CN1247816C - Multifunctional corrosion inhibitor and preparation method thereof - Google Patents
Multifunctional corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN1247816C CN1247816C CN03134877.7A CN03134877A CN1247816C CN 1247816 C CN1247816 C CN 1247816C CN 03134877 A CN03134877 A CN 03134877A CN 1247816 C CN1247816 C CN 1247816C
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- preparation
- inhibiter
- corrosion
- polyethers
- oil
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- 238000005260 corrosion Methods 0.000 title claims abstract description 25
- 230000007797 corrosion Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003112 inhibitor Substances 0.000 title abstract description 6
- 229920000570 polyether Polymers 0.000 claims abstract description 15
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000001412 amines Chemical class 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 6
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960001124 trientine Drugs 0.000 claims abstract description 5
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims abstract description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims abstract description 3
- 229960003237 betaine Drugs 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 7
- 239000003350 kerosene Substances 0.000 claims description 5
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- GZBMXTMYZCMQJT-UHFFFAOYSA-N [Na].BrC(F)(F)F Chemical compound [Na].BrC(F)(F)F GZBMXTMYZCMQJT-UHFFFAOYSA-N 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical group CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 2
- 238000012512 characterization method Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
- -1 polyethylene Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000839 emulsion Substances 0.000 abstract description 5
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract 1
- 238000004581 coalescence Methods 0.000 abstract 1
- 238000005536 corrosion prevention Methods 0.000 abstract 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 230000006837 decompression Effects 0.000 description 6
- 239000000376 reactant Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007764 o/w emulsion Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Landscapes
- Polyethers (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention relates to a multifunctional corrosion inhibitor applied to corrosion prevention of a top pipe component of a normal and reduced pressure tower of an oil refinery and a preparation method thereof, wherein the molecular structure of the corrosion inhibitor is characterized by sulfonic acid betaine type, belongs to zwitterions and has excellent corrosion inhibition performance, the polymer takes amine (such as triethylene tetramine) as an initiator, and propylene oxide and ethylene oxide block polyether are introduced, so that the polymer is an excellent demulsifier, and has the characteristics of good coalescence effect, high dehydration rate, clear color of dehydrated water and small using amount for water-in-oil (O/W) emulsion.
Description
Technical field
The present invention relates to a kind of refinery ordinary decompression column push pipe parts rot-resistant multi-functional corrosion inhibior and preparation method thereof that is applied to.
Background technology
Sodium ions content in the refinery heavy oil catalytic cracking process requirement catalytically cracked stock for this reason, has been cancelled the anti-corrosion measure that atmospheric and vacuum distillation is annotated alkali behind the crude oil desalting less than 1ppm.Therefore, the ordinary decompression column top volatilization line decompression cat head HCl-H of condenser system that finds time
2O-H
2S-O
2-H
2The O corrosive medium is to the corrosion aggravation of processing unit pipeline.At present, extensively adopt injection filming amine inhibiter to slow down the corrosion of initial set district, inner wall of tower and internals.The use of inhibiter all has certain conditions: 1. inhibiter pH use range.It is the most effective that general use inhibiter wishes that the pH value remains between the 5.5-7.0.Being lower than this scope needs very high dosage, uneconomical; It is very little to be higher than this scope inhibiter effect.Because inhibiter will form complete protective membrane, need exist by a metal sulfide film, and under high pH value, sulfide has dissolved tendency.2. solvability.The solvability of most of film inhibitors is all very poor, in the use, all will could be dispersed in the overhead product well by solvent.The good inhibiter of oil soluble can form layer protecting film in the metallic surface.Simultaneously, in order to protect the metallic surface of aqueous portion, also wish to have certain water dispersible.3. concentration range.Inhibiter is various in style, and nature difference is big, and the concentration of use also has nothing in common with each other.Some inhibiter does not just have provide protection when concentration is lower than certain numerical value; When consumption was big, most of filming amine inhibiter all had the certain surface activity, can cause that phenomenons such as oil emulsion, foaming make the defective and increase loss of oil quality.
Summary of the invention
The objective of the invention is synthetic a kind of oil soluble organic inhibitor, make carbon steel in water and oil-phase medium, all be subjected to excellent protection, and have oil product breakdown of emulsion function concurrently, reduce the oil product loss with premium properties.In the medium that uses, have good chemical stability, be applicable to the pH value scope of broad, oil quality is had no adverse effects.
Multi-functional corrosion inhibior molecular characterization of the present invention is the sulphonic acid betaine type, and its molecular formula is:
Wherein, R
1=(C
3H
6O)
y(C
2H4O)
xH, x=5-30; Y=15-50; Q=2-3; R=1-3.
Multi-functional corrosion inhibior preparation process of the present invention is as follows, is initiator with the organic amine, and these initiators can be quadrols, diethylenetriamine, triethylene tetramine, polyethylene polyamine, and their mixture, and propylene oxide (PO) polymerization, with sodium hydroxide or potassium hydroxide is catalyzer, and temperature of reaction 90-150 ℃, reaction pressure is 0.15-0.45MPa, treat to feed oxyethane (EO) again after PO absorbs fully, EO is polyethers after absorbing fully.Get above-mentioned polyethers, splash into bromotrifluoromethane sodium sulfonate or 1 behind the adding solvent cut, 3-trimethylene base-sulfinic acid lactone, temperature of reaction is 40-60 ℃, steams the dissolving of solvent adding kerosene after reacting completely and evenly is finished product.In the reaction process, by the molecular weight of adjusting material add-on control polyethers and the ratio of PO/EO.One or more alkylsulphonic acid groups can be with in a plurality of active centre on the initiator; Each alkylsulphonic acid group contains 2-3 carbon atom.
Multi-functional corrosion inhibior of the present invention belongs to zwitter-ion, has good surfactivity and lower water-soluble.Chelation group and surface active groups are become one; can arrive the metallic surface rapidly, strengthen them greatly in the metallic surface chemisorption, form the unit molecule protective membrane of one deck densification with the sequestering power of metal ion; play the effect of passive metal protection metal, had good corrosion inhibition.In addition, this polymkeric substance is an initiator with organic amine (as triethylene tetramine), introduces propylene oxide and ethylene oxide block polyethers, is a kind of good emulsion splitter.Have coalescent effectively for water-in-oil-type (O/W) milk sap, rate of water loss is fast, deviates from the characteristics that the water color is clear and consumption is few.
Embodiment
Embodiment 1
1. propylene oxide (PO), oxyethane (EO) block co-polyether
In the 500ml autoclave of electric mixer is housed, add the 23.0g diethylenetriamine, and the 80ml Mixed XYLENE, adding 0.2g potassium hydroxide is catalyzer, under the condition of heating and stirring, feeds 70.0gPO and 15.0gEO successively, range of reaction temperature 120-140 ℃.Decompression steams dimethylbenzene and promptly gets required polyethers after absorbing fully.
2. inhibiter is synthetic
In band stirring, thermometer, the prolong 500ml there-necked flask, add polyethers 41.0g and 220ml dehydrated alcohol.Carefully add 36.0g bromotrifluoromethane sodium sulfonate in three batches, temperature of reaction is 60 ℃, and reinforced 2.5 hours heat filterings of Bi Huiliu are removed white solid in the solution, steams the product that the ethanol in the filtrate obtains then and is finished product.
The inhibiter simulative corrosion test
In an airtight band stirred flask, test(ing) medium is for containing 1200ppm HCl; 800ppmH
2The sour water of S, inhibiter add-on are 30ppm; The test piece material is A
3Carbon steel, speed of rotation are 60-80 rev/min, and test period is 48 hours, and test temperature is 85 ± 1 ℃.
Inhibiter simulative corrosion test result:
| Inhibiter | Add-on ppm | Test piece area cm 2 | The weightless g of test piece | Corrosion rate mm/a | Average corrosion rate mm/a | Corrosion inhibition rate % | Etch state |
| Blank | 0 | 14.4636 | 0.4145 | 6.7053 | 7.0288 | 0 | Severe pitting |
| Blank | 0 | 14.8042 | 0.4652 | 7.3523 | Severe pitting | ||
| Example 1 | 30 | 14.0802 | 0.0056 | 0.0931 | 0.0923 | 98.7 | Uniform corrosion |
| Example 1 | 30 | 13.0358 | 0.0051 | 0.0915 | Uniform corrosion |
Embodiment 2
1. propylene oxide (PO), oxyethane (EO) block co-polyether
In the 500ml autoclave of electric mixer is housed, add the 23.0g triethylene tetramine, and the 80ml Mixed XYLENE, adding 0.2g sodium hydroxide is catalyzer, under the condition of heating and stirring, feeds 70.0gPO and 15.0gEO successively, range of reaction temperature 120-140 ℃.Decompression steams dimethylbenzene and promptly gets institute after absorbing fully
Need polyethers.
2. inhibiter is synthetic
In band stirring, thermometer, the prolong 500ml there-necked flask, add polyethers 40.0g and 200ml1, in the 2-ethylene dichloride, be heated to 50 ℃, slowly drip 1,3-trimethylene base-sulfinic acid lactone 21.0g (the dropping time is about 50 minutes), this reaction is thermopositive reaction, should take the external cooling measure, temperature of reaction is 40 ℃.Dropwise, reactant refluxes and made reaction reach complete in about 2.5 hours.Removal of solvent under reduced pressure and unreacted reactant are cooled to the dissolving of room temperature adding 40ml kerosene and evenly are finished product.
The test of inhibiter breakdown of emulsion effect
Dehydration test is carried out (bottle examination method) according to ordinary method.Under the room temperature condition, get kerosene 800.0g, add emulsifying agent 2.0g, treat to add the 200.0g deionized water after the stirring and dissolving, carry out emulsification with the emulsification pretreatment machine, rotating speed is 5000-5500 rev/min, and the time is 3-5 minute, and oil in water emulsion is standby.Add above-mentioned oil in water emulsion 75.0g in the tapered test tube of 100ml tool plug band scale, and example 2.2 inhibiter that add metering put into water bath with thermostatic control and takes out after 15 minutes, vibrated 5 minutes on vibrator, put back in the water bath with thermostatic control again, time recording is deviate from the water body product.
The oil sample water ratio is 20%; 85 ± 1 ℃ of bath temperatures; Density of corrosion inhibitor 100ppm.
| Inhibiter | Add-on ppm | Dehydration rate amount ml | Dehydration rate % | The sewage color | ||||
| Dewatering time min | 10 | 20 | 30 | 60 | 90 | |||
| Blank | 0 | 2.6 | 3.9 | 6.2 | 7.4 | No change | 49.3 | The interface is unclear |
| Blank | 0 | 3.1 | 4.2 | 6.3 | 7.8 | No change | 52.0 | The interface is unclear |
| Example 2 | 100 | 7.9 | 12.3 | 13.1 | 13.9 | No change | 92.7 | The interface is clear |
| Example 2 | 100 | 8.5 | 12.8 | 13.5 | 14.2 | No change | 94.7 | The interface is clear |
Embodiment 3
In the 500ml autoclave of electric mixer is housed, add the 23.0g quadrol, and the 80ml Mixed XYLENE, adding 0.2g sodium hydroxide is catalyzer, under the condition of heating and stirring, feeds 70.0gPO and 15.0gEO successively, range of reaction temperature 120-140 ℃.Decompression steams dimethylbenzene and promptly gets required polyethers after absorbing fully.
Inhibiter is synthetic
In band stirring, thermometer, the prolong 500ml there-necked flask, add polyethers 40.0g and 200ml1, in the 2-ethylene dichloride, be heated to 50 ℃, slowly drip 1,3-trimethylene base-sulfinic acid lactone 21.0g (the dropping time is about 50 minutes), this reaction should be taked the external cooling measure for thermopositive reaction.Dropwise, reactant refluxes and made reaction reach complete in about 2.5 hours.Removal of solvent under reduced pressure and unreacted reactant are cooled to the dissolving of room temperature adding 40ml kerosene and evenly are finished product.
Claims (3)
1. the preparation method of a multi-functional corrosion inhibior, it is characterized in that: be initiator with the organic amine, and propylene oxide (PO) polymerization, be catalyzer with sodium hydroxide or potassium hydroxide, temperature of reaction 90-150 ℃, reaction pressure is 0.15-0.45MPa, treat to feed oxyethane (EO) again after PO absorbs fully, EO is polyethers after absorbing fully, splashes into bromotrifluoromethane sodium sulfonate or 1 behind the adding solvent cut, 3-trimethylene base-sulfinic acid lactone steams the dissolving of solvent adding kerosene and evenly is finished product after reacting completely.
2. the preparation method of multi-functional corrosion inhibior according to claim 1, it is characterized in that: organic amine is quadrol, diethylenetriamine, triethylene tetramine, polyethylene polyamine or their mixture.
3. the multi-functional corrosion inhibior of the preparation method of multi-functional corrosion inhibior according to claim 1 preparation, it is characterized in that: the inhibiter molecular characterization is the sulphonic acid betaine polyethers, belongs to zwitterionics, its molecular formula is
Wherein, R
1=(C
3H
6O)
y(C
2H
4O)
xH, x=5-30; Y=15-50; Q=2-3; R=1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN03134877.7A CN1247816C (en) | 2003-09-27 | 2003-09-27 | Multifunctional corrosion inhibitor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN03134877.7A CN1247816C (en) | 2003-09-27 | 2003-09-27 | Multifunctional corrosion inhibitor and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1600902A CN1600902A (en) | 2005-03-30 |
| CN1247816C true CN1247816C (en) | 2006-03-29 |
Family
ID=34659131
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN03134877.7A Expired - Fee Related CN1247816C (en) | 2003-09-27 | 2003-09-27 | Multifunctional corrosion inhibitor and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1247816C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368049C (en) * | 2005-06-06 | 2008-02-13 | 中国科学院化学研究所 | Chemical demulsifier |
| CN100526508C (en) * | 2006-04-04 | 2009-08-12 | 中国石油天然气股份有限公司 | Corrosion inhibitor for inhibiting metal corrosion and preparation method thereof |
| CN101642692B (en) * | 2008-08-05 | 2012-07-25 | 中国科学院化学研究所 | Composite type crude oil demulsifier and preparation method thereof |
| CN104592957B (en) * | 2013-11-01 | 2017-05-17 | 中国石油化工股份有限公司 | Sulfonic-group-containing polyamine shale inhibitor and preparation method thereof |
| CN104404485B (en) * | 2014-11-14 | 2017-04-05 | 无锡伊佩克科技有限公司 | A kind of galvanized layer chromium-free passivant and preparation method thereof |
| CN107603582B (en) * | 2017-10-20 | 2020-06-09 | 陕西省石油化工研究设计院 | Efficient foaming agent for air foam flooding and preparation method thereof |
-
2003
- 2003-09-27 CN CN03134877.7A patent/CN1247816C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1600902A (en) | 2005-03-30 |
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