CN102912366B - 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 petrochemical technology field, particularly a kind of ferrous sulfide deactivation cleaning agent that prevents Iron sulfuret spontaneous combustion in petrochemical equipment.
Background technology
Iron sulfuret spontaneous combustion in petrochemical equipment (especially refining device) mainly occurs in 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 that prevents Iron sulfuret spontaneous combustion has three kinds at present:
1. isolation method: prevent that Iron sulfuret from contacting with airborne oxygen, as used nitrogen protection, water seal protection etc.;
2. washing out method: will remove on Iron sulfuret slave unit, as equipment is carried out to 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 in maintenance process, is difficult to effectively prevent the spontaneous combustion of Iron sulfuret.The cost of deactivation method is higher, and can not will on Iron sulfuret slave unit, remove.Washing out method comprises physical cleaning and matting, and physical cleaning is mainly to utilize special machine cleaning equipment surface dirt layer; Matting has alkali cleaning, pickling, organic solvent to clean, and the cleaning of the mixed chemical cleaning solution that forms of the tensio-active agent adopting according to the difference of fouling kind and alkali, organic solvent etc.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 extensively adopting at present, is actually traditional washing out method and deactivation method and combines, and in chemical, suitably adds the composition of passivator again.The main passivation clean-out system using mainly contains potassium permanganate, dioxide peroxide, acid, alkaline hydrogen oxygenant.Although these passivation clean-out systems have met petroleum chemical enterprise's safety in production requirement at elimination Iron sulfuret.But use potassium permanganate in 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 to spot corrosion; Pickling comparatively will weigh the corrosion of equipment, although add inhibiter to reduce corrosion, the waste liquid after cleaning still needs to 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 adhering in refining device, the generation of unharmful substance, can absorb the toxic and harmful such as hydrogen sulfide, yperite producing in petrochemical equipment simultaneously, the passivation clean-out system of a kind of efficient, safety, environmental protection, cheapness, deodorizing, also have simultaneously save time, 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-tetra-sodium), potassium ferrate, tensio-active agent and water.
Wherein, in described passivation clean-out system, 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.
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene (OP-10), fatty alcohol-polyoxyethylene ether.
The present invention also provides the preparation method of above-mentioned ferrous sulfide deactivation cleaning agent, comprising:
The first step, gets part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step, in proportion adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in the solution obtaining in the first step, continue to add water to needed amount, regulate 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 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 having not only can be sterilized, and environmentally friendly, be a kind ofly integrate oxidation, adsorb, 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, it is fast to act on, 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-tetra-sodium), potassium ferrate, tensio-active agent and water.
Further, described ferrous sulfide deactivation cleaning agent is only made up of said components.
Wherein, in described passivation clean-out system, 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 ferrous sulfide deactivation cleaning agent provided by the present invention, use potassium ferrate as passivator, potassium ferrate not only can be sterilized, and environmentally friendly, be a kind ofly integrate oxidation, adsorb, 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 be oxidized multiple inorganic, organic substance, 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 the mankind and environment are the strong oxidizers of a kind of ideal, efficient, highly selective;
2, 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 decontaminated water
2-and hypertoxic CN
-, yperite etc.; Ferric acid radical ion decomposes generation Fe (OH) in addition
3can be used as sorbent material, adsorb various zwitterions, there is sewage purification effect, all there is superiority than the various water purification agents that use in the market as alum, polymerize aluminum chloride, ferric sulfate etc., simultaneously, potassium ferrate has absorption, flocculating function, decolouring, deodorizing, the biological oxygen demand (BOD) (BOD) that effectively reduces water body, chemical oxygen demand (COD) value.
3, compared with the oxygenant Manganse Dioxide general with environmental protection aspect, potassium permanganate, chromium trichloride, potassium bichromate, the secondary pollution of potassium ferrate heavy metal free.Compared with chlorinated product, potassium ferrate, without " three cause " effect, does not produce methylene dichloride, trichloromethane compound, does not produce the chlorinated phenols of peculiar smell yet.
4, described potassium ferrate have that sterilization effect is good, consumption is few, it is fast to act on, 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), fatty alcohol-polyoxyethylene ether.
In described passivation clean-out system, in the time that the ferrous sulfide scale in required equipment to be processed is more, can improve the content of potassium ferrate, thoroughly make ferrous sulfide deactivation inactivation, the weight percent of described potassium ferrate in described passivation clean-out system is 0.1～10%, if but be less than 0.1%, can not make the complete passivation of Iron sulfuret in petrochemical equipment, passivation effect is bad, if weight percent exceedes 10%, very easily form reddish-brown precipitation, be attached to cleaning equipment and make.
In described passivation clean-out system, the number residual according to greasy dirt, the content of increase tensio-active agent that can be suitable, improves device cleaning performance, and the weight percent of described tensio-active agent in described passivation clean-out system is 0.1～5%, but, if be less than 0.1%, cannot remove the greasy dirt in cleaned petrochemical equipment, 5% excessive if concentration exceedes, make part surface bioactive molecule cannot touch water, cause the waste of tensio-active agent.
If salt concn or heavy metal ion is more in described petrochemical equipment, can improve the usage quantity of tetrasodium ethylenediamine tetraacetate (EDTA-tetra-sodium), the weight percent of described tetrasodium ethylenediamine tetraacetate in described passivation clean-out system is 0.1～5%, if be less than 0.1%, cannot well take out salt or the heavy metal ion in described petrochemical equipment, and increase tetrasodium ethylenediamine tetraacetate (EDTA-tetra-sodium) content more can be efficiently, salt or the heavy metal ion in complexing petrochemical equipment fast.
Sodium bicarbonate Main Function in described Cleaning and Passivation agent composition is to absorb obnoxious flavour in 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 too low or the too high requirement that all can not meet passivation clean-out system, also fall flat.
Clorox Main Function in 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%, if weight percent will not have oxygenizement lower than 1%, if weight percent exceedes 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-tetra-sodium), potassium ferrate, tensio-active agent and water;
In described passivation clean-out system, 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;
Described tensio-active agent can be a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene (OP-10), fatty alcohol-polyoxyethylene ether.
The present invention also provides the preparation method of above-mentioned ferrous sulfide deactivation cleaning agent, comprising:
The first step, gets part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step, in proportion adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in the solution obtaining in the first step, continue to add water to needed amount, regulate 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 petrochemical unit cleaning process.
Describe embodiments of the present invention in detail below with reference to embodiment, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.
The preparation of embodiment 1 passivation clean-out system
Take 15g Sodium dodecylbenzene sulfonate, 10g sodium lauryl sulphate, 5g alkylphenol polyoxyethylene (OP-10), 8g fatty alcohol-polyoxyethylene ether as tensio-active agent, add in 800g water, stir, dissolve, leave standstill.Then in above-mentioned solution, add 10g potassium ferrate, 50g clorox, 5g ethylenediamine tetraacetic acid (EDTA)-tetra-sodium (EDTA-tetra-sodium), 10g sodium bicarbonate, stirring and dissolving, adds water to 1000g, and making its pH value is 10, and continuation stirring makes solute dissolving, acquisition passivation clean-out system.
Embodiment 2 passivation clean-out systems clean Iron sulfuret experiment relatively
Utilize the reaction of chance water to emit gas reactor and carry out cleaning performance contrast verification to cleaning forward and backward Iron sulfuret residue.
Embodiment
Get passivation clean-out system 100g prepared by embodiment 1, take 1.0g Iron sulfuret powder, be placed in 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 passivation scavenging solution to carry out cleaning reaction with synthermal, same frequency, equal time.
Embodiment and the comparison of comparative example result
By with tap water scavenging solution and utilize passivator scavenging solution clean after residue filter, again residue is cleaned 2-3 time with clear water, after vacuum drying, pack into and meet in water reactor, utilize and control software set test procedure, in testing tube, packing 5% hydrochloric acid into reacts, start testing software, opening switch makes in the disposable inflow reactor of hydrochloric acid, calculate and emit gas content according to rate of gas release, 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, illustrate that passivation scavenging solution cleaning performance is good.
Utilize GB/T15456-2008 " the mensuration peracid potassium method of chemical oxygen demand (COD) in industrial circulating cooling water " to measure the COD value of cleaning residual night.
COD pH-value determination pH in 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 Erlenmeyer flask, add 50mL water, 2.5mL sulphuric acid soln, 1-5 drips sulfuric acid saturated solution, and then pipette 10mL potassium permanganate standard volumetric solution, heating on electric mantle is until after boiling, boil again 5 minutes, waste liquid should be pink or red, if colourless, reorder the again potassium permanganate standard volumetric solution of volume, again boil after 5 minutes, 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 again 10mL sodium oxalate reference liquid, then dropping to pink with potassium permanganate standard volumetric solution is terminal.Do blank test simultaneously, calculate chemical oxygen demand (COD) (COD) in waste liquid for maximum value is 18.254mg/L, meet national standard.
SO4 after utilizing volumetric precipitation method titration to clean in solution
2-, the cleaning performance of sign passivation clean-out system.
Volumetry titration SO
4 2-
(1) accurately draw 5mL passivation and clean rear supernatant liquor, be placed in 250mL Erlenmeyer flask, drip 1mL hydrochloric acid and carry out acidifying, from drop-burette, add certain volume V
1barium chloride standard solution, limit edged shakes up, to reduce the absorption of precipitation, and with after 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 to drip chromium black T indicator, after shaking up, with the titration of EDTA reference liquid, it is terminal that solution becomes pure blue from purple.Record uses the volume V of EDTA reference liquid
2, doing blank test simultaneously, 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 supernatant liquor titration results
2-concentration is 7.1651g/L, and by mass conversion, can calculate cleaning rate is 91.95%, has met 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%.By the gas-phase space sulfureted hydrogen gas concentration of Cleaning and Passivation reaction is detected and is found, the Cleaning and Passivation agent of not adding potassium ferrate can detect that hydrogen sulfide (foul smell) gas emits, and the Cleaning and Passivation agent of adding potassium ferrate almost can't detect hydrogen sulfide (foul smell) gas.Experiment shows, the Cleaning and Passivation agent of adding high ferro acid value can reach good Cleaning and Passivation effect and the assimilation effect of foul smell.
All above-mentioned these intellecture properties of primary enforcement, do 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, be only preferred embodiment of the present invention, is not the restriction of the present invention being made to 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 depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (4)
1. a ferrous sulfide deactivation cleaning agent, is characterized in that, comprising: sodium bicarbonate, clorox, tetrasodium ethylenediamine tetraacetate (EDTA-tetra-sodium), potassium ferrate, tensio-active agent and water;
In described passivation clean-out system, 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.
2. ferrous sulfide deactivation cleaning agent as claimed in claim 1, is characterized in that: described tensio-active agent is a kind of or several mixing in dodecylbenzene sulfonate, dodecyl sulfate, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether.
3. the preparation method of ferrous sulfide deactivation cleaning agent described in claim 1 or 2, is characterized in that, comprising:
The first step, gets part water, adds in proportion described tensio-active agent in described water, and stirring and dissolving leaves standstill;
Second step, in proportion adds potassium ferrate, clorox, tetrasodium ethylenediamine tetraacetate and sodium bicarbonate, stirring and dissolving in the solution obtaining in the first step, continue to add water to needed amount, regulate pH value between 10～11, continue to stir, obtain described passivation clean-out system.
4. the application of the ferrous sulfide deactivation cleaning agent described in claim 1 or 2 in the Iron sulfuret process of cleaning in petrochemical equipment.
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| CN101565828B (en) * | 2009-06-03 | 2010-10-27 | 北京科技大学 | Organic and inorganic composite magnesium alloy non-chromium passivation treatment fluid |
| CN102373122B (en) * | 2010-08-12 | 2013-04-24 | 中国石油化工股份有限公司 | Inorganic ferrous sulfide passivation abluent |
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