CN102912366A - Ferrous sulfide passivation cleaning agent and preparation method and application thereof - Google Patents
Ferrous sulfide passivation cleaning agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a ferrous sulfide passivation cleaning agent which comprises sodium bicarbonate, sodium hypochlorite, ethylene diamine tetraacetic acid-tetrasodium (EDTA-tetrasodium), potassium ferrate, surfactant and water. The passivation cleaning agent provided by the invention is safe, efficient, environment-friendly and low in price and can absorb harmful gases; the component potassium ferrate is bactericidal and environment-friendly and is a novel efficient multifunctional passivation treating agent integrating oxidation, adsorption, flocculation, coagulant aid, sterilization, insect killing and deodorization; and the component potassium ferrate has the advantages of good sterilization effect, little dosage, fast effect, multiple functions, high safety and the like, and is convenient to use and widely applicable.
Description
Technical field
The invention belongs to the petrochemical technology field, particularly a kind of ferrous sulfide deactivation cleaning agent that prevents Iron sulfuret spontaneous combustion in the petrochemical equipment.
Background technology
Iron sulfuret spontaneous combustion in the petrochemical equipment (especially refining device) mainly occurs in the maintenance process, when equipment is opened in maintenance, the Iron sulfuret dirt that is attached to equipment surface contacts with air, and Iron sulfuret and airborne oxygen generation chemical reaction produce spontaneous combustion.The industrial method of Iron sulfuret spontaneous combustion that prevents has three kinds at present:
1. isolation method: prevent that namely Iron sulfuret from contacting with airborne oxygen, as use nitrogen protection, water seal protection etc.;
2. washing out method: will remove on the Iron sulfuret slave unit, as equipment is carried out mechanical cleaning, matting etc.;
3. deactivation method: carry out device processes with passivator, the Iron sulfuret of easy spontaneous combustion is converted into more stable compound, thereby prevents the spontaneous combustion of Iron sulfuret.
Isolation method is applicable to online protection, but is difficult to effectively prevent the spontaneous combustion of Iron sulfuret in maintenance process.The cost of deactivation method is higher, and can not will remove on the Iron sulfuret slave unit.Washing out method comprises physical cleaning and matting, and physical cleaning mainly is to utilize special machine cleaning equipment surface dirt layer; Matting has alkali cleaning, pickling, organic solvent to clean, and the cleaning of the tensio-active agent that adopts according to the difference of fouling kind and the mixed chemical cleaning solution of the compositions such as alkali, organic solvent.Comparatively speaking, washing out method is simple and effective, and cost is low, is the method for relatively commonly using.
The matting of the petrochemical equipment that extensively adopts at present is actually traditional washing out method and deactivation method and combines, and namely suitably adds the composition of passivator in chemical again.The main passivation clean-out system that uses mainly contains potassium permanganate, dioxide peroxide, acid, alkaline hydrogen oxygenant.Although these passivation clean-out systems have satisfied petroleum chemical enterprise's safety in production requirement at the elimination Iron sulfuret.But use potassium permanganate in the passivation scavenging solution, to contain a large amount of mn ions, easily cause secondary pollution; Dioxide peroxide has corrosion to equipment, especially stainless steel is easily produced spot corrosion; Pickling comparatively will weigh the corrosion of equipment, reduces corrosion although add inhibiter, and the waste liquid after cleaning still need solve; Clorox easily produces objectionable impurities.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of new passivation clean-out system, its advantage is for can wash fast and effectively petrochemical equipment, especially the Iron sulfuret that adheres in the refining device, the generation of unharmful substance, can absorb simultaneously the toxic and harmfuls such as the hydrogen sulfide that produces in the petrochemical equipment, yperite, the passivation clean-out system of a kind of efficient, safety, environmental protection, cheapness, deodorizing, also have simultaneously save time, the effect of dart.
For solving the problems of the technologies described above, the invention provides a kind of ferrous sulfide deactivation cleaning agent, it comprises sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), potassium ferrate, tensio-active agent and water.
Wherein, the weight percent of each component is in the described passivation clean-out system: 0.1～5% sodium bicarbonate, 0.1～10% potassium ferrate, 1～10% clorox, 0.1～5% tetrasodium ethylenediamine tetraacetate, 0.1～5% tensio-active agent and the water of surplus.
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene (OP-10), the fatty alcohol-polyoxyethylene ether.
The present invention also provides the preparation method of above-mentioned ferrous sulfide deactivation cleaning agent, comprising:
The first step is got part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in proportion in the solution that the first step obtains, continue to add water to needed amount, regulate the pH value between 10～11, continue to stir, obtain described passivation clean-out system.
The present invention also provides the application of above-mentioned ferrous sulfide deactivation cleaning agent in the petrochemical unit cleaning process.
The technique effect that the present invention is useful is:
Passivation clean-out system provided by the present invention has safety, efficient, environmental protection, cheap, and can absorb the advantage of toxic and harmful, the potassium ferrate component that has not only can be sterilized, and environmentally friendly, be a kind ofly integrate oxidation, absorption, flocculate, help solidifying, sterilization, the new and effective multi-functional passivation treating agent of desinsection, deodorizing, this potassium ferrate component has that sterilization effect is good, consumption is few, effect fast, functional many, security good, easy to use, the plurality of advantages such as be widely used.
Embodiment
The invention provides a kind of ferrous sulfide deactivation cleaning agent, it comprises sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), potassium ferrate, tensio-active agent and water.
Further, described ferrous sulfide deactivation cleaning agent only is made of said components.
Wherein, the weight percent of each component is in the described passivation clean-out system: 0.1～5% sodium bicarbonate, 0.1～10% potassium ferrate, 1～10% clorox, 0.1～5% tetrasodium ethylenediamine tetraacetate, 0.1～5% tensio-active agent and the water of surplus.
Used potassium ferrate as passivator in the ferrous sulfide deactivation cleaning agent provided by the present invention, potassium ferrate not only can be sterilized, and environmentally friendly, be a kind ofly integrate oxidation, absorption, flocculate, help solidifying, sterilization, the new and effective multifunctional green water conditioner of desinsection, deodorizing.Its advantage is as follows:
1, described potassium ferrate has very strong oxidation capacity, can multiple inorganic, the organic substance of oxidation, and such as NH
3, S
2O
4 2-, SCN-, H
2Compounds such as S, alcohol, acid, amine, hydroxyl ketone, quinhydrones, phenylhydrazone, oxime, and can not cause any damage to human and environment, be a kind of ideal, efficiently, the strong oxidizer of highly selective;
2, the ferric acid radical ion can also kill intestinal bacteria and general bacterium in the aqueous solution, can be except harmful organic substance, the NO in the decontaminated water
2-And hypertoxic CN
-, yperite etc.; The ferric acid radical ion decomposes generation Fe (OH) in addition
3Can be used as sorbent material, adsorb various zwitterions, has the sewage purification effect, the various water purification agents that ratio uses in the market such as alum, polymerize aluminum chloride, ferric sulfate etc. all have superiority, simultaneously, potassium ferrate has absorption, flocculating function, decolouring, deodorizing, effectively reduces biological oxygen demand (BOD) (BOD), chemical oxygen demand (COD) value of water body.
3, compare the secondary pollution of potassium ferrate heavy metal free with general oxygenant Manganse Dioxide, potassium permanganate, chromium trichloride, the potassium bichromate in environmental protection aspect.Compare with chlorinated product, potassium ferrate does not produce methylene dichloride, trichloromethane compound without " three cause " effect, does not produce the chlorinated phenols of peculiar smell yet.
4, described potassium ferrate have that sterilization effect is good, consumption is few, effect fast, functional many, security good, easy to use, the plurality of advantages such as be widely used.
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene (OP-10), the fatty alcohol-polyoxyethylene ether.
In described passivation clean-out system, when the ferrous sulfide scale in the required equipment to be processed is more, can improve the content of potassium ferrate, thoroughly make the ferrous sulfide deactivation inactivation, the weight percent of described potassium ferrate in described passivation clean-out system is 0.1～10%, if but less than 0.1%, then can not make the complete passivation of Iron sulfuret in the petrochemical equipment, passivation effect is bad, if weight percent surpasses 10%, very easily form reddish-brown precipitation, be attached to cleaning equipment and make.
In described passivation clean-out system, according to residual what of greasy dirt, the content of increase tensio-active agent that can be suitable improves the device cleaning performance, and the weight percent of described tensio-active agent in described passivation clean-out system is 0.1～5%, but, if less than 0.1%, then can't remove the greasy dirt in the petrochemical equipment that cleans, if concentration is excessive above 5%, make the part surface bioactive molecule can't touch water, cause the waste of tensio-active agent.
If salt concn or heavy metal ion is more in the described petrochemical equipment, can improve the usage quantity of tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), the weight percent of described tetrasodium ethylenediamine tetraacetate in described passivation clean-out system is 0.1～5%, if less than 0.1%, then can't well take out salt or heavy metal ion in the described petrochemical equipment, and increase tetrasodium ethylenediamine tetraacetate (EDTA-four sodium) content more can be efficiently, salt or the heavy metal ion in the complexing petrochemical equipment fast.
Sodium bicarbonate Main Function in the described Cleaning and Passivation agent composition is to absorb obnoxious flavour in the petrochemical complex production unit and the PH of regulator solution, the weight percent of described sodium bicarbonate in described Cleaning and Passivation agent is 0.1～5%, if concentration is crossed the low or too high requirement that all can not satisfy the passivation clean-out system, also fall flat.
Clorox Main Function in the described Cleaning and Passivation agent is and potassium ferrate synergistic oxidation Iron sulfuret.The weight percent of described clorox in described Cleaning and Passivation agent is 1～10%, will not have oxygenizement if weight percent is lower than 1%, if weight percent surpasses 10%, oxidation effectiveness strengthens, but will increase the weight of the corrosion of equipment, causes vicious cycle.
The present invention also provides a kind of ferrous sulfide deactivation cleaning agent, and it comprises sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), potassium ferrate, tensio-active agent and water;
The weight percent of each component is in the described passivation clean-out system: 0.1～5% sodium bicarbonate, 0.1～10% potassium ferrate, 1～10% clorox, 0.1～5% tetrasodium ethylenediamine tetraacetate, 0.1～5% tensio-active agent and the water of surplus;
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene (OP-10), the fatty alcohol-polyoxyethylene ether.
The present invention also provides the preparation method of above-mentioned ferrous sulfide deactivation cleaning agent, comprising:
The first step is got part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in proportion in the solution that the first step obtains, continue to add water to needed amount, regulate the pH value between 10～11, continue to stir, obtain described passivation clean-out system.
The present invention also provides the application of above-mentioned ferrous sulfide deactivation cleaning agent in the petrochemical unit cleaning process.
Describe embodiments of the present invention in detail below with reference to embodiment, how the utilisation technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implements according to this.
The preparation of embodiment 1 passivation clean-out system
Take by weighing 15g Sodium dodecylbenzene sulfonate, 10g sodium lauryl sulphate, 5g alkylphenol polyoxyethylene (OP-10), 8g fatty alcohol-polyoxyethylene ether as tensio-active agent, add in the 800g water, stir, dissolve, leave standstill.Then in mentioned solution, add 10g potassium ferrate, 50g clorox, 5g ethylenediamine tetraacetic acid (EDTA)-four sodium (EDTA-four sodium), 10g sodium bicarbonate, stirring and dissolving adds water to 1000g, and making its pH value is 10, and the continuation stirring makes the solute dissolving, acquisition passivation clean-out system.
Embodiment 2 passivation clean-out systems clean the Iron sulfuret experiment relatively
Utilize the reaction of chance water to emit gas reactor and carry out the cleaning performance contrast verification to cleaning forward and backward Iron sulfuret residue.
Embodiment
Get the passivation clean-out system 100g of embodiment 1 preparation, take by weighing 1.0g Iron sulfuret powder, place 50 ℃ of waters bath with thermostatic control, react take vibrational frequency as 150r/min.
Comparative example
The Iron sulfuret of quality such as choose, 100g water replaces the passivation scavenging solution to carry out cleaning reaction with synthermal, same frequency, equal time.
Embodiment and comparative example result are relatively
To and utilize the residue after the passivator scavenging solution cleans to filter with the tap water scavenging solution, again residue is cleaned 2-3 time with clear water, pack into behind the vacuum drying and meet in the water reactor, utilize control software set test procedure, 5% the hydrochloric acid of packing in testing tube reacts, start testing software, opening switch makes in the disposable inflow reactor of hydrochloric acid, calculate according to rate of gas release and to emit gas content, find that the gas volume that adopts passivation clean-out system chance hydrochloric acid reaction of the present invention to emit only has 3ml, it is 96mL that tap water cleans the gas of emitting, and illustrates that passivation scavenging solution cleaning performance is good.
Utilize GB/T15456-2008 " the mensuration peracid potassium method of chemical oxygen demand (COD) in the industrial circulating cooling water " to measure the COD value of cleaning residual night.
COD pH-value determination pH in the waste liquid
Reagent: Sulfuric acid disilver salt saturated solution; Sulphuric acid soln (volume ratio is 1:3); Sodium oxalate reference liquid (0.01mol/L); Potassium permanganate standard titration solution (0.009964mol/L)
Operation: 1. pipette 5mL and clean in waste liquid and the Erlenmeyer flask, add 50mL water, 2.5mL sulphuric acid soln, 1-5 drips the sulfuric acid saturated solution, and then pipette 10mL potassium permanganate standard volumetric solution, heat until after the boiling at electric mantle, boiled again 5 minutes, waste liquid should be pink or red, if colourless, the potassium permanganate standard volumetric solution of the volume of reordering again, again boil 5 minutes after, be cooled to 60～80 ℃, add 10mL sodium oxalate reference liquid with transfer pipet, it is colourless that waste liquid should be, if take on a red color, add 10mL sodium oxalate reference liquid, then dropping to pink with potassium permanganate standard volumetric solution is terminal point again.Do simultaneously blank test, calculate chemical oxygen demand (COD) (COD) in the waste liquid for maximum value is 18.254mg/L, meet national standard.
SO4 after utilizing the volumetric precipitation method titration to clean in the solution
2-, the cleaning performance of sign passivation clean-out system.
Volumetry titration SO
4 2-
(1) accurately draws the 5mL passivation and clean rear supernatant liquor, place the 250mL Erlenmeyer flask, drip 1mL hydrochloric acid and carry out acidifying, from drop-burette, add certain volume V
1Barium chloride standard solution, the limit edged shakes up, to reduce the absorption of precipitation, and with behind the distilled water flushing inwall, the very hot 2min that boils is cooled to room temperature, add again 10mLMg-EDTA solution, 10mL dehydrated alcohol, 2mL oxammonium hydrochloride, 3mL trolamine, 10mL buffered soln, 3-5 and drip chromium black T indicator, after shaking up, with the titration of EDTA reference liquid, it is terminal point that solution becomes pure blue by purple.Record uses the volume V of EDTA reference liquid
2, do simultaneously blank test, record consumes the volume V of EDTA reference liquid
0
(2) calculate SO4
2-Concentration:
SO
4 2-（g/L）=[C
1V
1-C
2(C
2(V
2-V
0))*M/5
C
1: barium chloride standard solution concentration, moL/L;
C
2: EDTA concentration of standard solution, moL/L;
The quality of M:1moL sulfate radical, g.
By calculating SO4 to cleaning the supernatant liquor titration results
2-Concentration is 7.1651g/L, and by mass conversion, can calculate cleaning rate is 91.95%, has satisfied cleaning performance.
By not adding potassium ferrate and adding two groups of experiments of potassium ferrate, calculate SO4 by described volumetric precipitation method
2-Concentration is respectively 4.03452g/L, 7.1651g/L, is converted into cleaning rate and is respectively 51.80%, 91.95%.Detect discovery by the gas-phase space sulfureted hydrogen gas concentration to the Cleaning and Passivation reaction, the Cleaning and Passivation agent of not adding potassium ferrate can detect hydrogen sulfide (foul smell) gas and emit, and the Cleaning and Passivation agent of interpolation potassium ferrate almost can't detect hydrogen sulfide (foul smell) gas.Experiment shows, the Cleaning and Passivation agent of adding the high ferro acid value can reach good Cleaning and Passivation effect and the assimilation effect of foul smell.
This intellecture property of primary enforcement that all are above-mentioned is not set restriction this product innovation of other forms of enforcement and/or novel method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on product innovation of the present invention.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment does, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (6)
1. a ferrous sulfide deactivation cleaning agent is characterized in that, comprising: sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), potassium ferrate, tensio-active agent and water.
2. ferrous sulfide deactivation cleaning agent as claimed in claim 1 is characterized in that: the weight percent of each component is 0.1～5% sodium bicarbonate, 0.1～10% potassium ferrate, 1～10% clorox, 0.1～5% tetrasodium ethylenediamine tetraacetate, 0.1～5% tensio-active agent and the water of surplus in the described passivation clean-out system.
3. ferrous sulfide deactivation cleaning agent as claimed in claim 1, it is characterized in that: described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene, the fatty alcohol-polyoxyethylene ether.
4. a ferrous sulfide deactivation cleaning agent is characterized in that, comprising: sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-four sodium), potassium ferrate, tensio-active agent and water;
The weight percent of each component is in the described passivation clean-out system: 0.1～5% sodium bicarbonate, 0.1～10% potassium ferrate, 1～10% clorox, 0.1～5% tetrasodium ethylenediamine tetraacetate, 0.1～5% tensio-active agent and the water of surplus;
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene, the fatty alcohol-polyoxyethylene ether.
5. the preparation method of the described ferrous sulfide deactivation cleaning agent of claim 1 to 4 is characterized in that, comprising:
The first step is got part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in proportion in the solution that the first step obtains, continue to add water to needed amount, regulate the pH value between 10～11, continue to stir, obtain described passivation clean-out system.
6. the application in the Iron sulfuret process of the described ferrous sulfide deactivation cleaning agent of claim 1 to 4 in cleaning described petrochemical equipment.
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