CN106987842B - A kind of high temperature resistant corrosion inhibitor and preparation method thereof - Google Patents
A kind of high temperature resistant corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN106987842B CN106987842B CN201710270960.3A CN201710270960A CN106987842B CN 106987842 B CN106987842 B CN 106987842B CN 201710270960 A CN201710270960 A CN 201710270960A CN 106987842 B CN106987842 B CN 106987842B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/16—Sulfur-containing compounds
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Abstract
The invention discloses a kind of preparation methods of high temperature resistant corrosion inhibitor, which comprises the following steps: (1) amino-phenol is reacted to synthesis of alkyl amide groups phenol with long chain fatty acids；(2) by alkylamidoalkyl phenol and strong sulfuric acid response, then potassium hydroxide solid is compounded to get sulphonated fatty amide base phenol corrosion inhibiter is arrived.The invention has the beneficial effects that: the corrosion inhibiter thermal stability for using method of the invention to be prepared is good, inhibition efficiency is high at high temperature, at 300 DEG C, naphthenic acidity is 10mgKOH/g, when corrosion inhibiter dosage is greater than 10mg/L, it can reach 90% to the corrosion inhibition rate of A3 steel disc in white oil medium, and corrosion rate is less than 0.080mm/a.
Description
Technical field
The present invention relates to a kind of corrosion inhibiter and preparation method thereof, and in particular to a kind of resistance to height for inhibiting petroleum acid corrosion equipment
Warm corrosion inhibiter and preparation method thereof belongs to oil field technical field of anticorrosion.
Background technique
Acidic materials in petroleum are referred to as petroleum acids.Petroleum acids mainly includes aphthenic acids, fatty acid, aromatic acid and some
Other inorganic acids account for the 1%-2% of crude oil.
Petroleum acids, organic sulfur, inorganic salts and it is some have corrosive auxiliary agent be to be caused in oil extraction and process
The principal element of equipment corrosion.And petroleum acids has the corrosion of very strong corrosivity, especially high temperature position most to oil refining apparatus
It is serious.
Currently, being one of the most effective measure for inhibiting petroleum acid corrosion equipment by the way that high-temperature corrosion inhibitor is added.However, due to
Petroleum refining need to carry out at a high temperature of 300 DEG C or so, this just proposes very high requirement to the heat resistance of corrosion inhibiter.
In recent years, many scientific research personnel are dedicated to the R&D work of high-temperature corrosion inhibitor in the world, and also developing many has
The corrosion inhibiter of preferable corrosion inhibition and heat resistance.But most of high-temperature corrosion inhibitor or there is toxicity or be difficult to degrade,
Certain harm is caused to the mankind and environment or corrosion mitigating effect at high temperature is undesirable.
Therefore, the ecological requirements that environmental-friendly high-temperature corrosion inhibitor more meets today's society are developed.However, high-temperature corrosion inhibitor
Type and application are less at present, and generally compound to obtain using several reagents, and corrosion mitigating effect in practical applications is also paid no attention to
Think, therefore develops a kind of without phosphorus high-temperature corrosion inhibitor for being able to satisfy refinery's demand and have broad application prospects.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide it is a kind of it is environmental-friendly, refinery can be met simultaneously
The preparation method of corrosion inhibiter and the corrosion inhibiter that high temperature resistant and high-efficient corrosion inhibition type require.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A kind of preparation method of high temperature resistant corrosion inhibitor, which comprises the following steps:
Step1: amino-phenol is dissolved in dimethylformamide, is heated to 60 DEG C, long-chain fat is added dropwise while stirring
The molar ratio of acid, long chain fatty acids and amino-phenol is 1:1.2, and 80 DEG C are warming up to after being added dropwise to complete, continues to be stirred to react 3h, so
After be warming up to 160 DEG C -180 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after be cooled to 90 DEG C -95 DEG C,
With the solvent dimethylformamide in Rotary Evaporators removed under reduced pressure product, yellow, viscous liquid is obtained；
The concentrated sulfuric acid, the molar ratio of yellow, viscous liquid and the concentrated sulfuric acid are added in Step2: Xiang Shangshu yellow, viscous liquid
For 1:1.25,70 DEG C of -75 DEG C of reaction 2h-3h of reaction temperature are controlled, potassium hydroxide solid is added after the reaction was completed and is compounded, obtains
To high temperature resistant corrosion inhibitor, the molar ratio of potassium hydroxide and the concentrated sulfuric acid is 1:2.
The preparation method of high temperature resistant corrosion inhibitor above-mentioned, which is characterized in that in Step1, aforementioned amino-phenol is to ammonia
Base phenol, o-aminophenol or m-aminophenol, preferably para-aminophenol.
The preparation method of high temperature resistant corrosion inhibitor above-mentioned, which is characterized in that in Step1, aforementioned amino-phenol and diformazan
The mass ratio of base formamide is 1:6-8.
The preparation method of high temperature resistant corrosion inhibitor above-mentioned, which is characterized in that in Step1, foregoing long-chain fatty acid isR is C10-C20Alkyl.
The invention has the beneficial effects that: the corrosion inhibiter thermal stability being prepared using method of the invention is good, in height
The lower inhibition efficiency of temperature is high, at 300 DEG C, naphthenic acidity 10mgKOH/g, when corrosion inhibiter dosage is greater than 10mg/L, in white oil
90% can be reached to the corrosion inhibition rate of A3 steel disc in medium, corrosion rate is less than 0.080mm/a.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 1；
Fig. 2 is the thermogravimetric thermal stability analysis result figure of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 1；
Fig. 3 is the infrared spectrogram of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 2；
Fig. 4 is the thermogravimetric thermal stability analysis result figure of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 2；
Fig. 5 is the infrared spectrogram of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 3；
Fig. 6 is the thermogravimetric thermal stability analysis result figure of sulphonated fatty amide base phenol corrosion inhibiter synthesized by embodiment 3.
Specific embodiment
Specific introduce is made to the present invention below in conjunction with the drawings and specific embodiments.
Embodiment 1
It weighs 10g para-aminophenol to be dissolved in 80g dimethylformamide (DMF), is heated to 60 DEG C, is added dropwise while stirring
25g ready denier oil acid (molar ratio of ready denier oil acid and para-aminophenol is 1:1.2), is warming up to 80 after being added dropwise
DEG C, continue to be stirred to react 3h, then heat to 170 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after drop
Temperature, with the solvent DMF in Rotary Evaporators removed under reduced pressure product, obtains yellow, viscous liquid alkyl amide groups phenol to 95 DEG C.
The concentrated sulfuric acid (alkylamidoalkyl phenol and the dense sulphur that 13g mass fraction is 98% are added into above-mentioned alkylamidoalkyl phenol
The molar ratio of acid is 1:1.25), 70 DEG C of reaction 3h of reaction temperature are controlled, 14g potassium hydroxide solid (hydrogen-oxygen is added after the reaction was completed
Changing potassium with the molar ratio of the concentrated sulfuric acid is 1:2) it is compounded, obtain sulphonated fatty amide base phenol corrosion inhibiter.
The infrared spectrogram of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 1.
Infrared structure analysis: 3287cm-1- OH the stretching vibration of the phenol for being absorbed as intermolecular poly association of place Qiang Erkuan,
3080cm-1For the N-H stretching vibration of secondary amide, strong 1690cm-1It is absorbed as the peak C=O of secondary amide, 1337cm-1It is sulfonic group
O=S=O stretching absorbance peak, 669cm-1It is sulfonic C-S stretching vibration absworption peak, 903cm-1、1907cm-1、1989cm-1
The absorption peak at place is the C-H out-of-plane bending vibration absorption peak of 1,2,4 substituted benzene rings.
We evaluate corrosion inhibiter thermal stability by thermogravimetry, so that the Applicable temperature of corrosion inhibiter is investigated,
The thermogravimetric thermal stability analysis result figure of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 2.
As shown in Figure 2: the decomposition temperature of synthesized sulphonated fatty amide base phenol corrosion inhibiter illustrates this at 340 DEG C or so
The good thermal stability of corrosion inhibiter.
Embodiment 2
It weighs 10g m-aminophenol to be dissolved in 80g dimethylformamide (DMF), is heated to 60 DEG C, is added dropwise while stirring
25g ready denier oil acid (molar ratio of ready denier oil acid and m-aminophenol is 1:1.2), is warming up to 80 after being added dropwise
DEG C, continue to be stirred to react 3h, then heat to 180 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after drop
Temperature, with the solvent DMF in Rotary Evaporators removed under reduced pressure product, obtains yellow, viscous liquid alkyl amide groups phenol to 90 DEG C.
The concentrated sulfuric acid (alkylamidoalkyl phenol and the dense sulphur that 13g mass fraction is 98% are added into above-mentioned alkylamidoalkyl phenol
The molar ratio of acid is 1:1.25), 70 DEG C of reaction 3h of reaction temperature are controlled, 14g potassium hydroxide solid (hydrogen-oxygen is added after the reaction was completed
Changing potassium with the molar ratio of the concentrated sulfuric acid is 1:2) it is compounded, obtain sulphonated fatty amide base phenol corrosion inhibiter.
The infrared spectrogram of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 3.
Infrared structure analysis: 3287cm-1- OH the stretching vibration of the phenol for being absorbed as intermolecular poly association of place Qiang Erkuan,
3080cm-1For the N-H stretching vibration of secondary amide, strong 1690cm-1It is absorbed as the peak C=O of secondary amide, 1337cm-1It is sulfonic group
O=S=O stretching absorbance peak, 669cm-1It is sulfonic C-S stretching vibration absworption peak, 903cm-1、1907cm-1、1989cm-1
The absorption peak at place is the C-H out-of-plane bending vibration absorption peak of 1,2,4 substituted benzene rings.
We evaluate corrosion inhibiter thermal stability by thermogravimetry, so that the Applicable temperature of corrosion inhibiter is investigated,
The thermogravimetric thermal stability analysis result figure of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 4.
As shown in Figure 4: the decomposition temperature of synthesized sulphonated fatty amide base phenol corrosion inhibiter illustrates this at 340 DEG C or so
The good thermal stability of corrosion inhibiter.
Embodiment 3
It weighs 10g o-aminophenol to be dissolved in 80g dimethylformamide (DMF), is heated to 60 DEG C, is added dropwise while stirring
25g ready denier oil acid (molar ratio of ready denier oil acid and o-aminophenol is 1:1.2), is warming up to 80 after being added dropwise
DEG C, continue to be stirred to react 3h, then heat to 180 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after drop
Temperature, with the solvent DMF in Rotary Evaporators removed under reduced pressure product, obtains yellow, viscous liquid alkyl amide groups phenol to 90 DEG C.
The concentrated sulfuric acid (alkylamidoalkyl phenol and the dense sulphur that 13g mass fraction is 98% are added into above-mentioned alkylamidoalkyl phenol
The molar ratio of acid is 1:1.25), 70 DEG C of reaction 3h of reaction temperature are controlled, 14g potassium hydroxide solid (hydrogen-oxygen is added after the reaction was completed
Changing potassium with the molar ratio of the concentrated sulfuric acid is 1:2) it is compounded, obtain sulphonated fatty amide base phenol corrosion inhibiter.
The infrared spectrogram of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 5.
Infrared structure analysis: 3287cm-1- OH the stretching vibration of the phenol for being absorbed as intermolecular poly association of place Qiang Erkuan,
3080cm-1For the N-H stretching vibration of secondary amide, strong 1690cm-1It is absorbed as the peak C=O of secondary amide, 1337cm-1It is sulfonic group
O=S=O stretching absorbance peak, 669cm-1It is sulfonic C-S stretching vibration absworption peak, 903cm-1、1907cm-1、1989cm-1
The absorption peak at place is the C-H out-of-plane bending vibration absorption peak of 1,2,4 substituted benzene rings.
We evaluate corrosion inhibiter thermal stability by thermogravimetry, so that the Applicable temperature of corrosion inhibiter is investigated,
The thermogravimetric thermal stability analysis result figure of synthesized sulphonated fatty amide base phenol corrosion inhibiter is shown in Fig. 6.
As shown in Figure 6: the decomposition temperature of synthesized sulphonated fatty amide base phenol corrosion inhibiter illustrates this at 380 DEG C or so
The good thermal stability of corrosion inhibiter.
Embodiment 4
It weighs 10g para-aminophenol to be dissolved in 80g dimethylformamide (DMF), is heated to 60 DEG C, is added dropwise while stirring
22g stearic acid (molar ratio of stearic acid and para-aminophenol is 1:1.2), is warming up to 80 DEG C, it is anti-to continue stirring after being added dropwise
Answer 3h, then heat to 180 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after be cooled to 90 DEG C, with rotation
Turn the solvent DMF in evaporation under reduced pressure removing product, obtains yellow, viscous liquid alkyl amide groups phenol.
The concentrated sulfuric acid (alkylamidoalkyl phenol and the dense sulphur that 13g mass fraction is 98% are added into above-mentioned alkylamidoalkyl phenol
The molar ratio of acid is 1:1.25), 75 DEG C of reaction 2h of reaction temperature are controlled, 14g potassium hydroxide solid (hydrogen-oxygen is added after the reaction was completed
Changing potassium with the molar ratio of the concentrated sulfuric acid is 1:2) it is compounded, obtain sulphonated fatty amide base phenol corrosion inhibiter.
Embodiment 5
It weighs 10g para-aminophenol to be dissolved in 80g dimethylformamide (DMF), is heated to 60 DEG C, is added dropwise while stirring
20g palmitinic acid (molar ratio of palmitinic acid and para-aminophenol is 1:1.2), is warming up to 80 DEG C, it is anti-to continue stirring after being added dropwise
Answer 3h, then heat to 180 DEG C, separate from water segregator the water of generation by flowing back, it is anhydrous distillate after be cooled to 90 DEG C, with rotation
Turn the solvent DMF in evaporation under reduced pressure removing product, obtains yellow, viscous liquid alkyl amide groups phenol.
The concentrated sulfuric acid (alkylamidoalkyl phenol and the dense sulphur that 13g mass fraction is 98% are added into above-mentioned alkylamidoalkyl phenol
The molar ratio of acid is 1:1.25), 75 DEG C of reaction 2h of reaction temperature are controlled, 14g potassium hydroxide solid (hydrogen-oxygen is added after the reaction was completed
Changing potassium with the molar ratio of the concentrated sulfuric acid is 1:2) it is compounded, obtain sulphonated fatty amide base phenol corrosion inhibiter.
The performance evaluation of high-temperature corrosion inhibitor
Experimental raw: aphthenic acids/white oil medium (acid value 10mgKOH/g).
Experimental provision: corrosion inhibiter laboratory evaluation device.
Experimental temperature: 260~340 DEG C.
Measures: sealing and circulating.
Experimental period: 12h.
Experiment corrosion inhibiter: the preparation-obtained high-temperature corrosion inhibitor of embodiment 1-5.
Corrosion inhibiter dosage: 10mg/L.
Method measures high temperature referring to the measurement rotary hanging plate method of national standard GB/T 18175-2000 water treatment agent corrosion inhibition
The corrosion inhibition rate of non-phosphate inhibitor, evaluating result are shown in Table 1.
1 corrosion inhibiter performance evaluation of table
From the test result of table 1: the corrosion inhibiter thermal stability being prepared using method of the invention is good, in high temperature
Lower inhibition efficiency is high, and at 300 DEG C, naphthenic acidity 10mgKOH/g when corrosion inhibiter dosage is greater than 10mg/L, is situated between in white oil
90% can be reached to the corrosion inhibition rate of A3 steel disc in matter, corrosion rate is less than 0.080mm/a.
It can be seen that by the corrosion inhibiter use being prepared using method of the invention on refining equipment, it can be effective
Inhibit naphthenic acid corrosion refining equipment.
It should be noted that the above embodiments do not limit the invention in any form, it is all to use equivalent replacement or equivalent change
The mode changed technical solution obtained, falls within the scope of protection of the present invention.
Claims (6)
1. a kind of preparation method of high temperature resistant corrosion inhibitor, which comprises the following steps:
Step1: amino-phenol is dissolved in dimethylformamide, is heated to 60 DEG C, and long chain fatty acids are added dropwise while stirring, long
The molar ratio of chain fatty acid and amino-phenol is 1:1.2, and 80 DEG C are warming up to after being added dropwise to complete, continues to be stirred to react 3h, then rise
Temperature separates from water segregator the water of generation by flowing back to 160 DEG C -180 DEG C, it is anhydrous distillate after be cooled to 90 DEG C -95 DEG C, with rotation
Turn the solvent dimethylformamide in evaporation under reduced pressure removing product, obtains yellow, viscous liquid；
It is added the concentrated sulfuric acid in Step2: Xiang Shangshu yellow, viscous liquid, the molar ratio of yellow, viscous liquid and the concentrated sulfuric acid is 1:
1.25,70 DEG C of -75 DEG C of reaction 2h-3h of reaction temperature are controlled, potassium hydroxide solid is added after the reaction was completed and is compounded, obtains resistance to
The molar ratio of high-temperature corrosion inhibitor, potassium hydroxide and the concentrated sulfuric acid is 1:2.
2. the preparation method of high temperature resistant corrosion inhibitor according to claim 1, which is characterized in that in Step1, the amino
Phenol is para-aminophenol, o-aminophenol or m-aminophenol.
3. the preparation method of high temperature resistant corrosion inhibitor according to claim 2, which is characterized in that in Step1, the amino
Phenol is para-aminophenol.
4. the preparation method of high temperature resistant corrosion inhibitor according to claim 1, which is characterized in that in Step1, the amino
The mass ratio of phenol and dimethylformamide is 1:6-8.
5. the preparation method of high temperature resistant corrosion inhibitor according to claim 1, which is characterized in that in Step1, the long-chain
Fatty acid isR is C10-C20Alkyl.
6. a kind of high temperature resistant corrosion inhibitor that the preparation method as described in claim 1 to 5 any one is prepared.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5252254A (en) * | 1992-12-30 | 1993-10-12 | Nalco Chemical Company | Naphthenic acid corrosion inhibitor |
| CN101440493A (en) * | 2008-12-17 | 2009-05-27 | 南京石油化工股份有限公司 | High temperature corrosion inhibitor for atmospheric vacuum distillation apparatus |
| CN102304069A (en) * | 2011-06-23 | 2012-01-04 | 东北石油大学 | Method for synthesizing saturated cardanol sulfonate surfactant for oil displacement |
| CN102367575A (en) * | 2011-08-29 | 2012-03-07 | 上海贵通新材料科技有限公司 | High temperature resistant corrosion inhibitor for oil refining device, its preparation method and application |
| CN106433781A (en) * | 2016-09-09 | 2017-02-22 | 徐文忠 | High-temperature corrosion inhibitor for oilfield exploitation and petroleum refining process and preparation method of high-temperature corrosion inhibitor |
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- 2017-04-24 CN CN201710270960.3A patent/CN106987842B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5252254A (en) * | 1992-12-30 | 1993-10-12 | Nalco Chemical Company | Naphthenic acid corrosion inhibitor |
| CN101440493A (en) * | 2008-12-17 | 2009-05-27 | 南京石油化工股份有限公司 | High temperature corrosion inhibitor for atmospheric vacuum distillation apparatus |
| CN102304069A (en) * | 2011-06-23 | 2012-01-04 | 东北石油大学 | Method for synthesizing saturated cardanol sulfonate surfactant for oil displacement |
| CN102367575A (en) * | 2011-08-29 | 2012-03-07 | 上海贵通新材料科技有限公司 | High temperature resistant corrosion inhibitor for oil refining device, its preparation method and application |
| CN106433781A (en) * | 2016-09-09 | 2017-02-22 | 徐文忠 | High-temperature corrosion inhibitor for oilfield exploitation and petroleum refining process and preparation method of high-temperature corrosion inhibitor |
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