CN106732478A - A kind of diatomite desulfurizing agent and its preparation method and application - Google Patents
A kind of diatomite desulfurizing agent and its preparation method and application Download PDFInfo
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- CN106732478A CN106732478A CN201611113634.3A CN201611113634A CN106732478A CN 106732478 A CN106732478 A CN 106732478A CN 201611113634 A CN201611113634 A CN 201611113634A CN 106732478 A CN106732478 A CN 106732478A
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- diatomite
- desulfurizing agent
- acetic acid
- perillaldehyde
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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
- B01J20/14—Diatomaceous earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- 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
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/302—Sulfur oxides
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of diatomite desulfurizing agent and its preparation method and application, the desulfurizing agent is made up of the following raw material according to weight portion：28 36 parts of diatomite, 15 parts of hydroxypropylguar, 37 parts of perillaldehyde, 11 19 parts of acetic acid.The present invention is with diatomite as raw material, after hydroxypropylguar mixed grinding, again through obtained desulfurizing agents such as peracetic acid, the treatment of perillaldehyde, 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 diatomite desulfurizing agent and its preparation method and application.
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) is one of main pollutant in air, and 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.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, which kind of technique to be effectively reduced sulfur content in FCC gasoline using turns into 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, diatomite 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 diatomite desulfurizing agent and its preparation method and application, to solve above-mentioned background
The problem proposed in technology.
To achieve the above object, the present invention provides following technical scheme：
A kind of diatomite desulfurizing agent, is made up of the following raw material according to weight portion：Diatomite 28-36 parts, hydroxypropyl guar
Bean gum 1-5 parts, perillaldehyde 3-7 parts, acetic acid 11-19 parts.
As further scheme of the invention：The diatomite desulfurizing agent, is made up of the following raw material according to weight portion：Silicon
Diatomaceous earth 30-34 parts, hydroxypropylguar 2-4 parts, perillaldehyde 4-6 parts, acetic acid 13-17 parts.
As further scheme of the invention：The diatomite desulfurizing agent, is made up of the following raw material according to weight portion：Silicon
32 parts of diatomaceous earth, 3 parts of hydroxypropylguar, 5 parts of perillaldehyde, 15 parts of acetic acid.
Another object of the present invention is to provide a kind of preparation method of diatomite 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 diatomite and hydroxypropylguar mixed grinding 1.5-1.6h, acetic acid solution is subsequently adding, is warming up to 69
DEG C and at such a temperature seal stir process 1.9h, then heat to 83 DEG C and perillaldehyde be added dropwise, in the temperature after being added dropwise to complete
Under ultrasonically treated 22min, ultrasonic power is 1000W, then is stirred at a temperature of 99-101 DEG C to dry, then in 440 DEG C of horse
4.3h is not calcined in stove 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 beneficial effects of the invention are as follows：
The present invention with diatomite as raw material, after hydroxypropylguar mixed grinding, then through peracetic acid, the place of perillaldehyde
The obtained desulfurizing agents such as reason, make gasoline in the case where RON losses are less than 2.0, can obtain sulfur content in the super of below 6 μ g/g
The gasoline of low sulfur content.Selectivity to sulphur of the invention is good, desulfurization depth is high, can be in the sulfur-containing compound in deep removal gasoline
While, 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,
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 industrialization
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 diatomite desulfurizing agent is made up of the following raw material according to weight portion：Diatomite 28
Part, 1 part of hydroxypropylguar, 3 parts of perillaldehyde, 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 diatomite with
Hydroxypropylguar mixed grinding 1.5h, is subsequently adding acetic 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 perillaldehyde is added dropwise, ultrasonically treated 22min, ultrasonic power at such a temperature after being added dropwise to complete
It is 1000W, then is 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 diatomite desulfurizing agent is made up of the following raw material according to weight portion：Diatomite 36
Part, 5 parts of hydroxypropylguar, 7 parts of perillaldehyde, 19 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.By diatomite and hydroxypropyl guar beans
Glue mixed grinding 1.6h, is subsequently adding acetic 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 perillaldehyde, ultrasonically treated 22min at such a temperature after being added dropwise to complete, and ultrasonic power is 1000W, then
Stirred at a temperature of 101 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 diatomite desulfurizing agent is made up of the following raw material according to weight portion：Diatomite 30
Part, 2 parts of hydroxypropylguar, 4 parts of perillaldehyde, 13 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.By diatomite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, 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 perillaldehyde 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 diatomite desulfurizing agent is made up of the following raw material according to weight portion：Diatomite 34
Part, 4 parts of hydroxypropylguar, 6 parts of perillaldehyde, 17 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.By diatomite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, 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 perillaldehyde 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 diatomite desulfurizing agent is made up of the following raw material according to weight portion：Diatomite 32
Part, 3 parts of hydroxypropylguar, 5 parts of perillaldehyde, 15 parts of acetic acid.
6.8 times of 65% ethanol of acetic acid and its quality is mixed, acetic acid solution is obtained.By diatomite and hydroxypropyl guar beans
Glue mixed grinding 1.55h, 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 perillaldehyde 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 perillaldehyde is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
In addition to hydroxypropylguar and perillaldehyde is not contained, its material content and preparation process are consistent with embodiment 5.
Embodiment 6
Sour gasoline is selected respectively using the diatomite 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 by sulfur content in 398 μ g/g takes off with the diatomite obtained by embodiment 1-5 and comparative example 1-3 respectively
Sulphur 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.
Sour gasoline used and respectively through obtained by embodiment 1-5 and comparative example 1-3 in above-mentioned Application Example
Diatomite desulfurizing 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 diatomite 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 gained of embodiment 5 diatomite desulfurizing agent 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 with carry out contacting treatment 10h under conditions of sour gasoline volume ratio 100
Afterwards, that is, 1 desulfurization process of diatomite desulfurizing agent is completed.
Diatomite desulfurizing 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, often
Pressure carries out burning sulphur 2.5h, is then down to room temperature, that is, complete the regeneration of the diatomite desulfurizing agent after inactivation.
By the diatomite desulfurizing 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 diatomite desulfurizing 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
As can be seen from the above table, diatomite desulfurizing 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, the activity of diatomite desulfurizing agent of the invention, selection
Property 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 diatomite desulfurizing agent, it is characterised in that be made up of the following raw material according to weight portion：Diatomite 28-36 parts, hydroxyl
1-5 parts, perillaldehyde 3-7 parts, acetic acid 11-19 parts of propyl group guar gum.
2. diatomite desulfurizing agent according to claim 1, it is characterised in that be made up of the following raw material according to weight portion：
Diatomite 30-34 parts, hydroxypropylguar 2-4 parts, perillaldehyde 4-6 parts, acetic acid 13-17 parts.
3. diatomite 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 diatomite, 3 parts of hydroxypropylguar, 5 parts of perillaldehyde, 15 parts of acetic acid.
4. the preparation method of a kind of diatomite desulfurizing agent as described in claim 1-3 is any, 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 diatomite and hydroxypropylguar mixed grinding 1.5-1.6h, acetic acid solution is subsequently adding, is warming up to 69 DEG C simultaneously
Stir process 1.9h is sealed at such a temperature, 83 DEG C is then heated to and perillaldehyde is added dropwise, surpass at such a temperature after being added dropwise to complete
Sonication 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
Middle 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.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875551A (en) * | 2009-04-28 | 2010-11-03 | 北京泰华美邦建材有限责任公司 | Clay capable of absorbing, purifying and decomposing harmful substances indoors |
| CN105289472A (en) * | 2015-11-19 | 2016-02-03 | 兰州坤仑环保科技有限公司 | Honeycomb attapulgite ceramsite diesel oil desulfurizer |
| CN105597516A (en) * | 2016-02-29 | 2016-05-25 | 北京三聚环保新材料股份有限公司 | Magnetic ferric oxide desulfurizer and preparation method thereof |
| CN105727884A (en) * | 2016-04-11 | 2016-07-06 | 张兴华 | Bentonite clay particles and preparation method thereof |
| CN105941508A (en) * | 2016-03-23 | 2016-09-21 | 绩溪袁稻农业产业科技有限公司 | Modified-plant-ash blue-green algae inhibitor and preparation method thereof |
-
2016
- 2016-12-07 CN CN201611113634.3A patent/CN106732478A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875551A (en) * | 2009-04-28 | 2010-11-03 | 北京泰华美邦建材有限责任公司 | Clay capable of absorbing, purifying and decomposing harmful substances indoors |
| CN105289472A (en) * | 2015-11-19 | 2016-02-03 | 兰州坤仑环保科技有限公司 | Honeycomb attapulgite ceramsite diesel oil desulfurizer |
| CN105597516A (en) * | 2016-02-29 | 2016-05-25 | 北京三聚环保新材料股份有限公司 | Magnetic ferric oxide desulfurizer and preparation method thereof |
| CN105941508A (en) * | 2016-03-23 | 2016-09-21 | 绩溪袁稻农业产业科技有限公司 | Modified-plant-ash blue-green algae inhibitor and preparation method thereof |
| CN105727884A (en) * | 2016-04-11 | 2016-07-06 | 张兴华 | Bentonite clay particles and preparation method thereof |
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Application publication date: 20170531 |