CN102382682B - Hydrogenation scale and corrosion inhibitor and application of scale and corrosion inhibitor - Google Patents
Hydrogenation scale and corrosion inhibitor and application of scale and corrosion inhibitor Download PDFInfo
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- CN102382682B CN102382682B CN2010102672842A CN201010267284A CN102382682B CN 102382682 B CN102382682 B CN 102382682B CN 2010102672842 A CN2010102672842 A CN 2010102672842A CN 201010267284 A CN201010267284 A CN 201010267284A CN 102382682 B CN102382682 B CN 102382682B
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- incrustation corrosion
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Abstract
The invention discloses a hydrogenation scale and corrosion inhibitor and the application of the scale and corrosion inhibitor, which resolve the problems of scaling and corroding of air coolers, heat exchangers, lower pipelines and the like of hydrogenation equipment in petroleum refining. The scale and corrosion inhibitor for hydrogenation includes following components, based on the total weight of the scale and corrosion inhibitor, (A) 5-20% of dihydric alcohol polyoxyethylene ether phosphate or trihydric alcohol polyoxyethylene ether phosphate, (B) 3-8% of benzotriazole or derivatives of the benzotriazole, (C) 5-10% of copolymer, (D) 15-50% of organic amines in a range between C2 and C6, and (E) 12-72% of alcohol compounds in a range between C1 and C9. The hydrogenation scale and corrosion inhibitor is added into working fluid at the temperature ranging from 50 DEG C to 300 DEG C and at a proportion of 5-100 micrograms per gram.
Description
Technical field
The invention belongs to a kind of corrosion inhibitor of applying in processing or coverting hydrocarbon oils equipment, relate in particular to a kind of anti-incrustation corrosion inhibitor of hydrogenation unit.
Background technology
Increasingly stringent along with oil quality and environmental requirement, hydrogen addition technology such as hydrocracking, hydrofining, hydrotreatment have become the important process process of crude oil secondary processing, in recent years, domestic oil refining enterprises processing high-sulfur, high-nitrogen stock increase gradually, corrosion failure frequently appears in the hydrogenation unit reaction effluent air cooler, failure mode is more, reason is different, the mechanism of corrosion complexity, mainly contain the galvanic corrosion of erosion, underdeposit corrosion, dew point corrosion and liquid phase, common corrosion is erosion, underdeposit corrosion.
The Cl of the S in raw material, N and trace changes H into through hydrogenation reaction
2S, NH
3And HCl, NH
3And H
2S, HCl, generate NH after reaction
4HS and NH
4Cl.Lacking under the condition of liquid water NH
4HS and NH
4Cl is directly separated out and is become solid crystals by gas phase, stops up rapidly tube bank.Common NH
4The Tc of Cl is at 210 ℃, and its crystallization is often from starting the interchanger before air cooler; And NH
4The Tc of SH is about 121 ℃, so crystallization often occurs in air cooler.In order to prevent stopping up, water filling flushing in reaction effluent before air cooler usually, flushing has been alleviated obstruction and has but been caused NH
4HS, NH
4The erosion of the Cl aqueous solution and underdeposit corrosion.
According to the variation of development need and the petroleum products demand structure of petroleum industry, the hydrogen addition technology ratio strengthens gradually.Simultaneously, it is more and more heavier that the crude oil of processing becomes the trend of weight, high-sulfur, peracid, and this has higher requirement to the anticorrosion of hydrogenation unit equipment.
At present, domestic refinery has for the prevention and control measure of Cooler in Hydro-processing corrosion: the air cooler structure design is improved; Process modification; Pipe arrangement is optimized; The material upgrading; The methods such as filling anti-incrustation corrosion inhibitor.Wherein use anti-incrustation corrosion inhibitor because investment is little, do not need to set up complicated equipment, use flexibly, easy to operate, can determine filling position and consumption according to corrosion condition, and become the important method that prevents the Cooler in Hydro-processing corrosion.It is reported; the refinery hydrogenation unit generally adopts polysulfide as composite as sodium polysulphide, ammonium polysulfide or the compounds such as polysulfide and benzotriazole as the air cooler anti-incrustation corrosion inhibitor; such inhibiter effect is better; its inhibition mechanism is: sodium polysulphide first reacts with wall and tube wall; on metallic surface, form FeS fine and close protective membrane, then Na
2S
XAgain with NH
3And other aminated compounds reaction formation ammonium polysulfide, thereby reduced NH
4HS, NH
4The fouling of Cl and deposition, suppressed corrosion.But, because dividing, sodium polysulphide chance air parses elemental sulfur, make the place's fouling of high pressure water injection pump mechanical sealing, have a strong impact on going into operation the life-span of waterflood pump.In addition, a kind of water-soluble anti-incrustation corrosion inhibitor of ocean, bibliographical information Shenyang chemistry company limited development uses and obtains good effect at Liaoyang Petrochemical Company's refinery hydroeracking unit air cooler.China Petrochemical Industry's Guangzhou Branch adds a kind of anti-incrustation corrosion inhibitor before the high-pressure air cooler water filling, the sour water iron ion content of high-pressure separator obviously descends, and has effectively suppressed the corrosion of air cooler and pipeline.
The inhibiter patent of using about oil refining apparatus both at home and abroad is very many, but few for the anti-incrustation corrosion inhibitor of hydrogenation unit reaction effluent air cooler, interchanger.Chinese patent CN1804000A discloses a kind of by polyoxy alkene aminated compounds, tertiary butyl phenols, acrylic copolymer, homopolymer, aromatic hydrocarbon based one or more anti-incrustation corrosion inhibitors that form, and the polyoxy alkene aminated compounds that uses in this technology, tertiary butyl phenols material cause mainly for free radical the organic deposition that chain reaction or polymer substance condensation reaction generate; Acrylic copolymer, homopolymer class are that calcium phosphate, calcium carbonate, calcium phosphate etc. are had to good dispersion, restraining effect, to NH
4HS, NH
4The ammonium salts such as Cl but do not have restraining effect.Patent CN1754944A discloses a kind of anti-incrustation corrosion inhibitor that is comprised of fatty nitrogenous compound, aromatic series sulfocompound, organic acid acetic, imidazoles woods derivative, in this technology, used a kind of raw material of m-sulfanilic acid, this material has severe toxicity, is not suitable in industrial a large amount of uses.US Patent No. 5387733 discloses and non-filming amine compounds is added on to the position of stream temperature before reducing has suppressed NH in oil refining process
4Cl is deposited on equipment surface; Patent US5256276 disclose the use phospholipids compounds as Yelkin TTS as suppressing NH
4The Scale inhibitors of Cl salt sedimentation; Patent 5282956 discloses with dimethyl amine compounds and dimethyl thiourea and has suppressed NH as anti-incrustation corrosion inhibitor
4The deposition of Cl salt.These technology are mainly from suppressing NH
4The fouling of Cl salt sedimentation is set out, and does not consider corrosion inhibition, but, in the equipment such as Cooler in Hydro-processing, also has H
2S-HCl-NH
3Solution corrosion and erosion, so if the corrosion of ACU should be considered scale inhibition and corrosion inhibition simultaneously.
There is following problem in disclosed patent about the hydrogenation anti-incrustation corrosion inhibitor at present:
1. the scale inhibition composition in anti-incrustation corrosion inhibitor is mainly for the separating out, deposit of the calcium salts such as calcium carbonate, calcium phosphate, or causes for free radical the organic deposition that chain reaction or polymer substance condensation reaction generate.
2. function singleness, what possess scale inhibition function does not possess corrosion inhibitive function; What possess corrosion inhibitive function does not possess scale inhibition function, does not have simultaneously the auxiliary agent of scale inhibition and corrosion inhibitive function.
Summary of the invention
The present invention is directed to hydrocracking, hydrotreater air cooler, interchanger and downstream line because of NH
4Cl, NH
4Underdeposit corrosion and solution erosion that HS deposition causes, provide a kind of novel anti-incrustation corrosion inhibitor composition with scale inhibition, corrosion inhibitive function, with and application.
Composite corrosion inhibitor provided by the invention is comprised of following component:
(A) the dibasic alcohol polyoxyethylene ether phosphate of 5～20 % by weight or trivalent alcohol polyoxyethylene ether phosphate;
(B) the benzotriazole or derivatives thereof of 3～8 % by weight;
(C) multipolymer of 5～10 % by weight;
(D) the small molecules organic amine of 15～50 % by weight;
(E) 12～72 % by weight alcohol compounds;
The best proportioning of each component is:
(A) the dibasic alcohol polyoxyethylene ether phosphate of 10～15 % by weight or trivalent alcohol polyoxyethylene ether phosphate;
(B) the benzotriazole or derivatives thereof of 4～6 % by weight;
(C) multipolymer of 6～8 % by weight;
(D) the small molecules organic amine of 35～45 % by weight;
(E) 26～45 % by weight alcohol compounds;
Wherein dibasic alcohol polyoxyethylene ether phosphate general structure is suc as formula shown in (1); Trivalent alcohol polyoxyethylene ether phosphate general structure is suc as formula shown in (2).
In formula, m, n, k are 3～10 integers; X in formula (1) is 0～2 integer; R1 and R2 are H, methyl or ethyl; Y, z in formula (2) is 0～1 integer; R3 and R4 are H or methyl.
The general structure of benzotriazole is suc as formula shown in (3),
Described Benzotriazole Derivative can be 4-methyl benzotriazazole or 5-methyl benzotriazazole.
Described multipolymer is toxilic acid and acrylic copolymer, toxilic acid and acrylate copolymer or vinylformic acid and acrylate copolymer, preferred toxilic acid and methyl acrylate copolymer or vinylformic acid and Propylene glycol monoacrylate multipolymer, preferably toxilic acid and methyl acrylate copolymer.
Described small molecules organic amine is primary amine or secondary amine, preferred C
2～C
6Alkylamine, C
2～C
4Hydramine or various polyethylene polyamine.C
2～C
6The preferred Tri N-Propyl Amine of alkylamine, n-Butyl Amine 99, n-amylamine, normal hexyl Amine, quadrol or butanediamine, preferably quadrol; C
2～C
4The preferred Monoethanolamine MEA BASF of hydramine, diethanolamine or trolamine, preferably Monoethanolamine MEA BASF; The preferred diethylenetriamine of polyethylene polyamine, triethylene tetramine or tetraethylene pentamine.Preferably diethylenetriamine or triethylene tetramine.
Described organic solvent is C
1～C
9Alcohols, preferred alcohol, propyl alcohol, ethylene glycol or propylene glycol.
Anti-incrustation corrosion inhibitor of the present invention, its preparation method is at normal temperature, normal pressure with under constantly stirring, respectively by the dibasic alcohol polyoxyethylene ether phosphate of certain mass or trivalent alcohol polyoxyethylene ether phosphate, benzotriazole or derivatives thereof, multipolymer, small molecules organic amine, join in alcohol compound, until each component is dissolved fully, namely make anti-incrustation corrosion inhibitor of the present invention.
The application of a kind of hydrogenation anti-incrustation corrosion inhibitor of the present invention, add 5～100 μ g/g in the working fluid of 50～300 ℃, preferred 10～50 μ g/g.Particularly the hydrogenation anti-incrustation corrosion inhibitor is joined in the desalination water pot, after mixing, by water filling, be injected into together in working fluid, corrosion inhibition rate can reach more than 80%.
A kind of hydrogenation anti-incrustation corrosion inhibitor of the present invention is specially adapted in air cooler, interchanger and the pipeline thereof of the process units such as hydrocracking, hydrotreatment, hydrofining.
A kind of hydrogenation anti-incrustation corrosion inhibitor of the present invention compared with prior art, has the following advantages: on the one hand can with NH
4Cl, NH
4Chemical reaction occurs in HS ammonium salts etc., generate a kind of material that is difficult for crystallization under air cooler, heat exchange temperature condition, thereby avoided separating out, depositing of ammonium salt, to the ammonium salt that has deposited, has on the one hand the effect of dispersion, have simultaneously stronger corrosion inhibitive function, suppress the effect of corrosive medium to equipment surface.
Embodiment
Below with specific embodiment, describe the present invention in detail, but embodiment does not limit the scope of the invention.
Embodiment 1-7 is that anti-incrustation corrosion inhibitor prepares example, refers to table 1.
Under normal temperature, normal pressure, the continuous stirring, respectively a certain amount of compound in table 1 is joined in the alcohol compound of respective amount, until each component is dissolved fully, namely make anti-incrustation corrosion inhibitor of the present invention.
Table 1 embodiment 1-7 anti-incrustation corrosion inhibitor component and proportioning
Embodiment 8～14
With the anti-incrustation corrosion inhibitor sample of embodiment 1～7, carry out respectively the evaluation example of scale-inhibiting properties, the results are shown in Table 2.
In round-bottomed flask, prepare the heavy aromatics of 200ml, add the NH of 0.31g
4Cl, be heated to boiling temperature, and the distillation certain hour, with the distilled water flushing prolong of 100ml, is collected water of condensation, and the nitrogen content in minute bleed, calculate NH thus
4The distillation amount of Cl.Contrast adds the nitrogen content in agent and blank assay prolong wash-down water, with this, calculates scale inhibition performance, sample 1
#～7
#It is respectively the anti-incrustation corrosion inhibitor sample of embodiment 1～7 preparation.
Table 2 anti-incrustation corrosion inhibitor scale-inhibiting properties experimental result
Embodiment 15～22
With the anti-incrustation corrosion inhibitor sample of embodiment 1～7, carry out respectively the evaluation of corrosion inhibition, the results are shown in Table 3.On the air cooler of 100ml/h hydrocracking experimental installation, carry out coupon test.
Processing condition are as follows:
Temperature: refining 380 ℃; 390 ℃ of crackings
Pressure: 10Mpa
Oil inlet quantity: 100g/h
Amounts of hydrogen: 1000ml/min
Water injection rate: 18g/h
Air cooler temperature in: 140
Air cooler temperature out: 40 ℃
Add dosage: 50 μ g/g
Test period: 144 hours
N content in raw material: 944 μ g/g
S content in raw material: 2.32%
For making NH in water filling
4HS Theoretical Calculation concentration reaches 5%, in water filling, adds a certain amount of ammoniacal liquor, in raw material, adds a certain amount of CS
2, with this understanding, the weightlessness of 144 hours is 22.0mg, sample 1
#～7
#It is respectively the anti-incrustation corrosion inhibitor sample of embodiment 1～7 preparation.
The corrosion inhibition experimental result of table 3 anti-incrustation corrosion inhibitor
| Embodiment | Sample | Weightlessness/mg | Corrosion inhibition rate, % |
| Blank | 22.0 | ||
| Embodiment 15 | 1# | 1.408 | 93.6 |
| Embodiment 16 | 2# | 8.492 | 61.4 |
| Embodiment 17 | 3# | 6.6 | 70.0 |
| Embodiment 18 | 4# | 2.068 | 90.6 |
| Embodiment 19 | 5# | 3.234 | 85.3 |
| Embodiment 20 | 6# | 7.15 | 67.5 |
| Embodiment 21 | 7# | 2.772 | 87.4 |
From the result of table 2 and table 3, can find out, the anti-incrustation corrosion inhibitor sample of embodiment 1～7 preparation shows good scale inhibitor effect.
Claims (8)
1. hydrogenation anti-incrustation corrosion inhibitor, it is characterized in that: this hydrogenation anti-incrustation corrosion inhibitor is comprised of following component:
(A) the dibasic alcohol polyoxyethylene ether phosphate of 5～20 % by weight or trivalent alcohol polyoxyethylene ether phosphate;
(B) benzotriazole of 3～8 % by weight or 4-methyl benzotriazazole or 5-methyl benzotriazazole;
(C) toxilic acid of 5～10 % by weight and acrylic copolymer, toxilic acid and acrylate copolymer or acrylic acid and acrylic ester copolymers;
(D) C of 15～50 % by weight
2～C
6Alkylamine, C
2～C
4Hydramine or polyethylene polyamine;
(E) C of 12～72 % by weight
1～C
9Alcohol compound;
In the anti-incrustation corrosion inhibitor gross weight;
Wherein dibasic alcohol polyoxyethylene ether phosphate general structure is suc as formula shown in (1); Trivalent alcohol polyoxyethylene ether phosphate general structure is suc as formula shown in (2):
In formula, m, n, k are 3～10 integers; X in formula (1) is 0～2 integer; R1 and R2 are H, methyl or ethyl; Y, z in formula (2) is 0～1 integer; R3 and R4 are H or methyl.
2. hydrogenation anti-incrustation corrosion inhibitor according to claim 1, it is characterized in that: component (A) is 10～15 % by weight; Component (B) is 4～6 % by weight; Component (C) is 6～8 % by weight; Component (D) is 35～45 % by weight; Component (E) is 26～45 % by weight; In the anti-incrustation corrosion inhibitor gross weight.
3. hydrogenation anti-incrustation corrosion inhibitor according to claim 1, it is characterized in that: described component (C) is toxilic acid and methyl acrylate copolymer or vinylformic acid and Propylene glycol monoacrylate multipolymer.
4. hydrogenation anti-incrustation corrosion inhibitor according to claim 1, it is characterized in that: described component (C) is toxilic acid and methyl acrylate copolymer.
5. hydrogenation anti-incrustation corrosion inhibitor according to claim 1, is characterized in that: C
2～C
6Alkylamine be Tri N-Propyl Amine, n-Butyl Amine 99, n-amylamine, normal hexyl Amine, quadrol or butanediamine; C
2～C
4Hydramine be Monoethanolamine MEA BASF, diethanolamine or trolamine; Polyethylene polyamine is diethylenetriamine, triethylene tetramine or tetraethylene pentamine.
6. hydrogenation anti-incrustation corrosion inhibitor according to claim 1, is characterized in that: C
2～C
6Alkylamine be quadrol; C
2～C
4Hydramine be Monoethanolamine MEA BASF; Polyethylene polyamine is diethylenetriamine or triethylene tetramine.
7. the application of a hydrogenation anti-incrustation corrosion inhibitor, it is characterized in that: the hydrogenation anti-incrustation corrosion inhibitor that adds 5～100 μ g/g in the working fluid of 50～300 ℃, this hydrogenation anti-incrustation corrosion inhibitor is joined in the desalination water pot, after mixing, by water filling, be injected in working fluid together.
8. the application of hydrogenation anti-incrustation corrosion inhibitor according to claim 7 is characterized in that: the hydrogenation anti-incrustation corrosion inhibitor that adds 10～50 μ g/g in the working fluid of 50～300 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104293393A (en) * | 2014-07-21 | 2015-01-21 | 宜兴市星光宝亿化工有限公司 | Hydrogenation scale inhibitor of residual oil and preparation method thereof |
| WO2017189801A1 (en) * | 2016-04-29 | 2017-11-02 | Dow Global Technologies Llc | Process for controlling corrosion in petroleum refining units |
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|---|---|---|---|---|
| CN103820151B (en) * | 2014-03-17 | 2015-07-01 | 宜兴市宝隆化工有限公司 | Corrosion inhibitor for hydrogenation unit and preparation method thereof |
| CN104003528B (en) * | 2014-05-29 | 2016-04-20 | 西安石油大学 | A kind of disinfecting inhibiter |
| CN106244236A (en) * | 2016-08-30 | 2016-12-21 | 山东恒信科技发展有限公司 | A kind of anti-incrustation corrosion inhibitor for hydrogenation plant and preparation method thereof |
| CN112786118B (en) * | 2019-11-06 | 2024-05-03 | 中国石油化工股份有限公司 | Memory, corrosion risk assessment method, device and equipment for hydrogenation reaction effluent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5256276A (en) * | 1992-05-18 | 1993-10-26 | Betz Laboratories, Inc. | Method for the inhibition and removal of ammonium chloride deposition in hydrocarbon processing units by adding lecithin |
| CN1804000A (en) * | 2005-01-14 | 2006-07-19 | 上海贵通新材料科技有限公司 | Corrosion and scale inhibitor for hydrogenation plant |
-
2010
- 2010-08-25 CN CN2010102672842A patent/CN102382682B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5256276A (en) * | 1992-05-18 | 1993-10-26 | Betz Laboratories, Inc. | Method for the inhibition and removal of ammonium chloride deposition in hydrocarbon processing units by adding lecithin |
| CN1804000A (en) * | 2005-01-14 | 2006-07-19 | 上海贵通新材料科技有限公司 | Corrosion and scale inhibitor for hydrogenation plant |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104293393A (en) * | 2014-07-21 | 2015-01-21 | 宜兴市星光宝亿化工有限公司 | Hydrogenation scale inhibitor of residual oil and preparation method thereof |
| CN104293393B (en) * | 2014-07-21 | 2016-03-30 | 宜兴市星光宝亿化工有限公司 | A kind of residual hydrogenation Scale inhibitors and preparation method thereof |
| WO2017189801A1 (en) * | 2016-04-29 | 2017-11-02 | Dow Global Technologies Llc | Process for controlling corrosion in petroleum refining units |
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| CN102382682A (en) | 2012-03-21 |
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