CN105220158B - A kind of non-phosphorus system's high-temperature corrosion inhibitor and preparation method thereof - Google Patents
A kind of non-phosphorus system's high-temperature corrosion inhibitor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of non-phosphorus system's high-temperature corrosion inhibitor and preparation method thereof.Non-phosphorus system's high-temperature corrosion inhibitor is made up of 5~60 weight % Thiazoling type sulfide compound, 1~50 weight % organosilane polysulfides compound, 1~30 weight % organic amine compounds and 10~70 weight % solvents, with non-phosphorus system's high-temperature corrosion inhibitor gross weight meter.Non-phosphorus system's high-temperature corrosion inhibitor provided by the invention can be used for oil refining apparatus high-temperature naphthenic acid erosion environment, can significantly inhibit corrosion of the naphthenic acid corrosion medium to hardware and pipeline, while the corrosion inhibiter not phosphorus element-containing, and harm is not produced to following process device.
Description
Technical field
The invention belongs to metal erosion to suppress field, suppresses equipment in Refining Units and pipe more particularly to one kind
Non-phosphorus system's high-temperature corrosion inhibitor of road high-temperature naphthenic acid erosion and preparation method thereof.
Background technology
Crude resources develops towards the direction of in poor quality in world wide at present, increases year by year containing acid, sulfur crude processing amount
Add, crude oil with poor quality processing has turned into the problem of the World Refining enterprise facing.With the continuous increasing containing acid, sulfur crude processing amount
Add, aggravation trend is presented in the corrosion of equipment, and equipment corrosion is a difficulty for perplexing oil refining apparatus safety in production and long-term operation
Topic.Wherein, it is being the safety in production of puzzlement oil refining apparatus and long period containing acid, high-acid crude oil process high temperature naphthenic acid corrosion
One main hidden danger of operation.Slowing down the method for naphthenic acid corrosion at present mainly includes：1. high and low acid number crude oil is mixed acid number
It is reduced to below critical value；2. crude oil removes aphthenic acids in crude oil before entering distilling apparatus；3. upgrade high temperature position equipment and pipe
Road material；4. fill high-temperature corrosion inhibitor in high temperature position.Contrasted in terms of the economy of method and the possibility of application, filling is high
Warm corrosion inhibiter is considered as the processing method that a kind of effect is good, cost is low, simple to operate, be generally used for general corrosion situation or
Supported the use in seriously corroded with local upgrade of material.
High-temperature corrosion inhibitor can be divided into phosphorus system, non-phosphorus system and mixed type according to type of inhibitor.Under normal circumstances, phosphorus system inhibition
Agent is more more effective than non-phosphorus family corrosion inhibitor, but when using phosphorus family corrosion inhibitor, the catalysis that is easily caused in follow-up deep-processing process
Agent is poisoned.Patent USP5252254 discloses a kind of sulfonation nonyl that preparation is reacted by alkyl phenol and sulfur trioxide or oleum
Phenol high-temperature corrosion inhibitor, but inhibiter consumption is big, corrosion mitigating effect is low.USP5630964, USP5863415, USP6583091 and
USP7491318 is respectively organopolysulfides, piperazine, sulfosalicylic phthalate and mercaptan carboxylic acid's esters corrosion inhibiter, is equally existed
Dosage is big and the shortcomings of corrosion mitigating effect difference.Therefore exploitation has the characteristics that the corrosion inhibiter that not phosphorous, dosage is small, inhibition efficiency is high is
Development trend from now on.
The content of the invention
It is used to suppress the non-phosphorus of equipment in Refining Units and pipeline high-temperature naphthenic acid erosion it is an object of the invention to provide a kind of
It is high-temperature corrosion inhibitor and preparation method thereof.The corrosion inhibiter is a kind of film inhibitor, is by a variety of non-phosphorus with corrosion inhibition
Organic compound forms, and reacts to form deposition with the iron of metal surface by mutually acting synergistically, is covered in metal surface, in height
The surface of hardware and pipeline is played a good protection under warm naphthenic acid corrosion environment.
The present invention provides a kind of non-phosphorus system's high-temperature corrosion inhibitor, it is characterised in that the corrosion inhibiter is made up of following components：
With non-phosphorus system's high-temperature corrosion inhibitor gross weight meter.
Wherein, the Thiazoling type sulfide compound is usually to be prepared using thiazolidine thione and two bromo-hydrocarbons as raw material.Its
Shown in general structure such as formula (1)：
R1 is C in formula (1)1~C10Alkyl；
R2 is C2~C15Alkyl, alkylene or aromatic radical.
Thiazoling type sulfide compound preferred content is 10~50 weight %, with corrosion inhibiter gross weight meter.
The organosilane polysulfide compound is usually to be prepared using alkene and sulphur as raw material, its general structure such as formula (2) institute
Show：
R-SX-R’ (2)
R and R ' is C respectively in formula (2)4~C20Alkyl, cycloalkyl or aromatic radical, R and R ' can with it is identical can not also
Together；
The integer of X=1~8.
Organosilane polysulfide compound preferred content is 5~40 weight %, with corrosion inhibiter gross weight meter.
The organic amine compound is containing C6~C12Any one in the monoamine of alkyl, diamines, triamine or two kinds, it is excellent
It is 5~20 weight % to select content, with corrosion inhibiter gross weight meter.
The solvent is C6~C20Any one in aromatic hydrocarbons or two kinds, preferred content is 20~50 weight %, with corrosion inhibiter
Gross weight meter.
The present invention provides a kind of preparation method of non-phosphorus system's high-temperature corrosion inhibitor, it is characterised in that comprises the steps：
(a) preparation method of Thiazoling type sulfide compound：
By alkylthiazolidine thioketones and potassium hydroxide according to 1: 1 mixed in molar ratio, it is total then to add 4~8 times of above-mentioned substance
The absolute ethyl alcohol of weight, is mixed at room temperature.Be slowly added to two bromo-hydrocarbons after well mixed, two bromo-hydrocarbons according to alkyl
The mol ratio of thiazolidine thione 1: 2 to 1: 5 adds.After addition under the conditions of 30~70 DEG C stirring reaction 20~60 hours,
Reaction finishes to be stood into reaction product after addition distilled water, and distilled water adds according to the volume ratio of reaction product 1: 2, stands
There is Precipitation a period of time, then filters, drying to obtain Thiazoling type sulfide compound.
Shown in the structural formula such as formula (3) of wherein described alkylthiazolidine thioketones：
R1 is C in formula (3)1~C10Alkyl.
Two bromo-hydrocarbons is any one in dibromoalkane hydrocarbon, two bromo alkene or two bromo aromatic hydrocarbon.
(b) preparation of corrosion inhibiter：
Thiazoling type sulfide compound, organosilane polysulfide compound, organic amine compound and solvent prepared by step (a)
Proportionally mix and produce non-phosphorus system's high-temperature corrosion inhibitor.
Non-phosphorus system's high-temperature corrosion inhibitor provided by the invention can be used for oil refining apparatus high-temperature naphthenic acid erosion environment, in addition
Under conditions of 10~100 μ g/g, it is coordinated to form firm protection containing the hetero atoms such as S, N and metallic atom Fe in corrosion inhibiter
Film, metal surface is covered in, so as to significantly inhibit corrosion of the naphthenic acid corrosion medium to hardware and pipeline.
High-temperature corrosion inhibitor provided by the invention contains the polar group centered on multiple S, N hetero atoms simultaneously, and these are with miscellaneous
Polar group centered on atom mutually acts synergistically, and enhances the bond strength of high-temperature corrosion inhibitor and metal surface Fe atoms
And stability, substantially increase the inhibition efficiency of corrosion inhibiter.The corrosion inhibiter not phosphorus element-containing simultaneously, is not produced to following process device
Raw harm, it is a kind of efficient high-temperature corrosion inhibitor of low toxicity.
The present invention is described in further detail with reference to embodiment, still, these embodiments are not to use
Come the scope limiting the invention in any way.
Embodiment
Evaluation method
Corrosion inhibiter of the present invention is evaluated using corrosion coupon weight-loss method, specific method is as follows：By 800mL
Technical white oil or distillate containing Oil Containing Naphthenic Acid are added in 1L high-temperature high-pressure reaction kettles, add certain density hair
The bright corrosion inhibiter, then the 20# carbon steels test piece by pretreatment and correct amount is immersed in oil product with special hook,
Corrosion inhibiter benchmark test is carried out under conditions of 260~380 DEG C of experiment, rotating speed 800rpm, 48~96hr of test period.Experiment
Room temperature is cooled to after end, according to being weighed after standard ASTM G1-2003 step process after taking-up test piece, is accurate to 0.0001g.
Blank test operating method is same as above, and does not add any corrosion inhibiter during experiment simply.
The inhibition efficiency η of corrosion inhibiter：
η=(CR0-CR1)/CR0× 100%
CR in formula0The corrosion rate of carbon steel during to add corrosion inhibiter；
CR1For the corrosion rate of carbon steel after addition corrosion inhibiter.
Wherein 1~embodiment of embodiment 5 is the preparation of corrosion inhibiter, and embodiment 6 and 7 is tried for the corrosion inhibition evaluation of corrosion inhibiter
Test.
Embodiment
Embodiment 1
(1) then 5- ethyl -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 4 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to the bromo nonanes of 1,9- bis- after well mixed, 1,9- bis-
Bromo nonane adds according to the mol ratio of alkylthiazolidine thioketones 1: 3.After addition under the conditions of 50 DEG C stirring reaction 48
Hour, stood after then adding the distilled water of the volume of reaction product 1/2, there is suction filtration, drying to obtain thiazoline after Precipitation
Class sulfide compound A.
(2) Thiazoling type sulfide compound A, butyl polysulfides, octodrine and the dimethylbenzene prepared step (1) is molten
Agent mixes according to 35: 20: 10: 35 mass ratioes and produces high-temperature corrosion inhibitor HC01.
Embodiment 2
(1) then 5- octyl group -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 8 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to the bromic ethers of 1,2- bis- after well mixed, 1,2- bis-
Bromic ether adds according to the mol ratio of alkylthiazolidine thioketones 1: 2.After addition under the conditions of 40 DEG C stirring reaction 60
Hour, stood after then adding the distilled water of the volume of reaction product 1/2, there is suction filtration, drying to obtain thiazoline after Precipitation
Class sulfide compound B.
(2) it is the Thiazoling type sulfide compound B for preparing step (1), isoprene polysulfides, di-n-propylamine, just pungent
Amine mixes according to 50: 5: 15: 10: 20 mass ratioes with toluene solvant and produces high-temperature corrosion inhibitor HC02.
Embodiment 3
(1) then 5- butyl -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 5 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to after well mixed to xylylene bromide, to two bromomethyls
Benzene adds according to the mol ratio of alkylthiazolidine thioketones 1: 5.After addition under the conditions of 70 DEG C stirring reaction 24 hours, so
Stood after adding the distilled water of the volume of reaction product 1/2 afterwards, there is suction filtration, drying to obtain Thiazoling type thioetherification after Precipitation
Compound C.
(2) Thiazoling type sulfide compound C, cetyl polysulfides, n-dodecylamine and the benzene for preparing step (1)
Solvent mixes according to 15: 40: 5: 40 mass ratioes and produces high-temperature corrosion inhibitor HC03.
Embodiment 4
(1) then 5- methyl -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 5 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to the bromododecanes of 1,12- bis- after well mixed, 1,
The bromododecanes of 12- bis- add according to the mol ratio of alkylthiazolidine thioketones 1: 4.Stirred after addition under the conditions of 50 DEG C
Reaction 48 hours, stood after then adding the distilled water of the volume of reaction product 1/2, there is suction filtration, drying to obtain after Precipitation
Thiazoling type sulfide compound D.
(2) Thiazoling type sulfide compound D, cyclohexyl polysulfides, two n-hexylamines and the toluene for preparing step (1)
Solvent mixes according to 30: 20: 5: 45 mass ratioes and produces high-temperature corrosion inhibitor HC04.
Embodiment 5
(1) then 5- hexyl -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 6 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to the bromo hexanes of 1,6- bis- after well mixed, 1,6- bis-
Bromo hexane adds according to the mol ratio of alkylthiazolidine thioketones 1: 3.After addition under the conditions of 50 DEG C stirring reaction 40
Hour, stood after then adding the distilled water of the volume of reaction product 1/2, there is suction filtration, drying to obtain thiazoline after Precipitation
Class sulfide compound E.
(2) by the Thiazoling type sulfide compound E of step (1) preparation, styryl polysulfides, di-n-butylamine, three
Ethamine mixes according to 40: 15: 5: 5: 35 mass ratioes with xylene solvent and produces high-temperature corrosion inhibitor HC05.
Embodiment 6
(1) then 5- decyl -2- thiazolidine thiones and potassium hydroxide are added into above-mentioned substance 5 according to 1: 1 mixed in molar ratio
The absolute ethyl alcohol of times gross weight, is mixed at room temperature.It is slowly added to bromo -2- the butylene of Isosorbide-5-Nitrae-two after well mixed, Isosorbide-5-Nitrae -
Two bromo -2- butylene add according to the mol ratio of alkylthiazolidine thioketones 1: 4.Stirred instead under the conditions of 60 DEG C after addition
Answer 50 hours, stood after then adding the distilled water of the volume of reaction product 1/2, there is suction filtration, drying to obtain thiophene after Precipitation
Oxazolines sulfide compound F.
(2) it is the Thiazoling type sulfide compound F for preparing step (1), myrcenyl polysulfides, tripropyl amine (TPA), different pungent
Amine mixes according to 60: 5: 5: 2: 28 mass ratioes with xylene solvent and produces high-temperature corrosion inhibitor HC06.
Embodiment 7
Technical white oil and the acid number of commercial naphthenic acid allotment is used to be situated between for 15mgKOH/g high acid value oil product as corrosion
Matter, evaluation embodiment 1 arrive the performance of 6 six kinds of corrosion inhibiter of embodiment.Test temperature is 280 DEG C, and the test period is 72 hours, rotating speed
For 800rpm, result of the test is shown in Table 1.
The evaluation result of 1 different corrosion inhibiter of table
As it can be seen from table 16 kinds of corrosion inhibiter have good corrosion mitigating effect to high-temperature naphthenic acid erosion, its corrosion inhibiter is all
More than 92%；When the addition of corrosion inhibiter is 40 μ g/g, its corrosion inhibition rate is more than 94%.
Embodiment 8
Corrosive medium is same as Example 7, inhibition effects of the evaluation corrosion inhibiter HC01 and HC03 in the range of 250~340 DEG C
Fruit, test period are 48 hours, and corrosion inhibiter addition is 100 μ g/g, rotating speed 800rpm, and result of the test is shown in Table 2.
The corrosion inhibition of corrosion inhibiter under the different temperatures of table 2
As known from Table 2, the corrosion of high-temperature naphthenic acid is raised and increased with temperature in the range of 250~340 DEG C, adds high temperature
After corrosion inhibiter, although corrosion rate is increased slightly with temperature, amplitude of variation is smaller, corrosion rate all in below 0.12mm/y,
Corrosion inhibition rate is all more than 98%.Result of the test shows, in the serious temperature range of high-temperature naphthenic acid erosion (280~340 DEG C),
High-temperature corrosion inhibitor provided by the invention has good corrosion mitigating effect.
Claims (5)
1. a kind of non-phosphorus system's high-temperature corrosion inhibitor, it is characterised in that the corrosion inhibiter is made up of following components：
With non-phosphorus system's high-temperature corrosion inhibitor gross weight meter；
Wherein, shown in the general structure such as formula (1) of the Thiazoling type sulfide compound：
R1 is C in formula (1)1~C10Alkyl；R2 is C2~C15Alkyl, alkylene or aromatic radical；
Shown in the general structure such as formula (2) of the organosilane polysulfide compound：
R-SX-R’ (2)
R and R ' is C respectively in formula (2)4~C20Alkyl, cycloalkyl or aromatic radical；X is 1~8 integer.
2. non-phosphorus system's high-temperature corrosion inhibitor according to claim 1, it is characterised in that：The organic amine compound be containing
C6~C12Any one in the monoamine of alkyl, diamines, triamine or two kinds.
3. non-phosphorus system's high-temperature corrosion inhibitor according to claim 1, it is characterised in that：The solvent is C6~C20Appoint in aromatic hydrocarbons
Meaning is one or two kinds of.
4. non-phosphorus system's high-temperature corrosion inhibitor according to claim 1, it is characterised in that：The Thiazoling type sulfide compound
Content is 10~50 weight %, and the content of organosilane polysulfide compound is 5~40 weight %, and the content of organic amine compound is 5
~20 weight %, the content of solvent is 20~50 weight %, with corrosion inhibiter gross weight meter.
5. the preparation method of non-phosphorus system's high-temperature corrosion inhibitor described in a kind of claim 1, it is characterised in that comprise the steps：
(a) preparation method of Thiazoling type sulfide compound：
By alkylthiazolidine thioketones and potassium hydroxide according to 1: 1 mixed in molar ratio, 4~8 times of gross weights of above-mentioned substance are then added
Absolute ethyl alcohol, mix at room temperature, be slowly added to two bromo-hydrocarbons after well mixed, two bromo-hydrocarbons according to alkyl thiazole
The mol ratio of alkane thioketones 1: 2 to 1: 5 adds, stirring reaction 20~60 hours, reaction under the conditions of 30~70 DEG C after addition
Finish and stood after adding distilled water into reaction product, distilled water adds according to the volume ratio of reaction product 1: 2, stands one section
There is Precipitation time, then filters, drying to obtain Thiazoling type sulfide compound；Wherein two bromo-hydrocarbons are dibromoalkane
Any one in hydrocarbon, two bromo alkene or two bromo aromatic hydrocarbon, shown in the general structure such as formula (3) of alkylthiazolidine thioketones：
R1 is C in formula (3)1~C10Alkyl；
(b) preparation of corrosion inhibiter：
By Thiazoling type sulfide compound prepared by step (a) and the organosilane polysulfide compound described in claim 1, organic amine
Compound and solvent, which proportionally mix, produces non-phosphorus system's high-temperature corrosion inhibitor.
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| CN107829096A (en) * | 2017-10-10 | 2018-03-23 | 威海翔泽新材料科技有限公司 | A kind of plated film corrosion inhibiter and its preparation for refinery device |
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