CN107983322A - A kind of gasoline Special desulfurizing agent and its preparation method and application - Google Patents
A kind of gasoline Special desulfurizing agent and its preparation method and application Download PDFInfo
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- CN107983322A CN107983322A CN201711251526.7A CN201711251526A CN107983322A CN 107983322 A CN107983322 A CN 107983322A CN 201711251526 A CN201711251526 A CN 201711251526A CN 107983322 A CN107983322 A CN 107983322A
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- desulfurizing agent
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- trichloroacetic acid
- vermiculite
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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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
- 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
-
- 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)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of gasoline Special desulfurizing agent and its preparation method and application, which includes according to the raw material of parts by weight：15 25 parts of vermiculite, 7 15 parts of trichloroacetic acid, 15 parts of triethanolamine, 11 19 parts of cornstarch, 37 parts of cashew nut shell liquid phenol-formaldehyde resin modified.By vermiculite and cornstarch mixed grinding, then solution of trichloroacetic acid heating sealing stirring is added, then add and triethanolamine and be ultrasonically treated, then be warming up to 85 88 DEG C and add cashew nut shell liquid phenol-formaldehyde resin modified, stop heating and be ultrasonically treated after stirring, stir to doing, calcine to obtain the final product.Catalytically cracked gasoline inferior can be processed as sulfur content by the present invention<The high-quality cleaning sulfur-free gasoline of 6 μ g/g, loss of octane number is few, service life length, non-secondary pollution more friendly to environment；Regenerability is good, and activity is high, selectivity is good, and the gasoline stability after desulfurization is good.
Description
Technical field
The present invention relates to technical field of gasoline, is specifically a kind of gasoline Special desulfurizing agent and its preparation method and application.
Background technology
Sulfur content in China's gasoline is of a relatively high, its main cause is that gasoline about 70-80% in China's comes from catalysis and splits
Change (FCC) technique.About 90% due to olefin(e) centent in gasoline product and sulfur content comes from catalytically cracked gasoline, thus causes
China's gasoline products are far from the New Set requirement for meeting sulfur content≤10ppm, olefin(e) centent≤24%.Therefore, catalysis is reduced
Cracking gasoline sulfur content, is the key for realizing China's motor petrol quality upgrading.Adsorbing desulfurization can be under conditions of normal temperature and pressure
Carry out, its energy consumption is low, and octane number hardly loses, and is relatively one of deep desulfuration approach of tool potentiality.But adsorption desulfurizing agent because
Desulfurization depth and absorption Sulfur capacity are limited, selectivity is low, the service life is shorter, desulphurizing activated relatively low, and make the adsorbent reactivation after vulcanization
It is difficult.
The content of the invention
It is an object of the invention to provide a kind of gasoline Special desulfurizing agent and its preparation method and application, to solve the above-mentioned back of the body
The problem of being proposed in scape technology.
To achieve the above object, the present invention provides following technical solution：
A kind of gasoline Special desulfurizing agent, includes according to the raw material of parts by weight：15-25 parts of vermiculite, 7-15 parts of trichloroacetic acid, three
1-5 parts of monoethanolamine, 11-19 parts of cornstarch, 3-7 parts of cashew nut shell liquid phenol-formaldehyde resin modified.
As the further scheme of the present invention：The gasoline Special desulfurizing agent, includes according to the raw material of parts by weight：Vermiculite
18-22 parts, 9-13 parts of trichloroacetic acid, 2-4 parts of triethanolamine, 13-17 parts of cornstarch, cashew nut shell liquid phenol-formaldehyde resin modified 4-6
Part.
As the further scheme of the present invention：The gasoline Special desulfurizing agent, includes according to the raw material of parts by weight：Vermiculite 20
Part, 11 parts of trichloroacetic acid, 3 parts of triethanolamine, 15 parts of cornstarch, 5 parts of cashew nut shell liquid phenol-formaldehyde resin modified.
A kind of preparation method of gasoline Special desulfurizing agent, comprises the following steps：
1) deionized water of 7-8 times of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made；
2) by vermiculite and cornstarch mixed grinding 2h, solution of trichloroacetic acid is then added, is warming up to 62-65 DEG C and at this
At a temperature of seal stir process 1.7-1.9h, then add triethanolamine and be ultrasonically treated 30-40min, mixture A is made；
3) mixture A is warming up to 85-88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, then stirred at such a temperature
30-40min is handled, then stops heating and being ultrasonically treated 15min, is stirred for doing, is then calcined in 420 DEG C of Muffle furnace
3.5h is up to desulfurizing agent.
As the further scheme of the present invention：In step 2), ultrasonic power 800W.
As the further scheme of the present invention：In step 2), mixing speed 250r/min.
As the further scheme of the present invention：In step 3), ultrasonic power 400W.
As the further scheme of the present invention：In step 3), mixing speed 180r/min.
Another object of the present invention is to provide the application of the desulfurizing agent in the oil.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention uses vermiculite, trichloroacetic acid, triethanolamine, cornstarch, cashew nut shell liquid phenol-formaldehyde resin modified and preparation
Desulfurizing agent made from technique, can be processed as sulfur content by catalytically cracked gasoline inferior<The high-quality cleaning sulfur-free gasoline of 6 μ g/g, it is pungent
The loss of alkane value is few, service life length, non-secondary pollution more friendly to environment；For this external desulfurizer after 10 regeneration, it is de-
Sulphur rate is still up to 99.4%, and regenerability is good, and activity is high, selectivity is good, and the gasoline stability after desulfurization is good.This hair
Bright preparation process is simple, easy to operate, easy to control, and performance is stablized, and production cost is low, suitable for industrialized production.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of gasoline Special desulfurizing agent, including following raw material：Vermiculite 15kg, trichloroacetic acid 7kg,
Triethanolamine 1kg, cornstarch 11kg, cashew nut shell liquid phenol-formaldehyde resin modified 3kg.
7 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made.By vermiculite and cornstarch
Mixed grinding 2h, then adds solution of trichloroacetic acid, is warming up to 62 DEG C and seals stir process 1.7h at such a temperature, stirring speed
Spend for 250r/min, then add triethanolamine and be ultrasonically treated 30min, ultrasonic power 800W, mixture A is made.Will be mixed
Compound A is warming up to 85 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, and then stir process 30min, stirring are fast at such a temperature
Spend for 180r/min, then stop heating and being ultrasonically treated 15min, ultrasonic power 400W, be stirred for dry, then at 420 DEG C
Muffle furnace in calcine 3.5h up to desulfurizing agent.
Embodiment 2
In the embodiment of the present invention, a kind of gasoline Special desulfurizing agent, including following raw material：Vermiculite 25kg, trichloroacetic acid 15kg,
Triethanolamine 5kg, cornstarch 19kg, cashew nut shell liquid phenol-formaldehyde resin modified 7kg.
8 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made.By vermiculite and cornstarch
Mixed grinding 2h, then adds solution of trichloroacetic acid, is warming up to 65 DEG C and seals stir process 1.9h at such a temperature, stirring speed
Spend for 250r/min, then add triethanolamine and be ultrasonically treated 40min, ultrasonic power 800W, mixture A is made.Will be mixed
Compound A is warming up to 88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, and then stir process 40min, stirring are fast at such a temperature
Spend for 180r/min, then stop heating and being ultrasonically treated 15min, ultrasonic power 400W, be stirred for dry, then at 420 DEG C
Muffle furnace in calcine 3.5h up to desulfurizing agent.
Embodiment 3
In the embodiment of the present invention, a kind of gasoline Special desulfurizing agent, including following raw material：Vermiculite 18kg, trichloroacetic acid 9kg,
Triethanolamine 2kg, cornstarch 13kg, cashew nut shell liquid phenol-formaldehyde resin modified 4kg.
8 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made.By vermiculite and cornstarch
Mixed grinding 2h, then adds solution of trichloroacetic acid, is warming up to 64 DEG C and seals stir process 1.8h at such a temperature, stirring speed
Spend for 250r/min, then add triethanolamine and be ultrasonically treated 35min, ultrasonic power 800W, mixture A is made.Will be mixed
Compound A is warming up to 88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, and then stir process 35min, stirring are fast at such a temperature
Spend for 180r/min, then stop heating and being ultrasonically treated 15min, ultrasonic power 400W, be stirred for dry, then at 420 DEG C
Muffle furnace in calcine 3.5h up to desulfurizing agent.
Embodiment 4
In the embodiment of the present invention, a kind of gasoline Special desulfurizing agent, including following raw material：Vermiculite 22kg, trichloroacetic acid 13kg,
Triethanolamine 4kg, cornstarch 17kg, cashew nut shell liquid phenol-formaldehyde resin modified 6kg.
8 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made.By vermiculite and cornstarch
Mixed grinding 2h, then adds solution of trichloroacetic acid, is warming up to 64 DEG C and seals stir process 1.8h at such a temperature, stirring speed
Spend for 250r/min, then add triethanolamine and be ultrasonically treated 35min, ultrasonic power 800W, mixture A is made.Will be mixed
Compound A is warming up to 88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, and then stir process 35min, stirring are fast at such a temperature
Spend for 180r/min, then stop heating and being ultrasonically treated 15min, ultrasonic power 400W, be stirred for dry, then at 420 DEG C
Muffle furnace in calcine 3.5h up to desulfurizing agent.
Embodiment 5
In the embodiment of the present invention, a kind of gasoline Special desulfurizing agent, including following raw material：Vermiculite 20kg, trichloroacetic acid 11kg,
Triethanolamine 3kg, cornstarch 15kg, cashew nut shell liquid phenol-formaldehyde resin modified 5kg.
8 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made.By vermiculite and cornstarch
Mixed grinding 2h, then adds solution of trichloroacetic acid, is warming up to 64 DEG C and seals stir process 1.8h at such a temperature, stirring speed
Spend for 250r/min, then add triethanolamine and be ultrasonically treated 35min, ultrasonic power 800W, mixture A is made.Will be mixed
Compound A is warming up to 88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, and then stir process 35min, stirring are fast at such a temperature
Spend for 180r/min, then stop heating and being ultrasonically treated 15min, ultrasonic power 400W, be stirred for dry, then at 420 DEG C
Muffle furnace in calcine 3.5h up to desulfurizing agent.
Comparative example 1
In addition to trichloroacetic acid is not contained, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
Only vermiculite, its preparation process are consistent with embodiment 5.
Comparative example 3
Only vermiculite, trichloroacetic acid, its preparation process are consistent with embodiment 5.
Comparative example 4
Each raw material is directly mixed, adds the other materials that embodiment 5 is added, the stir process 35min at 88 DEG C, stirring
Speed is 180r/min, then stops heating and being ultrasonically treated 15min, ultrasonic power 400W, is stirred for doing, then 420
DEG C Muffle furnace in calcine 3.5h up to desulfurizing agent.The additive amount of each raw material is consistent with embodiment 5.
Embodiment 6
Making choice property of sour gasoline is taken off respectively using the desulfurizing agent obtained by above-described embodiment 1-5 and comparative example 1-4
Sulphur, feeding liquid volume space velocity 2.2h-1, under conditions of 110 DEG C of temperature, pressure 0.5MPa, hydrogen and sour gasoline volume ratio 100 into
Row contact.Result of the test is shown in Table 1.
Table 1
Embodiment 7
The desulfurizing agent that 1 desulfurization process is completed to above-described embodiment 5 regenerates, and uses air as regeneration gas, and control is empty
Air volume air speed is 180h-1, temperature be 420 DEG C, normal pressure carry out burning sulphur 3h, be then down to room temperature, that is, complete the desulfurization after inactivation
The regeneration of agent.By the desulfurizing agent after 1 regeneration of above-mentioned completion to sulfur content 405 μ g/g sour gasoline again according to embodiment
6 experiment carries out desulfurization process, then repeatedly desulfurization, regeneration 5 times, 10 times.
Desulfurization, result of the test are carried out to sour gasoline respectively using the regeneration 1 time of above-mentioned gained, 5 times, the desulfurizing agent of 10 times
As shown in table 2.
Table 2
| Feedstock oil | Regeneration 1 time | Regeneration 5 times | Regeneration 10 times | |
| Total sulfur (μ g/g) | 405 | 1 | 1.2 | 2.5 |
| Alkene (v%) | 27.3 | 23.0 | 22.7 | 22.0 |
| Research octane number (RON), RON | 91.7 | 90.9 | 90.7 | 90.4 |
| Desulfurization degree (%) | - | 99.8 | 99.7 | 99.4 |
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 realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than described above limits, 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 embodiment is only wrapped
Containing an independent technical solution, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (9)
1. a kind of gasoline Special desulfurizing agent, it is characterised in that include according to the raw material of parts by weight：15-25 parts of vermiculite, trichloroacetic acid
7-15 parts, 1-5 parts of triethanolamine, 11-19 parts of cornstarch, 3-7 parts of cashew nut shell liquid phenol-formaldehyde resin modified.
2. gasoline Special desulfurizing agent according to claim 1, it is characterised in that include according to the raw material of parts by weight：Vermiculite
18-22 parts, 9-13 parts of trichloroacetic acid, 2-4 parts of triethanolamine, 13-17 parts of cornstarch, cashew nut shell liquid phenol-formaldehyde resin modified 4-6
Part.
3. gasoline Special desulfurizing agent according to claim 1, it is characterised in that include according to the raw material of parts by weight：Vermiculite
20 parts, 11 parts of trichloroacetic acid, 3 parts of triethanolamine, 15 parts of cornstarch, 5 parts of cashew nut shell liquid phenol-formaldehyde resin modified.
4. the preparation method of a kind of gasoline Special desulfurizing agent as described in claim 1-3 is any, it is characterised in that including following
Step：
1）7-8 times of deionized water of trichloroacetic acid and its quality is mixed, solution of trichloroacetic acid is made；
2）By vermiculite and cornstarch mixed grinding 2h, solution of trichloroacetic acid is then added, is warming up to 62-65 DEG C and in the temperature
Lower sealing stir process 1.7-1.9h, then adds triethanolamine and is ultrasonically treated 30-40min, mixture A is made；
3）Mixture A is warming up to 85-88 DEG C and adds cashew nut shell liquid phenol-formaldehyde resin modified, then stir process at such a temperature
30-40min, then stop heating and being ultrasonically treated 15min, it is stirred for doing, 3.5h is then calcined in 420 DEG C of Muffle furnace is
Obtain desulfurizing agent.
5. the preparation method of gasoline Special desulfurizing agent according to claim 4, it is characterised in that step 2）In, ultrasonic work(
Rate is 800W.
6. the preparation method of gasoline Special desulfurizing agent according to claim 4, it is characterised in that step 2）In, stirring speed
Spend for 250r/min.
7. the preparation method of gasoline Special desulfurizing agent according to claim 4, it is characterised in that step 3）In, ultrasonic work(
Rate is 400W.
8. the preparation method of gasoline Special desulfurizing agent according to claim 4, it is characterised in that step 3）In, stirring speed
Spend for 180r/min.
9. the application of desulfurizing agent in the oil as described in claim 1-3 is any.
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2017
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| CN101327419A (en) * | 2008-08-01 | 2008-12-24 | 中国海洋石油总公司 | Method for preparing catalytic cracking gasoline adsorbing and desulfurizing agent |
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