CN101717944B - Method for preparing corrosion inhibitor by utilizing cottonseed oil - Google Patents
Method for preparing corrosion inhibitor by utilizing cottonseed oil Download PDFInfo
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- CN101717944B CN101717944B CN2009102545257A CN200910254525A CN101717944B CN 101717944 B CN101717944 B CN 101717944B CN 2009102545257 A CN2009102545257 A CN 2009102545257A CN 200910254525 A CN200910254525 A CN 200910254525A CN 101717944 B CN101717944 B CN 101717944B
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Abstract
The invention relates to a method for preparing a corrosion inhibitor by utilizing cottonseed oil. The cottonseed oil corrosion inhibitor is prepared by the following steps of: synthesizing a precursor of the corrosion inhibitor by using cottonseed oil and diethylenetriamine as raw materials; and reacting the precursor of the corrosion inhibitor with benzyl chloride to generate a water-solube cottonseed oil corrosion inhibitor. The prepared cottonseed oil corrosion inhibitor has good corrosion inhibition effect on hydrochloric acid at 70 DEG C, has the advantages of high corrosion inhibiting rate, good chemical stability and heat stability, and less medicine consumption, and is especially suitable for being used as a boiler acid cleaning corrosion inhibitor.
Description
Technical field
The invention belongs to corrosion and guard technology field, particularly a kind of method for preparing inhibiter with Oleum Gossypii semen.
Background technology
Pickling is widely used in industries such as metallic substance, machinery, metallurgy, chemical industry, is the important means of rust cleaning, scale removal.But because acid has corrosive nature to hardware, " crossing erosion " phenomenon often appears in acid cleaning process, especially the corrosion of mineral acid is even more serious, the hydrogen of being emitted simultaneously can spread to metal inside, makes and is washed equipment generation hydrogen embrittlement, therefore will add inhibiter when pickling, to suppress the corrosion of metal in acidic medium, reduce the usage quantity of acid, improve pickling effect, prolong the work-ing life of equipment.Not only to consider the molten iron ability of acid during pickling, also should consider other multiple factor, so the important step that a kind of effective inhibiter of selection is pickling.
The water-soluble imidazoline derivative is that a class does not have the specific stimulation smell, Heat stability is good, and the inhibiter that toxicity is low, it has good corrosion inhibition for general corrosions in acidic medium such as carbon steel, steel alloy, copper.But this type of inhibiter uses alkane reagent such as dimethylbenzene aborning mostly at present, very big environmental pollution and hazardness are arranged, and also there is the high shortcoming of price in product.
Summary of the invention
The object of the present invention is to provide a kind of renewable resources cottonseed that utilizes, with the Oleum Gossypii semen is the method for feedstock production imidazolines inhibiter owing to do not use alkane reagent such as dimethylbenzene, therefore pollute little, harm is low, and have a save energy, the characteristics that reduce production costs.
For achieving the above object, the technical solution used in the present invention is:
1) at first will get mixture in Oleum Gossypii semen and diethylenetriamine, triethylene tetramine or tetraethylene pentamine 1: 3 in molar ratio～4 adding there-necked flasks, under constantly stirring, be warming up to 110～130 ℃ of reactions 3～4 hours, be evacuated to vacuum tightness subsequently and be-0.1～-0.3MPa, continue to be warming up to 160～180 ℃ of reactions 2～3 hours, be warming up to 210～230 ℃ of reactions once more and reduce to room temperature after 2～3 hours and get the inhibiter precursor;
2) the inhibiter precursor is warming up to 100～120 ℃ and the stirring that constantly refluxes, 25～35% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 200～240 ℃ of reactions 2～4 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Oleum Gossypii semen of the present invention is crude cotton seed oil or cottonseed treated oil.
Utilization of the present invention be cotton the by product Oleum Gossypii semen as the preparation inhibiter raw material, the inhibiter of preparing, excellent property, cost is lower, and in preparation process, adopt vacuum condition, do not use alkane reagent such as dimethylbenzene, so pollution is little in the production process, harm is low.For inhibiter finds a kind of reproducible raw material sources, and have save energy, protection environment, improve the characteristics of cottonseed utilization ratio.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment 1: at first will get mixture in crude cotton seed oil and diethylenetriamine adding in 1: the 3 in molar ratio there-necked flask, under constantly stirring, be warming up to 110 ℃ of reactions 4 hours, being evacuated to vacuum tightness subsequently is-0.2MPa, continue to be warming up to 170 ℃ of reactions 2.5 hours, be warming up to 220 ℃ of reactions once more and reduce to room temperature after 2.5 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 100 ℃ and the stirring that constantly refluxes, 30% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 220 ℃ of reactions 3 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Embodiment 2: at first will get mixture in cottonseed treated oil and triethylene tetramine adding in 1: the 4 in molar ratio there-necked flask, under constantly stirring, be warming up to 120 ℃ of reactions 3.5 hours, being evacuated to vacuum tightness subsequently is-0.15MPa, continue to be warming up to 160 ℃ of reactions 3 hours, be warming up to 230 ℃ of reactions once more and reduce to room temperature after 2 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 110 ℃ and the stirring that constantly refluxes, 35% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 240 ℃ of reactions 2 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Embodiment 3: at first will get mixture in crude cotton seed oil and tetraethylene pentamine adding in 1: the 3.3 in molar ratio there-necked flask, under constantly stirring, be warming up to 130 ℃ of reactions 3 hours, being evacuated to vacuum tightness subsequently is-0.1MPa, continue to be warming up to 180 ℃ of reactions 2 hours, be warming up to 210 ℃ of reactions once more and reduce to room temperature after 3 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 120 ℃ and the stirring that constantly refluxes, 25% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 200 ℃ of reactions 4 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Embodiment 4: at first will get mixture in cottonseed treated oil and diethylenetriamine adding in 1: the 3.5 in molar ratio there-necked flask, under constantly stirring, be warming up to 115 ℃ of reactions 3.8 hours, being evacuated to vacuum tightness subsequently is-0.25MPa, continue to be warming up to 165 ℃ of reactions 2.8 hours, be warming up to 225 ℃ of reactions once more and reduce to room temperature after 2.3 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 105 ℃ and the stirring that constantly refluxes, 32% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 230 ℃ of reactions 2.5 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Embodiment 5: at first will get mixture in cottonseed treated oil and triethylene tetramine adding in 1: the 3.8 in molar ratio there-necked flask, under constantly stirring, be warming up to 125 ℃ of reactions 3.2 hours, being evacuated to vacuum tightness subsequently is-0.3MPa, continue to be warming up to 175 ℃ of reactions 2.2 hours, be warming up to 215 ℃ of reactions once more and reduce to room temperature after 2.8 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 115 ℃ and the stirring that constantly refluxes, 28% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 210 ℃ of reactions 3.5 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
The A20 steel disc in 70 ℃, 4% hydrochloric acid, add the inhibiter that embodiment 1 makes after, the result of corrosion 8h:
| Embodiment 1 consumption (mg/L) | Erosion rate (g/m 2·h) | Corrosion inhibition rate (%) |
| 50 | 2.69 | 91.03 |
| 100 | 1.85 | 93.83 |
| 150 | 1.59 | 94.70 |
| 200 | 1.50 | 95.00 |
The A20 steel disc adds the Corrosion results behind the inhibiter of the different embodiment of 150mg/L in 60 ℃, 4% hydrochloric acid:
| Inhibiter | Etching time (h) | Erosion rate (g/m2h) | Corrosion inhibition rate (%) |
| Embodiment 2 | 6 | 1.07 | 96.18 |
| Embodiment 3 | 12 | 1.49 | 94.68 |
| Embodiment 4 | 16 | 1.80 | 93.61 |
| Embodiment 5 | 24 | 2.10 | 92.53 |
Claims (6)
1. one kind prepares the method for inhibiter with Oleum Gossypii semen, it is characterized in that, may further comprise the steps:
1) at first will get mixture in Oleum Gossypii semen and diethylenetriamine, triethylene tetramine or tetraethylene pentamine 1: 3 in molar ratio～4 adding there-necked flasks, under constantly stirring, be warming up to 110～130 ℃ of reactions 3～4 hours, be evacuated to vacuum tightness subsequently and be-0.1～-0.3MPa, continue to be warming up to 160～180 ℃ of reactions 2～3 hours, be warming up to 210～230 ℃ of reactions once more and reduce to room temperature after 2～3 hours and get the inhibiter precursor; Said Oleum Gossypii semen is crude cotton seed oil or cottonseed treated oil;
2) the inhibiter precursor is warming up to 100～120 ℃ and the stirring that constantly refluxes, 25～35% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 200～240 ℃ of reactions 2～4 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
2. the method for preparing inhibiter with Oleum Gossypii semen according to claim 1, it is characterized in that: at first will get mixture in crude cotton seed oil and diethylenetriamine adding in 1: the 3 in molar ratio there-necked flask, under constantly stirring, be warming up to 110 ℃ of reactions 4 hours, being evacuated to vacuum tightness subsequently is-0.2MPa, continue to be warming up to 170 ℃ of reactions 2.5 hours, be warming up to 220 ℃ of reactions once more and reduce to room temperature after 2.5 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 100 ℃ and the stirring that constantly refluxes, 30% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 220 ℃ of reactions 3 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
3. the method for preparing inhibiter with Oleum Gossypii semen according to claim 1, it is characterized in that: at first will get mixture in cottonseed treated oil and triethylene tetramine adding in 1: the 4 in molar ratio there-necked flask, under constantly stirring, be warming up to 120 ℃ of reactions 3.5 hours, being evacuated to vacuum tightness subsequently is-0.15MPa, continue to be warming up to 160 ℃ of reactions 3 hours, be warming up to 230 ℃ of reactions once more and reduce to room temperature after 2 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 110 ℃ and the stirring that constantly refluxes, 35% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 240 ℃ of reactions 2 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
4. the method for preparing inhibiter with Oleum Gossypii semen according to claim 1, it is characterized in that: at first will get mixture in crude cotton seed oil and tetraethylene pentamine adding in 1: the 3.3 in molar ratio there-necked flask, under constantly stirring, be warming up to 130 ℃ of reactions 3 hours, being evacuated to vacuum tightness subsequently is-0.1MPa, continue to be warming up to 180 ℃ of reactions 2 hours, be warming up to 210 ℃ of reactions once more and reduce to room temperature after 3 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 120 ℃ and the stirring that constantly refluxes, 25% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 200 ℃ of reactions 4 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
5. the method for preparing inhibiter with Oleum Gossypii semen according to claim 1, it is characterized in that: at first will get mixture in cottonseed treated oil and diethylenetriamine adding in 1: the 3.5 in molar ratio there-necked flask, under constantly stirring, be warming up to 115 ℃ of reactions 3.8 hours, being evacuated to vacuum tightness subsequently is-0.25MPa, continue to be warming up to 165 ℃ of reactions 2.8 hours, be warming up to 225 ℃ of reactions once more and reduce to room temperature after 2.3 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 105 ℃ and the stirring that constantly refluxes, 32% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 230 ℃ of reactions 2.5 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
6. the method for preparing inhibiter with Oleum Gossypii semen according to claim 1, it is characterized in that: at first will get mixture in cottonseed treated oil and triethylene tetramine adding in 1: the 3.8 in molar ratio there-necked flask, under constantly stirring, be warming up to 125 ℃ of reactions 3.2 hours, being evacuated to vacuum tightness subsequently is-0.3MPa, continue to be warming up to 175 ℃ of reactions 2.2 hours, be warming up to 215 ℃ of reactions once more and reduce to room temperature after 2.8 hours and get the inhibiter precursor; The inhibiter precursor is warming up to 115 ℃ and the stirring that constantly refluxes, 28% Benzyl Chloride of inhibiter precursor gross weight is slowly joined in the inhibiter precursor, treat to add fully being warming up to 210 ℃ of reactions 3.5 hours, reduce to room temperature and promptly get water-soluble Oleum Gossypii semen inhibiter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102545257A CN101717944B (en) | 2009-12-25 | 2009-12-25 | Method for preparing corrosion inhibitor by utilizing cottonseed oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102545257A CN101717944B (en) | 2009-12-25 | 2009-12-25 | Method for preparing corrosion inhibitor by utilizing cottonseed oil |
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| Publication Number | Publication Date |
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| CN101717944A CN101717944A (en) | 2010-06-02 |
| CN101717944B true CN101717944B (en) | 2011-05-18 |
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| CN2009102545257A Expired - Fee Related CN101717944B (en) | 2009-12-25 | 2009-12-25 | Method for preparing corrosion inhibitor by utilizing cottonseed oil |
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| CN105088253B (en) * | 2015-08-19 | 2019-02-01 | 广东工业大学 | A method of imidazoline inhibitor is prepared using genetically engineered soybean oil |
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Granted publication date: 20110518 Termination date: 20131225 |