic power is 800W, then is stirred at a temperature of 99-101 DEG C
Mix to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace and obtain final product desulfuration adsorbent.
Another object of the present invention is to provide desulfuration adsorbent application in the oil.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention with illite as raw material, after strontium acetate mixed grinding, then through acrylic acid, process of triethanolamine etc.
Obtained desulfuration adsorbent, Sulfur capacity is big, desulfurization depth good to the selectivity of sulphur is high, sulphur can be taken off to 1ppmw;In addition use the longevity
Life length, non-secondary pollution more friendly to environment, renewable recycling.Preparation process is simple of the present invention, it is easy to operate, it is easily-controllable
System, stable performance, low production cost are suitable to industrialized production.The desulfuration adsorbent of present invention work when desulfurization is carried out to gasoline
Skill operating condition is gentle, can carry out, so as to save energy consumption, reduce running cost under normal pressure and lower temperature.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of desulfuration adsorbent for gasoline is made up of the following raw material according to weight portion:She
27 parts of sharp stone, 3 parts of strontium acetate, 13 parts of acrylic acid, 5 parts of triethanolamine.
5.5 times of deionized water of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution.By illite and strontium acetate mixed grinding, 120 mesh sieves are crossed, then
Acrylic acid solution is added, 66 DEG C is warming up to and is sealed stir process 2.3h at such a temperature, be subsequently adding triethanolamine solution, rise
Temperature to 79 DEG C and at such a temperature heating stirring process 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is
800W, then stir at a temperature of 99 DEG C to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
Embodiment 2
In the embodiment of the present invention, a kind of desulfuration adsorbent for gasoline is made up of the following raw material according to weight portion:She
35 parts of sharp stone, 7 parts of strontium acetate, 21 parts of acrylic acid, 13 parts of triethanolamine.
5.5 times of deionized water of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution.By illite and strontium acetate mixed grinding, 120 mesh sieves are crossed, then
Acrylic acid solution is added, 66 DEG C is warming up to and is sealed stir process 2.3h at such a temperature, be subsequently adding triethanolamine solution, rise
Temperature to 79 DEG C and at such a temperature heating stirring process 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is
800W, then stir at a temperature of 101 DEG C to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
Embodiment 3
In the embodiment of the present invention, a kind of desulfuration adsorbent for gasoline is made up of the following raw material according to weight portion:She
29 parts of sharp stone, 4 parts of strontium acetate, 15 parts of acrylic acid, 7 parts of triethanolamine.
5.5 times of deionized water of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution.By illite and strontium acetate mixed grinding, 120 mesh sieves are crossed, then
Acrylic acid solution is added, 66 DEG C is warming up to and is sealed stir process 2.3h at such a temperature, be subsequently adding triethanolamine solution, rise
Temperature to 79 DEG C and at such a temperature heating stirring process 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is
800W, then stir at a temperature of 100 DEG C to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
Embodiment 4
In the embodiment of the present invention, a kind of desulfuration adsorbent for gasoline is made up of the following raw material according to weight portion:She
33 parts of sharp stone, 6 parts of strontium acetate, 19 parts of acrylic acid, 11 parts of triethanolamine.
5.5 times of deionized water of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution.By illite and strontium acetate mixed grinding, 120 mesh sieves are crossed, then
Acrylic acid solution is added, 66 DEG C is warming up to and is sealed stir process 2.3h at such a temperature, be subsequently adding triethanolamine solution, rise
Temperature to 79 DEG C and at such a temperature heating stirring process 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is
800W, then stir at a temperature of 100 DEG C to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
Embodiment 5
In the embodiment of the present invention, a kind of desulfuration adsorbent for gasoline is made up of the following raw material according to weight portion:She
31 parts of sharp stone, 5 parts of strontium acetate, 17 parts of acrylic acid, 9 parts of triethanolamine.
5.5 times of deionized water of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution.By illite and strontium acetate mixed grinding, 120 mesh sieves are crossed, then
Acrylic acid solution is added, 66 DEG C is warming up to and is sealed stir process 2.3h at such a temperature, be subsequently adding triethanolamine solution, rise
Temperature to 79 DEG C and at such a temperature heating stirring process 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is
800W, then stir at a temperature of 100 DEG C to dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
Comparative example 1
In addition to strontium acetate is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to triethanolamine is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
In addition to strontium acetate and triethanolamine is not contained, its material content and preparation process are consistent with embodiment 5.
Embodiment 6
The specific surface area of detection embodiment of the present invention 1-5 and adsorbent obtained in comparative example 1-3, as shown in table 1.While with
The illite for not making any process is blank.
Table 1
Total specific surface area SBET/ (m2·g-1) | |
Embodiment 1 | 187.6 |
Embodiment 2 | 190.5 |
Embodiment 3 | 235.8 |
Embodiment 4 | 249.5 |
Embodiment 5 | 264.1 |
Comparative example 1 | 30.8 |
Comparative example 2 | 98.5 |
Comparative example 3 | 23.6 |
Untreated illite | 7.3 |
Embodiment 7
Respectively desulfuration adsorbent prepared by above-described embodiment 5 and comparative example 1-3 is filled in fixed bed reactors, to help
Southern catalytically cracked gasoline is raw material (its composition is shown in Table 2), is under 30 DEG C and condition of normal pressure, with the stream of 0.5mL/min in temperature
Speed implements the absorption desulfurization test of continuous 10 hours respectively, and absorption Desulfurization Test Results are shown in Table 3, and wherein Sulfur capacity adsorbs for 1g desulfurization
The total sulfur content (in gram) removed when the total sulfur content in gasoline stocks is down to below 10ppmw by agent, for example Sulfur capacity is
When 0.525, the total sulfur content removed when the total sulfur content in gasoline stocks is down to below 10ppmw by 1g desulfuration adsorbents is represented
For 0.525g.
The composition of 2 feed gasoline of table
The absorption Desulfurization Test Results of 3 desulfuration adsorbent of table
As seen from the results in Table 3:
1st, desulfuration adsorbent desulfurization depth prepared by the present invention is high, can be by feed gasoline in absorption desulfurization 5-6 hours
Sulphur be down to below 1ppmw, and service life is up to 9h or so;Additionally, its desulfuration adsorbent Sulfur capacity is big, particularly to thiophene
And its selectivity of derivative is good.
When the 2nd, not containing triethanolamine, the service life of desulfuration adsorbent is greatly shortened;When not containing strontium acetate, desulfurization is inhaled
The attached dose of selectivity to sulphur is low;And when not containing strontium acetate and triethanolamine, the Sulfur capacity of desulfuration adsorbent is less, and use the longevity
Life is short.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (5)
1. a kind of desulfuration adsorbent for gasoline, it is characterised in that be made up of the following raw material according to weight portion:Illite
27-35 parts, strontium acetate 3-7 parts, acrylic acid 13-21 parts, triethanolamine 5-13 parts.
2. the desulfuration adsorbent for gasoline according to claim 1, it is characterised in that by the following original according to weight portion
Material composition:Illite 29-33 parts, strontium acetate 4-6 parts, acrylic acid 15-19 parts, triethanolamine 7-11 parts.
3. the desulfuration adsorbent for gasoline according to claim 1, it is characterised in that by the following original according to weight portion
Material composition:31 parts of illite, 5 parts of strontium acetate, 17 parts of acrylic acid, 9 parts of triethanolamine.
4. a kind of preparation method of the desulfuration adsorbent for gasoline as described in claim 1-3 is arbitrary, it is characterised in that by
Following steps are constituted:
1) deionized water of 5.5 times of acrylic acid and its quality is mixed, acrylic acid solution is obtained;By triethanolamine and its quality
2.3 times of absolute ethyl alcohol mixing, is obtained triethanolamine solution;
2) by illite and strontium acetate mixed grinding, excessively 120 mesh sieves, acrylic acid solution is subsequently adding, 66 DEG C is warming up to and at this
At a temperature of seal stir process 2.3h, be subsequently adding triethanolamine solution, be warming up to 79 DEG C and at such a temperature at heating stirring
Reason 8min, then ultrasonically treated 26min at such a temperature, ultrasonic power is 800W, then stir at a temperature of 99-101 DEG C to
It is dry, then 4.8h is calcined in 450 DEG C of Muffle furnace obtain final product desulfuration adsorbent.
5. the application in the oil of the desulfuration adsorbent as described in claim 1-3 is arbitrary.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107983322A (en) * | 2017-12-01 | 2018-05-04 | 宁波甬凌新材料科技有限公司 | A kind of gasoline Special desulfurizing agent and its preparation method and application |
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US6245221B1 (en) * | 1997-08-22 | 2001-06-12 | Exxon Research And Engineering Company | Desulfurization process for refractory organosulfur heterocycles |
CN1519297A (en) * | 2003-01-24 | 2004-08-11 | 中国石油化工股份有限公司 | Adsorbent for desulfurizing fuel oil and preparation method |
CN101333455A (en) * | 2008-07-30 | 2008-12-31 | 浙江工业大学 | Desulphurization process of gasoline by catalytic oxidation and extraction |
CN103551107A (en) * | 2013-11-05 | 2014-02-05 | 中国石油大学(北京) | Desulfuration adsorbent for catalytic gasoline as well as preparation method and application of adsorbent |
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2016
- 2016-12-02 CN CN201611093233.6A patent/CN106512923A/en active Pending
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US5925239A (en) * | 1996-08-23 | 1999-07-20 | Exxon Research And Engineering Co. | Desulfurization and aromatic saturation of feedstreams containing refractory organosulfur heterocycles and aromatics |
US6245221B1 (en) * | 1997-08-22 | 2001-06-12 | Exxon Research And Engineering Company | Desulfurization process for refractory organosulfur heterocycles |
CN1519297A (en) * | 2003-01-24 | 2004-08-11 | 中国石油化工股份有限公司 | Adsorbent for desulfurizing fuel oil and preparation method |
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CN107983322A (en) * | 2017-12-01 | 2018-05-04 | 宁波甬凌新材料科技有限公司 | A kind of gasoline Special desulfurizing agent and its preparation method and application |
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