CN106732339A - A kind of selective desulfurization agent and preparation method thereof - Google Patents
A kind of selective desulfurization agent and preparation method thereof Download PDFInfo
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- CN106732339A CN106732339A CN201611247466.7A CN201611247466A CN106732339A CN 106732339 A CN106732339 A CN 106732339A CN 201611247466 A CN201611247466 A CN 201611247466A CN 106732339 A CN106732339 A CN 106732339A
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- parts
- formic acid
- illite
- gasoline
- cinnamic aldehyde
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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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- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
-
- 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
-
- 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
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/305—Octane number, e.g. motor octane number [MON], research octane number [RON]
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/02—Gasoline
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of selective desulfurization agent and preparation method thereof, the desulfurizing agent is made up of the following raw material according to weight portion：28 36 parts of illite, 15 parts of hydroxypropylguar, 37 parts of cinnamic aldehyde, 11 19 parts of formic acid.The present invention is with illite as raw material, after hydroxypropylguar mixed grinding, again through obtained desulfurizing agents such as performic acid, the treatment of cinnamic aldehyde, make gasoline in the case where RON losses are less than 2.0, gasoline of the sulfur content in the ultra-low sulfur of below 6 μ g/g can be obtained.Selectivity to sulphur of the invention is good, desulfurization depth is high, can be while the sulfur-containing compound in deep removal gasoline, it is to avoid the loss of octane number that olefins hydrogenation is caused, long service life is more friendly to environment, and non-secondary pollution, regenerability is good.Preparation process is simple of the present invention, easy to operate, easy to control, stable performance, low production cost is suitable to industrialized production.
Description
Technical field
The present invention relates to technical field of gasoline, specifically a kind of selective desulfurization agent and preparation method thereof.
Background technology
The ultra-deep desulfurization of gasoline has turned into a major issue urgently to be resolved hurrily in world wide.Combustion of sulfur in gasoline
Generation oxysulfide（SOx）It is one of main pollutant in air, it can form acid rain, the ecological ring of destruction in being discharged into air
Border.In addition, sulfur oxide can also corrosion and damage engine components, make motor-driven vehicle gas disposal catalyst poisoning, reduce it and urge
Change activity, increase the discharge of particulate pollutant, aggravate the pollution of urban environment.Therefore, limitation sulfur content is motor petrol standard
In an important indicator, be also evaluate gasoline cleaning degree key factor.Only 34% is during external gasoline blend component is constituted
Catalytic cracking（FCC）Gasoline, the blend component of the product oil of China has 80%（Volume fraction）From FCC gasoline, and in gasoline
The sulphur source of 85-95% from FCC gasoline, therefore, which kind of technique to be effectively reduced sulfur content in FCC gasoline using turns into China's vapour
The matter of utmost importance that oil quality upgrading faces.
Traditional gasoline desulfurization technology can be divided into hydrodesulfurization and two kinds of desulfurization of absorption.Hydrodesulfurization need high temperature, high pressure,
Substantial amounts of hydrogen wastage, also can cause the significantly loss of octane number with the saturation of olefin(e) compound.Absorption method gasoline desulfurization
There is Low investment, lower operational cost.But the physical adsorption process removal efficiency with various molecular sieves, activated carbon as representative compared with
It is low, and the life-span is shorter.Also there is discarded adsorbent secondary pollution and process problem in some materials.Additionally, existing desulfurizing agent is more
Using materials such as activated carbon, ZSM-5, illite makes it seldom be used due to the structure of its own.
The content of the invention
It is an object of the invention to provide a kind of selective desulfurization agent and preparation method thereof, with solving above-mentioned background technology
The problem of proposition.
To achieve the above object, the present invention provides following technical scheme：
A kind of selective desulfurization agent, is made up of the following raw material according to weight portion：Illite 28-36 parts, hydroxypropylguar
1-5 parts, cinnamic aldehyde 3-7 parts, formic acid 11-19 parts.
As further scheme of the invention：The selective desulfurization agent, is made up of the following raw material according to weight portion：She
Sharp stone 30-34 parts, hydroxypropylguar 2-4 parts, cinnamic aldehyde 4-6 parts, formic acid 13-17 parts.
As further scheme of the invention：The selective desulfurization agent, is made up of the following raw material according to weight portion：She
32 parts of sharp stone, 3 parts of hydroxypropylguar, 5 parts of cinnamic aldehyde, 15 parts of formic acid.
Another object of the present invention is to provide a kind of preparation method of selective desulfurization agent, comprises the steps of：
1）6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained；
2）By illite and hydroxypropylguar mixed grinding 1.5-1.6h, formic acid solution is subsequently adding, is warming up to 69 DEG C simultaneously
Stir process 1.9h is sealed at such a temperature, then heats to 83 DEG C and cinnamic aldehyde is added dropwise, it is ultrasonic at such a temperature after being added dropwise to complete
Treatment 22min, ultrasonic power is 1000W, then is stirred at a temperature of 99-101 DEG C to dry, then in 440 DEG C of Muffle furnace
Calcining 4.3h obtains final product desulfurizing agent.
Another object of the present invention is to provide desulfurizing agent application in the oil.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention after hydroxypropylguar mixed grinding, then makes with illite as raw material through performic acid, treatment of cinnamic aldehyde etc.
The desulfurizing agent for obtaining, makes gasoline in the case where RON losses are less than 2.0, and the super-low sulfur that can obtain sulfur content in below 6 μ g/g contains
The gasoline of amount.Selectivity to sulphur of the invention is good, desulfurization depth is high, can be in the same of the sulfur-containing compound in deep removal gasoline
When, it is to avoid the loss of octane number that olefins hydrogenation is caused, long service life is more friendly to environment, non-secondary pollution, regeneration
It is functional.Preparation process is simple of the present invention, easy to operate, easy to control, stable performance, low production cost is suitable to industrialized production.
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 whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of selective desulfurization agent is made up of the following raw material according to weight portion：28 parts of illite, hydroxyl
1 part of propyl group guar gum, 3 parts of cinnamic aldehyde, 11 parts of formic acid.
The ethanol that 6.8 times of volumetric concentration of formic acid and its quality is 65% is mixed, formic acid solution is obtained.By illite with
Hydroxypropylguar mixed grinding 1.5h, is subsequently adding formic acid solution, is warming up at 69 DEG C and at such a temperature sealing stirring
Reason 1.9h, then heats to 83 DEG C and cinnamic aldehyde is added dropwise, ultrasonically treated 22min at such a temperature after being added dropwise to complete, and ultrasonic power is
1000W, then stirred at a temperature of 99 DEG C to dry, 4.3h is then calcined in 440 DEG C of Muffle furnace and obtains final product desulfurizing agent.
Embodiment 2
In the embodiment of the present invention, a kind of selective desulfurization agent is made up of the following raw material according to weight portion：36 parts of illite, hydroxyl
5 parts of propyl group guar gum, 7 parts of cinnamic aldehyde, 19 parts of formic acid.
6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained.By illite and hydroxypropyl guar beans
Glue mixed grinding 1.6h, is subsequently adding formic acid solution, is warming up to 69 DEG C and at such a temperature sealing stir process 1.9h, Ran Housheng
Temperature to 83 DEG C and is added dropwise cinnamic aldehyde, ultrasonically treated 22min at such a temperature after being added dropwise to complete, and ultrasonic power is 1000W, then 101
Stirred at a temperature of DEG C to dry, 4.3h is then calcined in 440 DEG C of Muffle furnace and obtains final product desulfurizing agent.
Embodiment 3
In the embodiment of the present invention, a kind of selective desulfurization agent is made up of the following raw material according to weight portion：30 parts of illite, hydroxyl
2 parts of propyl group guar gum, 4 parts of cinnamic aldehyde, 13 parts of formic acid.
6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained.By illite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, is subsequently adding formic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, then
It is warming up to 83 DEG C and cinnamic aldehyde is added dropwise, ultrasonically treated 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stirred at a temperature of 100 DEG C to dry, 4.3h is then calcined in 440 DEG C of Muffle furnace and obtains final product desulfurizing agent.
Embodiment 4
In the embodiment of the present invention, a kind of selective desulfurization agent is made up of the following raw material according to weight portion：34 parts of illite, hydroxyl
4 parts of propyl group guar gum, 6 parts of cinnamic aldehyde, 17 parts of formic acid.
6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained.By illite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, is subsequently adding formic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, then
It is warming up to 83 DEG C and cinnamic aldehyde is added dropwise, ultrasonically treated 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stirred at a temperature of 100 DEG C to dry, 4.3h is then calcined in 440 DEG C of Muffle furnace and obtains final product desulfurizing agent.
Embodiment 5
In the embodiment of the present invention, a kind of selective desulfurization agent is made up of the following raw material according to weight portion：32 parts of illite, hydroxyl
3 parts of propyl group guar gum, 5 parts of cinnamic aldehyde, 15 parts of formic acid.
6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained.By illite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, is subsequently adding formic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, then
It is warming up to 83 DEG C and cinnamic aldehyde is added dropwise, ultrasonically treated 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stirred at a temperature of 100 DEG C to dry, 4.3h is then calcined in 440 DEG C of Muffle furnace and obtains final product desulfurizing agent.
Comparative example 1
In addition to hydroxypropylguar is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to cinnamic aldehyde is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
In addition to hydroxypropylguar and cinnamic aldehyde is not contained, its material content and preparation process are consistent with embodiment 5.
Embodiment 6
Selectivity is carried out to sour gasoline respectively using the selective desulfurization agent obtained by above-described embodiment 1-5 and comparative example 1-3
Desulfurization, comprises the following steps that：
By sulfur content 398 μ g/g sour gasoline respectively with the selective desulfurization agent obtained by embodiment 1-5 and comparative example 1-3
In feeding liquid volume space velocity 2h-1, carried out under conditions of 100 DEG C of temperature, pressure 0.8MPa, hydrogen and sour gasoline volume ratio 100
Contact.
Sour gasoline used and respectively through obtained by embodiment 1-5 and comparative example 1-3 in above-mentioned Application Example
Selective desulfurization agent carries out total sulfur, alkene, research octane number (RON), RON losses, the desulfurization degree after desulfurization in the sulfur-free gasoline of gained
After testing or calculate, it the results are shown in Table 1.
Table 1
As can be seen from the above table, catalytically cracked gasoline inferior can be processed as sulfur content by selective desulfurization agent of the invention<6µ
The high-quality cleaning sulfur-free gasoline of g/g, research octane number (RON) RON losses<2.0 units.
Embodiment 7
Using the gained of embodiment 5 selective desulfurization agent to sulfur content 398 μ g/g sour gasoline in feeding liquid volume space velocity
2h-1, 100 DEG C of temperature, pressure 0.8MPa, hydrogen with carry out contacting treatment 10h under conditions of sour gasoline volume ratio 100 after, i.e.,
Complete 1 desulfurization process of selective desulfurization agent.
Selective desulfurization agent to 1 desulfurization process of above-mentioned completion regenerates, and comprises the following steps that：
It is regeneration gas that above-mentioned regenerative process uses air, and it is 200h to control volume of air air speed-1, temperature be 440 DEG C, normal pressure
Carry out burning sulphur 2.5h, be then down to room temperature, that is, complete the regeneration of the selective desulfurization agent after inactivation.
By the selective desulfurization agent after the regeneration of above-mentioned completion 1 time to sulfur content 398 μ g/g sour gasoline again according to
Above-mentioned condition carries out desulfurization process, that is, repeat above-mentioned desulfurization, regeneration 5 times, 10 times.
Desulfurization, institute are carried out to sour gasoline respectively using the regeneration 1 time of above-mentioned gained, 5 times, the selective desulfurization agent of 10 times
Sour gasoline is that total sulfur in the sulfur-free gasoline of feedstock oil and gained, alkene, research octane number (RON), desulfurization degree the results are shown in Table
2：
Table 2
| Feedstock oil | Regeneration 1 time | Regeneration 5 times | Regeneration 10 times | |
| Total sulfur（μg/g） | 398 | 1 | 1 | 2 |
| Alkene（v%） | 26.8 | 21.8 | 21.8 | 21.9 |
| Research octane number (RON), RON | 91.3 | 90.6 | 90.6 | 90.5 |
| Desulfurization degree（%） | - | 99.7 | 99.7 | 99.5 |
As can be seen from the above table, selective desulfurization agent of the invention, it is after 10 times regenerate, and its desulfurization degree is still reachable
99.5-99.7%, has been indicated above during sour gasoline desulfurization, active, the selectivity of selective desulfurization agent of the invention
It is good, and the gasoline after desulfurization every reactivity worth index good stability.
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 without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.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 requires to be limited rather than described above, 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 the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (5)
1. a kind of selective desulfurization agent, it is characterised in that be made up of the following raw material according to weight portion：Illite 28-36 parts, hydroxyl
1-5 parts, cinnamic aldehyde 3-7 parts, formic acid 11-19 parts of propyl group guar gum.
2. selective desulfurization agent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：
Illite 30-34 parts, hydroxypropylguar 2-4 parts, cinnamic aldehyde 4-6 parts, formic acid 13-17 parts.
3. selective desulfurization agent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：
32 parts of illite, 3 parts of hydroxypropylguar, 5 parts of cinnamic aldehyde, 15 parts of formic acid.
4. the preparation method of a kind of selective desulfurization agent as described in claim 1-3 is any, it is characterised in that by following steps
Composition：
1）6.8 times of 65% ethanol of formic acid and its quality is mixed, formic acid solution is obtained；
2）By illite and hydroxypropylguar mixed grinding 1.5-1.6h, formic acid solution is subsequently adding, is warming up to 69 DEG C simultaneously
Stir process 1.9h is sealed at such a temperature, then heats to 83 DEG C and cinnamic aldehyde is added dropwise, it is ultrasonic at such a temperature after being added dropwise to complete
Treatment 22min, ultrasonic power is 1000W, then is stirred at a temperature of 99-101 DEG C to dry, then in 440 DEG C of Muffle furnace
Calcining 4.3h obtains final product desulfurizing agent.
5. the application in the oil of the desulfurizing agent as described in claim 1-3 is any.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611247466.7A CN106732339A (en) | 2016-12-29 | 2016-12-29 | A kind of selective desulfurization agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611247466.7A CN106732339A (en) | 2016-12-29 | 2016-12-29 | A kind of selective desulfurization agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106732339A true CN106732339A (en) | 2017-05-31 |
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2016
- 2016-12-29 CN CN201611247466.7A patent/CN106732339A/en active Pending
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Application publication date: 20170531 |