CN107574447B - Phosphoric acid restrainer and preparation method thereof - Google Patents
Phosphoric acid restrainer and preparation method thereof Download PDFInfo
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- CN107574447B CN107574447B CN201710679778.3A CN201710679778A CN107574447B CN 107574447 B CN107574447 B CN 107574447B CN 201710679778 A CN201710679778 A CN 201710679778A CN 107574447 B CN107574447 B CN 107574447B
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- ammonium salt
- quaternary ammonium
- phosphoric acid
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Abstract
The present invention provides a kind of phosphoric acid restrainer and preparation method thereof, phosphoric acid restrainer includes the component of following parts by weight: 2-15 parts of imidazoline quaternary ammonium salt, 2-10 parts of methyl phenylpropyl triazole Mannich base quaternary ammonium salt, 0-5 parts of surfactant, 70-96 parts of solvent；The imidazoline quaternary ammonium salt is the mixture of tung oil imidazoline quaternary ammonium salt and rosin imidazoline quaternary ammonium salt.Inventing the phosphoric acid restrainer provided can be during phosphoric acid carries out pickling to metallic matrix, a degree of inhibition Fe3+Corrosion to metallic matrix.
Description
Technical field
The present invention relates to pickling inhibiter technologies more particularly to a kind of phosphoric acid restrainer and preparation method thereof, belong to
In technical field of metal anti-corrosion.
Background technique
Acid pickling and rust removing, the method to descale are the methods that industrial circle is most widely used.It is molten to oxide using acid
The mechanical stripping effect that solution and corrosion generate hydrogen achievees the purpose that derust and descale.Using most commonly seen in pickling
It is hydrochloric acid, sulfuric acid, phosphoric acid, and since phosphoric acid will not generate corrosive, relatively safety in pickling.But in phosphorus
In sour acid cleaning process, acid solution has a large amount of Fe while removing oxidation on metal surface object3+And Fe2+Into acid solution, Fe2+With sky
Gas contacts Fe easily generated3+, Fe3+Presence can seriously aggravate the corrosion of metallic matrix, and most of conventional resistance to Fe of corrosion inhibiter3+It is rotten
Erosion is weaker, is there is a large amount of Fe3+In the presence of, corrosion mitigating effect is not achieved in corrosion inhibiter corrosion inhibition dramatic decrease.Therefore, it develops new
Resistance to Fe3+The phosphoric acid restrainer of corrosion has important practical value.
Summary of the invention
In view of the foregoing drawbacks, the present invention provides a kind of phosphoric acid restrainer and preparation method thereof, which can be
During phosphoric acid carries out pickling to metallic matrix, a degree of inhibition Fe3+Corrosion to metallic matrix.
The present invention provides a kind of phosphoric acid restrainer, the component including following parts by weight: 2-15 parts of imidazoline quaternary ammonium salt,
2-10 parts of methyl phenylpropyl triazole Mannich base quaternary ammonium salt, 0-5 parts of surfactant, 70-96 parts of solvent；Wherein, the imidazoles
Hyamine is the mixture of tung oil imidazoline quaternary ammonium salt and rosin imidazoline quaternary ammonium salt, the tung oil imidazoline quaternary ammonium salt such as formula
(1) shown in, shown in the rosin imidazoline quaternary ammonium salt such as formula (2), the methyl phenylpropyl triazole Mannich base quaternary ammonium salt such as formula
(3) shown in,
In above-mentioned phosphoric acid restrainer, imidazoline quaternary ammonium salt and methyl phenylpropyl triazole Mannich base quaternary ammonium salt are phosphorus
The effective component of sour restrainer.
In a specific embodiment of the invention, the imidazoline quaternary ammonium salt is prepared in accordance with the following steps:
1) under stirring, tung oil is mixed with water with molar ratio for 10:1, after 100 DEG C of heat preservation 1h, rosin, diformazan is added
Benzene is warming up to 140 DEG C, generates the first mixture；Wherein the molar ratio of the rosin, dimethylbenzene and tung oil is 3:(10-15): 1；
2) under nitrogen atmosphere protection, diethylenetriamine is added dropwise in the first mixture of Xiang Suoshu, in 140-150 DEG C of reaction 3h
Afterwards, 180 DEG C of reaction 2h are warming up to, are then warming up to 210 DEG C of reaction 5h again, generate intermediary；Wherein, the rosin and divinyl
The molar ratio of triamine is 1:(2.4-3.2)；
3) 90 DEG C are cooled to, benzyl chloride is added in Xiang Suoshu intermediary, reacts 4h, obtains the imidazoline quaternary ammonium salt；Wherein,
The molar ratio of the rosin and benzyl chloride is 1:(1.0-1.5).
It is worth noting that, above-mentioned imidazoline quaternary ammonium salt preparation method of the invention can divide in the same reaction system
Not Zhi get tung oil imidazoline quaternary ammonium salt and rosin imidazoline quaternary ammonium salt, the two react while being independent of each other, thus directly
Obtain imidazoline quaternary ammonium salt of the invention.When specific preparation, it can be carried out using stainless steel cauldron.
Wherein, the reaction equation of tung oil imidazoline quaternary ammonium salt is as follows:
Wherein, the reaction equation of rosin imidazoline quaternary ammonium salt is as follows:
In a specific embodiment of the invention, the methyl phenylpropyl triazole Mannich base quaternary ammonium salt is according to following step
Rapid preparation:
Under stirring, methyl phenylpropyl triazole is mixed with dimethylamine with molar ratio for 1:1, after adjusting pH value to 3-5, is added
Formalin is warming up to 60 DEG C of reaction 6h, benzyl chloride is then added, the reaction was continued after being warming up to 90 DEG C 4h, obtains the base benzene
Third triazole Mannich base quaternary ammonium salt；
Wherein, the methyl phenylpropyl triazole and the molar ratio of formaldehyde are 1:(1.3-1.6), the base phenylpropyl triazole with
The molar ratio of benzyl chloride is 1:(0.6-0.85).When specific preparation, it can be carried out using stainless steel cauldron.
The reaction equation of methyl phenylpropyl triazole Mannich base quaternary ammonium salt is as follows:
In a specific embodiment of the invention, in step 2), a length of 2h when the dropwise addition of the diethylenetriamine is controlled
Within.
In a specific embodiment of the invention, pH value is adjusted to 3- using the aqueous hydrochloric acid solution that mass concentration is 30%
5。
In a specific embodiment of the invention, the mass content of formaldehyde is 40% in the formalin.
In a specific embodiment of the invention, the surfactant is Tween-20 or OP-10.
In a specific embodiment of the invention, the solvent is dimethylformamide or dimethylformamide and two
The mixture of methyl sulfoxide.That is, the mixture of solvent selection dimethylformamide or dimethylformamide and dimethyl sulfoxide.
The present invention also provides a kind of preparation methods of any of the above-described phosphoric acid restrainer, by the imidazoline season
Ammonium salt, methyl phenylpropyl triazole Mannich base quaternary ammonium salt, surfactant, solvent mixing, are made the phosphoric acid restrainer.
Preparation method of the invention is simple to operation, assists without large scale equipment.
Phosphoric acid restrainer of the invention is containing Fe3+In 15% phosphoric acid solution of concentration≤10000mg/L, at 50 DEG C
3g/m is respectively less than to the corrosion rate of A3 steel2.h, A3 steel has been well solved containing Fe3+Etching problem in phosphoric acid solution.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this
Technical solution in inventive embodiments is clearly and completely described, it is clear that described embodiment is that a part of the invention is real
Example is applied, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creation
Property labour under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
The preparation of imidazoline quaternary ammonium salt
Tung oil 29.8g, water 0.6g are warming up to 100 DEG C of heat preservation 1h after mixing, rosin 33.7g, 80g dimethylbenzene, heating is added
To 140 DEG C, it is gradually added into 33g diethylenetriamine, is heated to 150 DEG C of reaction 3h, 180 DEG C of reaction 2h is heated to, is heated to 210 DEG C
5h is reacted, 90 DEG C of addition 27.6g benzyl chlorides are cooled to, reacts 4h to get imidazoline quaternary ammonium salt is arrived.
Embodiment 2
The preparation of methyl benzotriazazole Mannich base quaternary ammonium salt
Methyl phenylpropyl triazole 22.6g, dimethylamine (33% mass concentration) 27.7g, being gradually added into hydrochloric acid, (30% mass is dense
Degree) pH value is adjusted to 15g formalin (40% mass concentration) between 3-5, is then slowly added into, it is small to be heated to 60 DEG C of reactions 6
When, 20.2g benzyl chloride is then added, is warming up to 90 DEG C of reactions 4 hours to get methyl benzotriazazole Mannich base quaternary ammonium is arrived
Salt.
Embodiment 3
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 8kg imidazoline quaternary ammonium salt, 2kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 50kg dimethyl formyl
Amine, 37kg dimethyl sulfoxide and 3kg Tween-20 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 0ppm, carries out corrosion inhibition test using static steel weight-loss method,
Length of testing speech is 2h, and through detecting, at 50 DEG C, the corrosion rate of A3 steel is 0.41g/m2.h。
Embodiment 4
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 7kg imidazoline quaternary ammonium salt, 3kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 40kg dimethyl formyl
Amine, 48kg dimethyl sulfoxide and 2kg OP-10 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 0mg/L, carries out corrosion inhibition test using static steel weight-loss method,
Length of testing speech is 2h, and through detecting, at 50 DEG C, the corrosion rate of A3 steel is 0.35g/m2.h。
Embodiment 5
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 6kg imidazoline quaternary ammonium salt, 4kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 36kg dimethyl formyl
Amine, 46kg dimethyl sulfoxide and 4kg Tween-20 are mixed and made into the corrosion inhibiter containing 14kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 0mg/L, carries out corrosion inhibition test using static steel weight-loss method,
Length of testing speech is 2h, and through detecting, the corrosion rate of A3 steel is 0.26g/m at 50 DEG C2.h。
Embodiment 6
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 8kg imidazoline quaternary ammonium salt, 2kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 90kg dimethyl formyl
Amine is mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 500mg/L, carries out corrosion inhibition survey using static steel weight-loss method
Examination, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 0.93g/m at 50 DEG C2.h。
Embodiment 7
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 8kg imidazoline quaternary ammonium salt, 2kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 50kg dimethyl formyl
Amine, 37kg dimethyl sulfoxide and 3kg OP-10 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 1000mg/L, carries out corrosion inhibition survey using static steel weight-loss method
Examination, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 1.37g/m at 50 DEG C2.h。
Embodiment 8
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 5kg imidazoline quaternary ammonium salt, 5kg methyl benzotriazazole season Mannich base quaternary ammonium salt, with 30kg dimethyl methyl
Amide, 55kg dimethyl sulfoxide and 5kg Tween-20 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 5000mg/L, carries out corrosion inhibition survey using static steel weight-loss method
Examination, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 1.15g/m at 50 DEG C2.h。
Embodiment 9
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 2kg imidazoline quaternary ammonium salt, 8kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 30kg dimethyl formyl
Amine, 55kg dimethyl sulfoxide and 5kg Tween-20 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 5000mg/L, carries out corrosion inhibition survey using static steel weight-loss method
Examination, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 1.68g/m at 50 DEG C2.h。
Embodiment 10
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 6kg imidazoline quaternary ammonium salt, 4kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 40kg dimethyl formyl
Amine, 46kg dimethyl sulfoxide and 4kg OP-10 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 5000mg/L, carries out corrosion inhibition survey using static steel weight-loss method
Examination, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 1.02g/m at 50 DEG C2.h。
Embodiment 11
Ratio according to the invention weighs suitable tung oil, water, dimethylbenzene, rosin, diethylenetriamine and benzyl chloride, presses
According to the facts apply 1 preparation method preparation 10kg imidazoline quaternary ammonium salt.
Ratio according to the invention weighs suitable methyl phenylpropyl triazole, dimethylamine, formaldehyde and benzyl chloride, according to reality
Apply 2 preparation method preparation 10kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt.
Weigh 6kg imidazoline quaternary ammonium salt, 4kg methyl phenylpropyl triazole Mannich base quaternary ammonium salt, with 45kg dimethyl formyl
Amine, 42 dimethyl sulfoxides and 3kg Tween-20 are mixed and made into the corrosion inhibiter containing 10kg effective component.
Above-mentioned corrosion inhibiter is configured as the corrosion inhibiter aqueous solution that corrosion inhibiter additive amount is 0.5%, it is 15% that concentration, which is added,
Phosphoric acid solution in, the Fe in the phosphoric acid solution3+Content is 10000mg/L, carries out corrosion inhibition using static steel weight-loss method
Test, length of testing speech 2h, through detecting, the corrosion rate of A3 steel is 2.07g/m at 50 DEG C2.h。
From the testing result of above-described embodiment: phosphoric acid restrainer of the invention is containing Fe3+Concentration≤
In 15% phosphoric acid solution of 10000mg/L, 3g/m is respectively less than to the corrosion rate of A3 steel at 50 DEG C2.h, it well solves
A3 steel is containing Fe3+Etching problem in phosphoric acid solution.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (6)
1. a kind of phosphoric acid restrainer, which is characterized in that the component including following parts by weight: 2-15 parts of imidazoline quaternary ammonium salt,
2-10 parts of methyl phenylpropyl triazole Mannich base quaternary ammonium salt, 0-5 parts of surfactant and not be 0,70-96 parts of solvent；
Wherein, the imidazoline quaternary ammonium salt is the mixture of tung oil imidazoline quaternary ammonium salt and rosin imidazoline quaternary ammonium salt, the paulownia
Shown in oily imidazoline quaternary ammonium salt such as formula (1), shown in the rosin imidazoline quaternary ammonium salt such as formula (2), the methyl phenylpropyl triazole
Shown in Mannich base quaternary ammonium salt such as formula (3),
The surfactant be Tween-20 perhaps the OP-10 solvent be dimethylformamide or dimethylformamide and
The mixture of dimethyl sulfoxide；
The methyl phenylpropyl triazole Mannich base quaternary ammonium salt is prepared in accordance with the following steps:
Under stirring, methyl phenylpropyl triazole is mixed with dimethylamine with molar ratio for 1:1, after adjusting pH value to 3-5, formaldehyde is added
Solution is warming up to 60 DEG C of reaction 6h, benzyl chloride is then added, the reaction was continued after being warming up to 90 DEG C 4h, obtains the methylbenzene third
Triazole Mannich base quaternary ammonium salt；
Wherein, the methyl phenylpropyl triazole and the molar ratio of formaldehyde are 1:(1.3-1.6), the methyl phenylpropyl triazole and chlorine
The molar ratio for changing benzyl is 1:(0.6-0.85).
2. phosphoric acid restrainer according to claim 1, which is characterized in that the imidazoline quaternary ammonium salt is according to following step
Rapid preparation:
1) under stirring, tung oil is mixed with water with molar ratio for 10:1, after 100 DEG C of heat preservation 1h, rosin, dimethylbenzene is added, rises
Temperature generates the first mixture to 140 DEG C；Wherein the molar ratio of the rosin, dimethylbenzene and tung oil is 3:(10-15): 1；
2) under nitrogen atmosphere protection, diethylenetriamine is added dropwise in the first mixture of Xiang Suoshu, after 140-150 DEG C of reaction 3h,
180 DEG C of reaction 2h are warming up to, are then warming up to 210 DEG C of reaction 5h again, generate intermediary；Wherein, the rosin and divinyl three
The molar ratio of amine is 1:(2.4-3.2)；
3) 90 DEG C are cooled to, benzyl chloride is added in Xiang Suoshu intermediary, reacts 4h, obtains the imidazoline quaternary ammonium salt；Wherein, described
The molar ratio of rosin and benzyl chloride is 1:(1.0-1.5).
3. phosphoric acid restrainer according to claim 2, which is characterized in that in step 2), control the divinyl three
When the dropwise addition of amine within a length of 2h.
4. phosphoric acid restrainer according to claim 1, which is characterized in that the hydrochloric acid water for being 30% using mass concentration
Solution adjusts pH value to 3-5.
5. phosphoric acid restrainer according to claim 4, which is characterized in that the quality of formaldehyde contains in the formalin
Amount is 40%.
6. the preparation method of any phosphoric acid restrainer of claim 1-5, which is characterized in that by the imidazoline season
Ammonium salt, methyl phenylpropyl triazole Mannich base quaternary ammonium salt, surfactant, solvent mixing, are made the phosphoric acid restrainer.
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