CN109504440A - A kind of slurry fouling inhibitor - Google Patents
A kind of slurry fouling inhibitor Download PDFInfo
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- CN109504440A CN109504440A CN201811362491.9A CN201811362491A CN109504440A CN 109504440 A CN109504440 A CN 109504440A CN 201811362491 A CN201811362491 A CN 201811362491A CN 109504440 A CN109504440 A CN 109504440A
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- slurry
- fouling inhibitor
- polyisobutene
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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
- C10G75/00—Inhibiting corrosion or fouling in apparatus for treatment or conversion of hydrocarbon oils, in general
- C10G75/04—Inhibiting corrosion or fouling in apparatus for treatment or conversion of hydrocarbon oils, in general by addition of antifouling agents
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- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a kind of slurry fouling inhibitor, the component including following mass fraction: detergent dispersant 25~40%, phenol amine type antioxidant 6~12%, corrosion inhibiter 5~10%, detersive 0.5~3%, matal deactivator 0.4~0.5%, surplus is solvent.The detergent dispersant is polyisobutene succinimide and/or polybutadiene sulfenyl phosphoric acid hexylene glycol ester.Slurry fouling inhibitor freezing point of the present invention is low (≤- 15 DEG C), small (the 20 DEG C of kinematic viscosity≤50mm of viscosity2/s)；Oxidation resistance is strong, thermal stability is good, its property and service performance are not influenced under 350~400 DEG C of higher temperature, suitable for catalytic cracking unit in slurry service scale inhibition and scale removal application, additive amount of the slurry fouling inhibitor in slurry oil is 30~100ppm, the equipment coking such as slurry service, pipeline and heat exchanger can effectively be inhibited, scale inhibition performance guarantees equipment safety even running up to 90%.
Description
Technical field
The present invention relates to slurry service equipment knot is prevented when a kind of a kind of antisludging agent, in particular to catalytically cracked stock
Dirty, coking slurry fouling inhibitor.
Background technique
It is catalytic cracked into one of the important device of refinery.In recent years, with catalytic cracking technology be constantly progressive and petroleum
The raising of working depth, the ratio for mixing refining residual oil are continuously increased, and the raw material of catalytic cracking also becomes to become increasingly complex therewith, more next
It is heavier.Due to the deterioration of raw material oil nature, the condensed-nuclei aromatics condensation product and catalyst particle deposition formed in process is in oil
Slurry system, slurry service equipment scaling, coking phenomenon lead to the reduction of the slurry heat-exchanger thermal efficiency, affect the normal production of device
And long-term operation, and the safe operation of equipment is directly affected, cause device to be forced to stop production when serious.Therefore, catalysis is solved
The coking of cracking slurry service and fouling problem have become the important topic for guaranteeing Long Period Running of Fccu.Refinery operations
Person proposes a series of methods for solving scale problems, such as reduces Fractionator Bottom temperature from different angles such as equipment, technique, operations
Degree, reduction residence time, raising slurry oil flow velocity, installation slurry oil filter etc. all achieve certain effect, but all there is one
Fixed limitation.One of the most economic and effective method is exactly that trace mineral supplement-slurry oil is added in processing raw material
Antisludging agent, to inhibit the formation of dirt.
Generally contain metal surface passivant in existing antisludging agent, be mainly metallic salt, contains these components
Antisludging agent can have an impact to the ash content index of later product so that the quality decline of product, not metalline currently not yet
The antisludging agent of class occurs, therefore not can avoid the appearance of this problem.
Summary of the invention
The present invention provides a kind of inhibition slurry service coking for shortcoming existing for existing antisludging agent, reduces oil
Slurry heat exchanger dismantles the slurry fouling inhibitor and preparation method thereof of the cleaning frequency.
What the purpose of the present invention was achieved through the following technical solutions:
A kind of slurry fouling inhibitor, the component including following mass fraction: detergent dispersant 25~40%, phenol amine type antioxidant
6~12%, corrosion inhibiter 5~10%, detersive 0.5~3%, matal deactivator 0.4~0.5%, surplus is solvent.
The detergent dispersant is polyisobutene succinimide and/or polybutadiene sulfenyl phosphoric acid hexylene glycol ester.
Preferably, the detergent dispersant is polyisobutene succinimide and polybutadiene sulfenyl phosphoric acid hexylene glycol ester
Composition, the mass ratio of polyisobutene succinimide and polybutadiene sulfenyl phosphoric acid hexylene glycol ester is 8~15:1.
The polyisobutene succinimide be 2300 using molecular weight polyisobutene as raw material, through hot adduction technique
Synthesis.
The molecular weight of the polyisobutene is 2300, molecular weight distribution 1.8, and alpha-olefin content is 88%.
Specifically, the polyisobutene succinimide is as made from following methods:
Step (1), alkylation reaction: under conditions of nitrogen protection, maleic anhydride and polyisobutene are in temperature 210~220
4~5h is reacted at DEG C；It is evaporated under reduced pressure after reaction, steams maleic anhydride, obtain polyisobutylene butanedioic anhydride；Wherein, described
Maleic anhydride and polyisobutene molar ratio=1.4~1.6:1；
Step (2), aminating reaction: tetraethylenepentamine is slowly dropped to the polyisobutylene butanedioic anhydride of step (1) acquisition
In, 3~5h is reacted at 130~140 DEG C；Wherein, the molar ratio of the polyisobutylene butanedioic anhydride and tetraethylenepentamine is 1
~1.1:1.
The polybutadiene sulfenyl phosphoric acid hexylene glycol ester is as made from following methods: with polybutadiene sulfenyl phosphoric acid and
Hexylene glycol is raw material, using dimethylbenzene as solvent, in 150 DEG C of heating reflux reaction 2h, is then slowly increased to 180 DEG C, stops adding
Heat stops wait flowing back, obtains polybutadiene sulfenyl phosphoric acid hexylene glycol ester；Wherein polybutadiene sulfenyl phosphoric acid (polybutadiene monomers
Average relative molecular mass be 1300) and the molar ratio of hexylene glycol be 1:1.
The phenol amine type antioxidant is 2,6- di-t-butyl -1- dimethyl paracresol, is contained in slurry oil for removing
Oxygen reduces the generation of hydrocarbons polymerization reaction.
The corrosion inhibiter is benzimidazole mercaptan, can neutralize the acidic materials in hydrocarbon stream, is formed and is protected in equipment surface
The corrosion to equipment is mitigated or eliminated in cuticular layer.
The detersive is that super base number synthesizes sulfonic acid magnesium (detersive T107), and neutralising capacity is strong, rust-preventing characteristic is good and has
Certain dispersibility.
The matal deactivator is N- salicylamide phthalimide (matal deactivator THMD-5).
The solvent is dimethylbenzene and diesel quality ratio is 6~10:1 mixed solvent.
It is a further object to provide the preparation methods of the slurry fouling inhibitor, comprising: in temperature 35~40
At DEG C, detergent dispersant is added into solvent, until completely dissolved, sequentially adds detersive, phenol amine type antioxidant, metal passivation
Agent, corrosion inhibiter, stir evenly to get slurry fouling inhibitor.
The application of slurry fouling inhibitor of the present invention scale inhibition and scale removal in slurry service in catalytic cracking unit, especially
Suitable for mixing the scale inhibition of slurry service and scale removal the refining higher catalytic cracking unit of residual oil ratio.The slurry fouling inhibitor exists
Additive amount in slurry oil is 30~100ppm.
Compared to the prior art, beneficial effects of the present invention:
Polyisobutene succinimide of the present invention belongs to oil-soluble dispersant, is the nonpolar alkyl (oleophylic by being dissolved in oil
Base) and polar group (hydrophilic group) composition amphiphilic structure substance, and have stronger lipophilicity；Its polar group is oxygen-containing or nitrogen
Group.The lipophilic group of polyisobutene succinimide is bigger than metal detergent, can effectively barrier carbon deposit and jelly are mutual
Aggregation, can make the particle of 0~50nm size by peptization.Simultaneously because polyisobutene succinimide contain ionization polarity it is big,
It is allowed to be scattered in oil also by the bigger particle of charge repulsion peptization.When concentration is larger in the oil for oil soluble surfactant
When, mainly exist with micelle state, micella is by tens sides that surfactant molecule is inside with polar group, lipophilic group is outside
Formula aligns the molecule aggregate of composition.When generating the liquid solutes such as undissolvable water, organic acid in the oil in oil, glue
Beam is interacted by its polar group and liquid droplet and these liquid droplets is enclosed in inside micella, them are greatly reduced
Interfacial tension between oil, under the action of dispersing agent, above-mentioned original substance undissolvable in the oil becomes able to dissolve,
To reduce the activity of these compounds, the harmful deposits such as carbon deposit, paint film are gathered into after preventing its further oxidative condensation
Or corrosion surface of the work.Liquid polar material insoluble in oil, due to being divided there is the interaction between dispersing agent
It is scattered in oil, like the dissolution phenomena of solute.Polyisobutene succinimide in addition to play the role of reduce solution surface tension it
Outside, there are also the multiple functions such as dispersion, emulsification, solubilising, washing, wetting, infiltration, since isobutene succimide is basic species
Matter also has the function of neutralizing acidic materials.
In addition, polybutadiene sulfenyl phosphoric acid hexylene glycol ester is added in slurry fouling inhibitor, not only there are other types to hinder
The scale inhibition function of dirty agent, moreover it is possible to form phosphorous free radical, and generate metal-phosphorus complex with metal and cover metal surface, effectively
Prevent all kinds of dirts in equipment logistics side fouling.
Using benzimidazole mercaptan as corrosion inhibiter, the acidic materials in hydrocarbon stream can be neutralized, form protective film in equipment surface
Layer, is mitigated or eliminated the corrosion to equipment.Sulfonic acid magnesium is synthesized using super base number simultaneously, not only there is certain dispersibility, but also
Neutralising capacity is strong, and the acidic materials in hydrocarbon stream can be neutralized jointly with benzimidazole mercaptan, are provided simultaneously with rustless property, can be to setting
It is standby to play a protective role.
Using N- salicylamide phthalimide as matal deactivator, can the metal ions such as same iron, copper form chelate, make it
The catalytic capability to polymerization reaction is lost, the formation of organic polymer is inhibited and then reduces the generation of incrustation.2,6- di-t-butyl-
1- dimethyl paracresol can reduce the generation of hydrocarbons polymerization reaction for removing the oxygen contained in slurry oil.
Slurry fouling inhibitor freezing point of the present invention is low (≤- 15 DEG C), small (the 20 DEG C of kinematic viscosity≤50mm of viscosity2/s)；Antioxygen
Change ability is strong, and thermal stability is good, does not influence its property and service performance under 350~400 DEG C of higher temperature, can effectively inhibit
The equipment coking such as slurry service, pipeline and heat exchanger, scale inhibition performance guarantee equipment safety even running, heat exchanger up to 90%
After changing with reaction tower coking phenomenon, efficiency is improved, make to exchange heat and is reacted more abundant.
Detailed description of the invention
Fig. 1 is evaluation experimental device schematic diagram；
Fig. 1,1- slurry oil slot, 2- oil-slurry pump, 3- fouling measurement pipe, 4- heating furnace, 5- thermocouple.
Specific embodiment
Technical solution of the present invention is described further below by specific embodiment.
Polyisobutene succinimide is as made from following methods:
Step (1), alkylation reaction: under conditions of nitrogen protection, maleic anhydride and the polyisobutene (molecule of polyisobutene
Amount is 2300, molecular weight distribution 1.8, and alpha-olefin content is 88%) anti-at 210~220 DEG C of temperature according to molar ratio=1.4
Answer 5h；It is evaporated under reduced pressure after reaction, steams maleic anhydride, obtain polyisobutylene butanedioic anhydride；
Step (2), aminating reaction: tetraethylenepentamine is slowly dropped to the polyisobutylene butanedioic anhydride of step (1) acquisition
In, 5h is reacted at 140 DEG C；Wherein, the molar ratio of the polyisobutylene butanedioic anhydride and tetraethylenepentamine is 1.1:1.
Polybutadiene sulfenyl phosphoric acid hexylene glycol ester is as made from following methods: with polybutadiene sulfenyl phosphoric acid and hexylene glycol
In 150 DEG C of heating reflux reaction 2h, 180 DEG C are then slowly increased to, stops heating, wait return using dimethylbenzene as solvent for raw material
Stream stops, and obtains polybutadiene sulfenyl phosphoric acid hexylene glycol ester；Wherein polybutadiene sulfenyl phosphoric acid (the average phase of polybutadiene monomers
1300) to molecular weight be and the molar ratio of hexylene glycol is 1:1.
Embodiment 1
A kind of slurry fouling inhibitor, the component including following mass fraction: polyisobutene succinimide (detergent dispersant)
30%, 2,6- di-t-butyl -1- dimethyl paracresol (phenol amine type antioxidant) 10%, benzimidazole mercaptan (corrosion inhibiter) 5%, clearly
Net agent T107 0.8%, matal deactivator THMD-5 0.5%, surplus are the mixed solvent of dimethylbenzene and diesel quality ratio 10:1.
At 40 DEG C of temperature, detergent dispersant is added into solvent, until completely dissolved, sequentially add detersive T107,
2,6- di-t-butyl -1- dimethyl paracresol, matal deactivator THMD-5, benzimidazole mercaptan stir evenly to get slurry oil resistance
Dirty agent, -14.1 DEG C of freezing point, kinematic viscosity (20 DEG C) 42.6mm2/s。
Embodiment 2
A kind of slurry fouling inhibitor, the component including following mass fraction: polyisobutene succinimide (detergent dispersant)
30%, polybutadiene sulfenyl phosphoric acid hexylene glycol ester (detergent dispersant) 3%, 2,6- di-t-butyl -1- dimethyl paracresol (phenol amine
Type antioxidant) 10%, benzimidazole mercaptan (corrosion inhibiter) 5%, detersive T107 0.8%, matal deactivator THMD-5
0.5%, surplus is the mixed solvent of dimethylbenzene and diesel quality ratio 10:1.
The preparation method is the same as that of Example 1, resulting slurry fouling inhibitor, and -14.2 DEG C of freezing point, kinematic viscosity (20 DEG C)
42.9mm2/s。
Embodiment 3
A kind of slurry fouling inhibitor, the component including following mass fraction: polyisobutene succinimide (detergent dispersant)
32%, polybutadiene sulfenyl phosphoric acid hexylene glycol ester (detergent dispersant) 4%, 2,6- di-t-butyl -1- dimethyl paracresol (phenol amine
Type antioxidant) 10%, benzimidazole mercaptan (corrosion inhibiter) 5%, detersive T107 0.8%, matal deactivator THMD-5
0.5%, surplus is the mixed solvent of dimethylbenzene and diesel quality ratio 10:1.
The preparation method is the same as that of Example 1, resulting slurry fouling inhibitor, and -13.5 DEG C of freezing point, kinematic viscosity (20 DEG C)
42.4mm2/s。
Embodiment 4
A kind of slurry fouling inhibitor, the component including following mass fraction: polyisobutene succinimide (detergent dispersant)
28%, polybutadiene sulfenyl phosphoric acid hexylene glycol ester (detergent dispersant) 2%, 2,6- di-t-butyl -1- dimethyl paracresol (phenol amine
Type antioxidant) 10%, benzimidazole mercaptan (corrosion inhibiter) 5%, detersive T107 0.8%, matal deactivator THMD-5
0.5%, surplus is the mixed solvent of dimethylbenzene and diesel quality ratio 10:1.
The preparation method is the same as that of Example 1, resulting slurry fouling inhibitor, and -13.8 DEG C of freezing point, kinematic viscosity (20 DEG C)
42.7mm2/s。
Embodiment 5
A kind of slurry fouling inhibitor, the component including following mass fraction: polyisobutene succinimide (detergent dispersant)
28%, polybutadiene sulfenyl phosphoric acid hexylene glycol ester (detergent dispersant) 2%, 2,6- di-t-butyl -1- dimethyl paracresol (phenol amine
Type antioxidant) 6%, benzimidazole mercaptan (corrosion inhibiter) 8%, detersive T107 1.5%, matal deactivator THMD-5 0.4%,
Surplus is the mixed solvent of dimethylbenzene and diesel quality ratio 8:1.
The preparation method is the same as that of Example 1, resulting slurry fouling inhibitor, and -13.9 DEG C of freezing point, kinematic viscosity (20 DEG C)
43.0mm2/s。
Appraisal of scale mitigating effect
Evaluation experimental device mainly includes (see Fig. 1) such as oil-slurry pump (flow is adjustable), fouling measurement pipe, heating furnaces.In
State's petrochemical industry Shijiangzhuang Oil-Refining Chemical Co., Ltd. catalytic cracked oil pulp is raw material, presses 120g/h flow velocity for slurry oil with oil-slurry pump
It is sent into measurement pipe, effective heating furnace is measured and is heated to certain temperature and keeps temperature constant.With passing through for slurry oil, incrustation is being surveyed
Buret inner wall is constantly assembled, by measurement pipe is dropped to room temperature for 24 hours, weigh and measures incrustation amount.According to blank test group and add
The different incrustation amount of agent test group can find out scale inhibition performance.
Blank test: slurry fouling inhibitor is not added；Add agent test group: slurry fouling inhibitor additive amount is the 100ppm of slurry oil.
Table 1: appraisal of scale mitigating effect test result
Claims (10)
1. a kind of slurry fouling inhibitor, it is characterised in that the component including following mass fraction: detergent dispersant 25~40%, phenol amine
Type antioxidant 6~12%, corrosion inhibiter 5~10%, detersive 0.5~3%, matal deactivator 0.4~0.5%, surplus are solvent.
2. slurry fouling inhibitor according to claim 1, it is characterised in that the detergent dispersant is polyisobutene fourth two
Acid imide and/or polybutadiene sulfenyl phosphoric acid hexylene glycol ester.
3. slurry fouling inhibitor according to claim 2, it is characterised in that the detergent dispersant is polyisobutene fourth two
The composition of acid imide and polybutadiene sulfenyl phosphoric acid hexylene glycol ester, polyisobutene succinimide and polybutadiene sulfenyl phosphoric acid
The mass ratio of hexylene glycol ester is 8~15:1.
4. slurry fouling inhibitor according to claim 2 or 3, it is characterised in that the polyisobutene succinimide be with
The polyisobutene that molecular weight is 2300 is raw material, through the synthesis of hot adduction technique；The molecular weight of the polyisobutene is 2300,
Molecular weight distribution is 1.8, and alpha-olefin content is 88%.
5. slurry fouling inhibitor according to claim 1, it is characterised in that the phenol amine type antioxidant is the tertiary fourth of 2,6- bis-
Base -1- dimethyl paracresol.
6. slurry fouling inhibitor according to claim 1, it is characterised in that the corrosion inhibiter is benzimidazole mercaptan.
7. slurry fouling inhibitor according to claim 1, it is characterised in that the detersive is that super base number synthesizes sulfonic acid magnesium.
8. slurry fouling inhibitor according to claim 1, it is characterised in that the matal deactivator is N- salicylamide phthalein
Acid imide.
9. slurry fouling inhibitor according to claim 1, it is characterised in that the solvent is dimethylbenzene and diesel quality ratio
For 6~10:1 mixed solvent.
10. the application of slurry fouling inhibitor described in claim 1 scale inhibition and scale removal in slurry service in catalytic cracking unit, institute
Additive amount of the slurry fouling inhibitor stated in slurry oil is 30~100ppm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811362491.9A CN109504440A (en) | 2018-11-15 | 2018-11-15 | A kind of slurry fouling inhibitor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811362491.9A CN109504440A (en) | 2018-11-15 | 2018-11-15 | A kind of slurry fouling inhibitor |
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ID=65748607
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205161A (en) * | 2019-06-11 | 2019-09-06 | 黄河三角洲京博化工研究院有限公司 | A kind of high temperature resistant slurry fouling inhibitor |
| CN111925825A (en) * | 2020-07-28 | 2020-11-13 | 广东粤首新科技有限公司 | Scale inhibition and dispersion agent and preparation method and application thereof |
| CN113773875A (en) * | 2021-10-09 | 2021-12-10 | 江苏科创石化有限公司 | Catalytic cracking slurry oil scale inhibitor and preparation method thereof |
| CN116444702A (en) * | 2023-05-11 | 2023-07-18 | 山东非金属材料研究所 | Preparation method of polyisobutene oil for viscosity standard substance |
-
2018
- 2018-11-15 CN CN201811362491.9A patent/CN109504440A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205161A (en) * | 2019-06-11 | 2019-09-06 | 黄河三角洲京博化工研究院有限公司 | A kind of high temperature resistant slurry fouling inhibitor |
| CN110205161B (en) * | 2019-06-11 | 2021-05-07 | 山东益丰生化环保股份有限公司 | High-temperature-resistant oil slurry scale inhibitor |
| CN111925825A (en) * | 2020-07-28 | 2020-11-13 | 广东粤首新科技有限公司 | Scale inhibition and dispersion agent and preparation method and application thereof |
| CN113773875A (en) * | 2021-10-09 | 2021-12-10 | 江苏科创石化有限公司 | Catalytic cracking slurry oil scale inhibitor and preparation method thereof |
| CN116444702A (en) * | 2023-05-11 | 2023-07-18 | 山东非金属材料研究所 | Preparation method of polyisobutene oil for viscosity standard substance |
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Application publication date: 20190322 |