CN106590733A - Method of preparing diatomite desulfurizing agent - Google Patents
Method of preparing diatomite desulfurizing agent Download PDFInfo
- Publication number
- CN106590733A CN106590733A CN201611228862.5A CN201611228862A CN106590733A CN 106590733 A CN106590733 A CN 106590733A CN 201611228862 A CN201611228862 A CN 201611228862A CN 106590733 A CN106590733 A CN 106590733A
- Authority
- CN
- China
- Prior art keywords
- parts
- desulfurizing agent
- kieselguhr
- acetic acid
- hydroxypropyl methyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/02—Gasoline
Abstract
The invention discloses a method of preparing a diatomite desulfurizing agent. The desulfurizing agent is composed of the following raw materials in parts by weight: 28-36 parts of diatomite, 1-5 parts of hydroxypropyl methyl cellulose, 3-7 parts of purple perilla seeds and 11-19 parts of acetic acid. According to the desulfurizing agent prepared by the steps of mixing and grinding diatomite which is taken as a raw material and hydroxypropyl methyl cellulose and treating the same with acetic acid and purple perilla seeds, gasoline with an ultralow sulfur content which is smaller than 60 microgram/g can be obtained in the condition that the RON loss is smaller than 2.0. The desulfurizing agent disclosed by the invention is good in selectivity on sulfur and high in desulfurizing depth, can avoid octane number loss caused by saturated olefin hydrogenation while deeply remove sulfur-containing compounds in the gasoline, and is long in service life, relatively environmental-friendly, free of secondary pollution and good in regenerability. The method disclosed by the invention is simple in preparation process, easy to operate and control, stable in performance, low in production cost and suitable for industrial production.
Description
Technical field
The present invention relates to technical field of gasoline, method prepared by specifically a kind of kieselguhr desulfurizing agent.
Background technology
The ultra-deep desulfurization of gasoline has become a major issue urgently to be resolved hurrily in world wide.Combustion of sulfur in gasoline
It is one of main pollutant in air to generate oxysulfide (SOx), and which 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 which and urge
Change activity, increase the discharge of particulate pollutant, increase the pollution of urban environment.Therefore, it is motor petrol standard to limit sulfur content
In an important indicator, and evaluate gasoline cleaning degree key factor.External gasoline blend component only has 34% in constituting
It is catalytic cracking (FCC) gasoline, the blend component of the product oil of China has 80% (volume fraction) from FCC gasoline, and gasoline
The sulphur source of middle 85-95% from FCC gasoline, therefore, the sulfur content being effectively reduced using which kind of technique in FCC gasoline becomes China
The matter of utmost importance that quality of gasoline 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, kieselguhr makes which 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 method prepared by kieselguhr desulfurizing agent, to solve to carry in above-mentioned background technology
The problem for going out.
For achieving the above object, the present invention provides following technical scheme：
A kind of kieselguhr desulfurizing agent, is made up of the following raw material according to weight portion：Kieselguhr 28-36 parts, hydroxypropyl methyl
Cellulose 1-5 parts, Folium Perillae son's 3-7 parts, acetic acid 11-19 parts.
As further scheme of the invention：The kieselguhr desulfurizing agent, is made up of the following raw material according to weight portion：Silicon
Diatomaceous earth 30-34 part, hydroxypropyl methyl cellulose 2-4 parts, Folium Perillae son's 4-6 parts, acetic acid 13-17 parts.
As further scheme of the invention：The kieselguhr desulfurizing agent, is made up of the following raw material according to weight portion：Silicon
32 parts of diatomaceous earth, 3 parts of hydroxypropyl methyl cellulose, Folium Perillae son 5 parts, 15 parts of acetic acid.
Another object of the present invention is to provide a kind of preparation method of kieselguhr desulfurizing agent, comprises the steps of：
1) 65% ethanol of 6.8 times of acetic acid and its quality is mixed, acetic acid solution is obtained；
2) by kieselguhr and hydroxypropyl methyl cellulose mixed grinding 1.5-1.6h, acetic acid solution is subsequently adding, is warming up to
And stir process 1.9h is sealed at such a temperature, it is young to then heat to 83 DEG C and Deca Folium Perillae, in the temperature after being added dropwise to complete by 69 DEG C
Lower supersound process 22min of degree, ultrasonic power is 1000W, then is stirred at a temperature of 99-101 DEG C to dry, then at 440 DEG C
4.3h is calcined in Muffle furnace and 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 invention has the beneficial effects as follows：
The present invention is with kieselguhr as raw material, after hydroxypropyl methyl cellulose mixed grinding then young through acetic acid, Folium Perillae
The obtained desulfurizing agent such as process, makes gasoline in the case where RON losses are less than 2.0, can obtain sulfur content in below 6 μ g/g
The gasoline of ultra-low sulfur.The present invention is good to the selectivity of sulfur, desulfurization depth is high, sulfur-bearing chemical combination that can be in deep removal gasoline
While thing, it is to avoid the loss of octane number that olefins hydrogenation is caused, long service life are more friendly to environment, without secondary dirt
Dye, regenerability are good.Preparation process is simple of the present invention, easy to operate, easy to control, stable performance, low production cost are suitable to industry
Metaplasia is produced.
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 kieselguhr desulfurizing agent is made up of the following raw material according to weight portion：Kieselguhr 28
Part, 1 part of hydroxypropyl methyl cellulose, Folium Perillae son 3 parts, 11 parts of acetic acid.
The ethanol that 6.8 times of volumetric concentration of acetic acid and its quality is 65% is mixed, acetic acid solution is obtained.By kieselguhr with
Hydroxypropyl methyl cellulose mixed grinding 1.5h, is subsequently adding acetic acid solution, is warming up to 69 DEG C and sealing stirring at such a temperature
1.9h is processed, it is young to then heat to 83 DEG C and Deca Folium Perillae, supersound process 22min at such a temperature after being added dropwise to complete, ultrasonic work(
Rate is 1000W, then is stirred at a temperature of 99 DEG C to dry, then calcines 4.3h 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 kieselguhr desulfurizing agent is made up of the following raw material according to weight portion：Kieselguhr 36
Part, 5 parts of hydroxypropyl methyl cellulose, Folium Perillae son 7 parts, 19 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.Kieselguhr is fine with hydroxypropyl methyl
The plain mixed grinding 1.6h of dimension, is subsequently adding acetic 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 Deca Folium Perillae young, supersound process 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stir at a temperature of 101 DEG C to dry, then 4.3h is calcined in 440 DEG C of Muffle furnace and obtain final product desulfurizing agent.
Embodiment 3
In the embodiment of the present invention, a kind of kieselguhr desulfurizing agent is made up of the following raw material according to weight portion：Kieselguhr 30
Part, 2 parts of hydroxypropyl methyl cellulose, Folium Perillae son 4 parts, 13 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.Kieselguhr is fine with hydroxypropyl methyl
The plain mixed grinding 1.55h of dimension, is subsequently adding acetic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, so
After to be warming up to 83 DEG C and Deca Folium Perillae young, supersound process 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stir at a temperature of 100 DEG C to dry, then 4.3h is calcined in 440 DEG C of Muffle furnace and obtain final product desulfurizing agent.
Embodiment 4
In the embodiment of the present invention, a kind of kieselguhr desulfurizing agent is made up of the following raw material according to weight portion：Kieselguhr 34
Part, 4 parts of hydroxypropyl methyl cellulose, Folium Perillae son 6 parts, 17 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.Kieselguhr is fine with hydroxypropyl methyl
The plain mixed grinding 1.55h of dimension, is subsequently adding acetic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, so
After to be warming up to 83 DEG C and Deca Folium Perillae young, supersound process 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stir at a temperature of 100 DEG C to dry, then 4.3h is calcined in 440 DEG C of Muffle furnace and obtain final product desulfurizing agent.
Embodiment 5
In the embodiment of the present invention, a kind of kieselguhr desulfurizing agent is made up of the following raw material according to weight portion：Kieselguhr 32
Part, 3 parts of hydroxypropyl methyl cellulose, Folium Perillae son 5 parts, 15 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.Kieselguhr is fine with hydroxypropyl methyl
The plain mixed grinding 1.55h of dimension, is subsequently adding acetic acid solution, is warming up to 69 DEG C and seals stir process 1.9h at such a temperature, so
After to be warming up to 83 DEG C and Deca Folium Perillae young, supersound process 22min at such a temperature after being added dropwise to complete, ultrasonic power is 1000W, then
Stir at a temperature of 100 DEG C to dry, then 4.3h is calcined in 440 DEG C of Muffle furnace and obtain final product desulfurizing agent.
Comparative example 1
In addition to hydroxypropyl methyl cellulose is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to Folium Perillae son is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
It is young outer except hydroxypropyl methyl cellulose and Folium Perillae is not contained, its material content and preparation process and embodiment 5 one
Cause.
Embodiment 6
Respectively sour gasoline is selected using the kieselguhr desulfurizing agent obtained by above-described embodiment 1-5 and comparative example 1-3
The desulfurization of selecting property, comprises the following steps that：
Sour gasoline of the sulfur content in 398 μ g/g is taken off with the kieselguhr obtained by embodiment 1-5 and comparative example 1-3 respectively
Sulfur agent is in feeding liquid volume space velocity 2h-1, under conditions of 100 DEG C of temperature, pressure 0.8MPa, hydrogen and sour gasoline volume ratio 100
Contacted.
Obtained by sour gasoline and difference Jing embodiments 1-5 and comparative example 1-3 used by above-mentioned Application Example
Kieselguhr desulfurizing agent carries out total sulfur after desulfurization in the sulfur-free gasoline of gained, alkene, research octane number (RON), RON losses, desulfurization degree
After testing or calculate, which 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 kieselguhr desulfurizing agent of the invention
<The high-quality cleaning sulfur-free gasoline of 6 μ g/g, research octane number (RON) RON losses<2.0 units.
Embodiment 7
Using the kieselguhr desulfurizing agent obtained by embodiment 5 to sulfur content 398 μ g/g sour gasoline in feeding liquid volume
Air speed 2h-1, 100 DEG C of temperature, pressure 0.8MPa, hydrogen process 10h with carrying out contacting under conditions of sour gasoline volume ratio 100
Afterwards, that is, the desulfurization process of 1 kieselguhr desulfurizing agent are completed.
The above-mentioned kieselguhr desulfurizing agent for completing 1 desulfurization process is regenerated, is comprised the following steps that：
Above-mentioned regenerative process adopts air for regeneration gas, controls volume of air air speed for 200h-1, temperature be 440 DEG C, often
Pressure carries out burning sulfur 2.5h, is then down to room temperature, that is, the regeneration of the kieselguhr desulfurizing agent after completing to inactivate.
By it is above-mentioned complete 1 time regeneration after kieselguhr desulfurizing agent 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 respectively to sour gasoline using the regeneration 1 time of above-mentioned gained, 5 times, the kieselguhr desulfurizing agent of 10 times
Sour gasoline is that total sulfur in the sulfur-free gasoline of raw oil and gained, alkene, research octane number (RON), desulfurization degree the results are shown in Table
2：
Table 2
As can be seen from the above table, kieselguhr desulfurizing agent of the invention,, after 10 regeneration, its desulfurization degree is still reachable for which
99.5-99.7%, has been indicated above during sour gasoline desulfurization, the activity of the kieselguhr desulfurizing agent of the present invention, selection
Property is good, and every reactivity worth index good stability of the gasoline after desulfurization.
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 description is only that those skilled in the art should for clarity
Using description 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 kieselguhr desulfurizing agent, it is characterised in that be made up of the following raw material according to weight portion：Kieselguhr 28-36 parts, hydroxyl
Propyl methocel 1-5 parts, Folium Perillae son's 3-7 parts, acetic acid 11-19 parts.
2. kieselguhr desulfurizing agent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：
Kieselguhr 30-34 parts, hydroxypropyl methyl cellulose 2-4 parts, Folium Perillae son's 4-6 parts, acetic acid 13-17 parts.
3. kieselguhr desulfurizing 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 kieselguhr, 3 parts of hydroxypropyl methyl cellulose, Folium Perillae son 5 parts, 15 parts of acetic acid.
4. a kind of preparation method of the kieselguhr desulfurizing agent as described in claim 1-3 is arbitrary, it is characterised in that by following steps
Composition：
1) 65% ethanol of 6.8 times of acetic acid and its quality is mixed, acetic acid solution is obtained；
2) by kieselguhr and hydroxypropyl methyl cellulose mixed grinding 1.5-1.6h, acetic acid solution is subsequently adding, 69 DEG C are warming up to
And stir process 1.9h is sealed at such a temperature, then heat to 83 DEG C and Deca Folium Perillae is young, after being added dropwise to complete at such a temperature
Supersound process 22min, ultrasonic power are 1000W, then are stirred at a temperature of 99-101 DEG C to dry, then in 440 DEG C of Muffle
4.3h is calcined in stove and obtains final product desulfurizing agent.
5. the application in the oil of the desulfurizing agent as described in claim 1-3 is arbitrary.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611228862.5A CN106590733A (en) | 2016-12-27 | 2016-12-27 | Method of preparing diatomite desulfurizing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611228862.5A CN106590733A (en) | 2016-12-27 | 2016-12-27 | Method of preparing diatomite desulfurizing agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106590733A true CN106590733A (en) | 2017-04-26 |
Family
ID=58602620
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611228862.5A Pending CN106590733A (en) | 2016-12-27 | 2016-12-27 | Method of preparing diatomite desulfurizing agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106590733A (en) |
-
2016
- 2016-12-27 CN CN201611228862.5A patent/CN106590733A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5142588B2 (en) | Method for producing gasoline composition | |
| JP2007308569A (en) | A-type heavy oil composition | |
| CN104028208B (en) | A kind of gasoline high selectivity desulfuration adsorbent and preparation method and application | |
| CN106582505A (en) | Clay desulfurizer as well as preparation method and application thereof | |
| JP5189740B2 (en) | Hydrorefining method | |
| JP5117089B2 (en) | Method for producing light oil composition | |
| JP5072444B2 (en) | Method for producing light oil composition | |
| CN106590733A (en) | Method of preparing diatomite desulfurizing agent | |
| CN106433749B (en) | A kind of selective desulfurization agent and its preparation method and application | |
| CN106378099A (en) | Modified desulfuration adsorbent, and preparation method and application thereof | |
| JP5137335B2 (en) | Method for producing gasoline composition | |
| CN106554803B (en) | A kind of gasoline desulfurizer and its preparation method and application | |
| CN106732478A (en) | A kind of diatomite desulfurizing agent and its preparation method and application | |
| CN106732339A (en) | A kind of selective desulfurization agent and preparation method thereof | |
| CN107159096A (en) | Adsorbing and desulfurizing catalytic cracking gasoline agent and preparation method and application | |
| CN103468309B (en) | A kind of method of producing low-sulphur oil | |
| CN103059967B (en) | Mixed hydrogenation method for catalytic cracking gasoline and coking diesel oil | |
| CN106582512A (en) | Gasoline desulphurization agent and preparation method thereof | |
| CN108003920A (en) | A kind of oxidized sulfur method with load metal oxide double-function catalyzing adsorption desulfurizing agent | |
| CN105778979A (en) | Catalyst for reducing sulfur content of catalytically cracked gasoline and preparation method thereof | |
| CN106582501A (en) | Desulfuration adsorbent | |
| JP2023548698A (en) | Process for producing diesel fuel from biorenewable feeds with recycled sulfur | |
| CN106433741A (en) | Gasoline product desulfurizing agent, as well as preparation method and application thereof | |
| CN109486523B (en) | FCC gasoline desulfurization modification method | |
| CN106732479A (en) | A kind of modified desulfuration adsorbent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170426 |
|
| WD01 | Invention patent application deemed withdrawn after publication |