CN100529188C - Preparing process of gas phase corrosion inhibitor - Google Patents

Preparing process of gas phase corrosion inhibitor Download PDF

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CN100529188C
CN100529188C CNB2006101183109A CN200610118310A CN100529188C CN 100529188 C CN100529188 C CN 100529188C CN B2006101183109 A CNB2006101183109 A CN B2006101183109A CN 200610118310 A CN200610118310 A CN 200610118310A CN 100529188 C CN100529188 C CN 100529188C
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vapour
solution
phase inhibitor
polynite
deionized water
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高立新
张大全
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Lianyungang Dongsen Technology Development Co.,Ltd.
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Shanghai University of Electric Power
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Abstract

The preparation process of gas phase corrosion inhibitor includes the following steps: 1. dispersing montmorillonite into deionized water, pulping, taking the suspension, adding morpholine, and heating to evaporate solvent and separating out crystal; 2. adding formaldehyde to the solution, letting stand, adding dicyclohexane, letting stand, adding mixed solution of benzoic acid and acetone, letting stand to form while slurry, dispersing the slurry in deionized water, suction filtering, and drying at 80 deg.c to obtain target product. By means of in-situ intercalating synthesis process, the present invention prepares gas phase corrosion inhibitor with homogeneous structure, fine granulation, and improved volatilizing capacity and corrosion inhibiting performance.

Description

A kind of preparation method of vapour-phase inhibitor
Technical field
The present invention relates to prevent, delay the inhibiter of metallic corrosion, relate to a kind of preparation method of vapour-phase inhibitor in particular.
Background technology
Vapour-phase inhibitor (vapor phase inhibitor, be called for short VPI), be called volatile corrosion inhibitor (volatile corrosion inhibitor again, be called for short VCI), be a kind of gas adsorption that can volatilize automatically at normal temperatures at metallic surface, thereby prevent the protection against corrosion chemical of metallic corrosion.That vapour-phase inhibitor has is easy to use, clean, the characteristics of cleaning, has become an important directions that prevents the atomospheric corrosion technical development.Volatile rust prevention drying material (Vapor Phase corrosion inhibitordesiccant material) is to handle the vapor phase corrosion inhibitor agent solution with siccative, heating also evaporates a kind of vapour-phase inhibitor that moisture makes and siccative combines and the novel volatile rust prevention matrix material made, and it can remedy the deficiency of vapour-phase inhibitor rustless property under high humidity environment.Have the preparation method of more bibliographical information volatile rust prevention siccative both at home and abroad, as select that the aperture is suitable, two kinds of volatile rust prevention siccative that pH value neutral natural zeolite is handled the vapour-phase inhibitor preparation, in composition, accounting for of vapour-phase inhibitor wherein 20%～25%, main component organic acid amine salt, nitrite and benzotriazole etc.Chinese patent application application number 200410051943.3, October 18 2004 applying date, publication number CN1619014, open day on May 25th, 2005, a kind of gas phase and dry rust-proofing method are also disclosed, be that vapour-phase inhibitor and siccative are made into the dry bag of volatile rust prevention in proportion, the weight ratio of described vapour-phase inhibitor and siccative is 2%～40%, and they play rust inhibition simultaneously in same packing closed environment.Yet, vapour-phase inhibitor and siccative combine and the novel volatile rust prevention matrix material made in the prior art, mostly by simple mechanical complex method, wherein the content of siccative is much higher than the content of corresponding vapour-phase inhibitor, because siccative has the trend of strong absorption ambient moisture, this will damage the release rate of vapour-phase inhibitor component, thereby cause vapour-phase inhibitor anticorrosion ability variation.
Summary of the invention
Technical problem to be solved by this invention provides a kind of improved vapour-phase inhibitor preparation method, make vapour-phase inhibitor mutually compound with nanoscale with inorganic porous carrier, so just can make the vapour-phase inhibitor of even structure, fine size, the state of aggregation of vapour-phase inhibitor be can regulate and control, thereby its volatile performance and corrosion mitigating effect improved.
The technical solution used in the present invention: a kind of preparation method of vapour-phase inhibitor comprises the following steps:
A. polynite is scattered in the deionized water, pulls an oar, stirs, the suspension of getting solution then heats up to wherein adding morpholine, has precipitation to separate out in the solution;
B. in the solution of step a, add formaldehyde, leave standstill for some time, add dicyclohexyl amine, stirring reaction for some time, the mixing solutions of adding phenylformic acid and acetone in solution then, leave standstill for some time generation white slurry, at last slurry is scattered in the deionized water, suction filtration obtains white powder, 80 ℃ of forced air dryings, obtain described vapour-phase inhibitor.
Before step a is scattered in polynite in the deionized water, modification is carried out in polynite, described modification is with the polynite wiring solution-forming, get upper strata suspension after leaving standstill and be warmed up to 80 ℃, add 30% cetyl trimethylammonium bromide solution then, stir the back suction filtration, reduce Br 3～4 times as far as possible with deionized water rinsing -, put into 120 ℃ of dryings of baking oven and grind to form 500 order powder after 4 hours, obtain montmorillonite modified.
The consumption of polynite or montmorillonite modified accounts for the 1%-10% of entire reaction thing weight.Reactant does not comprise simple solvent.
Beneficial effect of the present invention: the present invention adds polynite in the preparation process of vapour-phase inhibitor, porous carrier by polynite is as template, synthesizing of regulation and control vapour-phase inhibitor, change its state of aggregation and stability, thereby improved the volatile performance and the gas phase corrosion inhibiting ability of vapour-phase inhibitor.The present invention has utilized in-situ inserted synthesis method, raw material, the auxiliary agent of synthetic gas phase corrosion inhibitor are inserted in the silicate lamella of polynite, it is synthetic to carry out original position then, a large amount of heats of emitting when utilization is synthetic have overcome the Coulomb's force between the silicate lamella, it is peeled off, thereby make the silicate lamella mutually compound with nanoscale with vapour-phase inhibitor, so just can make the vapour-phase inhibitor of even structure, fine size, regulate and control the state of aggregation of vapour-phase inhibitor, improved the volatilization ability and the application performance of vapour-phase inhibitor.
Description of drawings
The volatile loss trial curve figure of Fig. 1 vapour-phase inhibitor in enclosed space;
Fig. 2 electrochemical tests figure.
Embodiment
Below by embodiment the present invention is described in further detail: a kind of preparation method of vapour-phase inhibitor, comprise the following steps: that a. is scattered in polynite in the deionized water, pulls an oar, stirs, the suspension of getting solution then is to wherein adding morpholine, and heating up makes solution evaporation and separate out crystal; B. in the solution of step a, add formaldehyde, leave standstill for some time, add dicyclohexyl amine, leave standstill for some time, in solution, add the mixing solutions of phenylformic acid and acetone then, leave standstill for some time generation white slurry, at last slurry is scattered in the deionized water, suction filtration obtains white powder, 80 ℃ of forced air dryings, obtain described vapour-phase inhibitor.The present invention directly adds inorganic porous silicate material in the building-up process of vapour-phase inhibitor, raw material, the auxiliary agent of synthetic gas phase corrosion inhibitor are inserted in the silicate lamella of polynite, it is synthetic to carry out original position then, utilize a large amount of heats of emitting when synthesizing, overcome the Coulomb's force between the silicate lamella, it is peeled off, thereby make the silicate lamella mutually compound with nanoscale with vapour-phase inhibitor, so just can make the vapour-phase inhibitor of even structure, fine size, the state of aggregation of regulation and control vapour-phase inhibitor, thus its volatilization ability and application performance improved.Described vapour-phase inhibitor can be organic amine and its esters: as quadrol, hexanediamine, hexahydroaniline, dicyclohexyl amine, Diisopropylamine, benzylamine, monoethanolamine, diethanolamine, trolamine, n-Butyl Amine 99, Tributylamine, amylamine, stearylamine, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, hexamethylenetetramine (urotropine), morpholine, piperidines, piperazine etc.; Also can be mineral acid or organic acid and its esters: as phosphoric acid, nitrous acid, phenylformic acid, styracin, sad, capric acid, lauric acid, Succinic Acid etc., wherein phenylformic acid can be substituted by nitrobenzoic acid, cresotinic acid, Whitfield's ointment, tert-butylbenzene formic acid; Also can be organic heterocyclic class inhibiter such as the benzotriazole and the derivative thereof of some non-ferrous metals, benzothiazole etc.Inorganic porous carrier mainly is included as silica gel, alchlor, diatomite, zeolite molecular sieve, polynite, recessed soil etc., also comprises organically-modified inorganic carrier material, as organic polynite etc.Auxiliary agent is dibutyl phthalate (DBP) (hot fat), polyvinyl alcohol, Ployethylene Wax, quaternary amine tensio-active agent etc.
Below, by specific embodiment, describe the present invention in detail.Yet, mandatory declaration be organic amine and its esters vapour-phase inhibitor, the preparation feedback of organic acid and its esters vapour-phase inhibitor all is based on the salifiable reaction of soda acid, so the vapor phase inhibitor of not mentioning in the example all can carry out modification by following similar method, the present invention is not limited to these specific embodiments.
Embodiment 1
Take by weighing an amount of polynite, be scattered in the deionized water, making beating is about to the polynite activation, after stirring 24 hours, gets the suspension of solution, adds a certain amount of morpholine therein, is warming up to 80 ℃, and constant temperature 4-5 hour, at this moment, solution evaporation was also separated out solid; Add a certain amount of formaldehyde, left standstill 4 hours, do not have obvious phenomenon; Add a certain amount of dicyclohexyl amine, left standstill the solution layering 3 hours; The mixed solution of phenylformic acid and acetone is added wherein, left standstill 8 hours, generate white slurry and (note: in this process, need not stop to stir), in slurry dispersion and the deionized water, suction filtration, obtain white powder, forced air drying under 80 ℃ of conditions obtains 52g vapour-phase inhibitor 1.
Embodiment 2
Polynite wiring solution-forming (massfraction is 5%) with 20g leaves standstill for some time, and it is stand-by to get upper strata suspension.The cetyl trimethylammonium bromide solution (concentration is 105mmol/100g soil) of adding 30% stirs suction filtration after 1 hour in the time of 80 ℃, makes for 3-4 time with deionized water rinsing and reduces Br as far as possible -, put into baking oven and grind to form 500 order powder after 4 hours in 120 ℃ of dryings, get organo montmorillonite.Get the 1.0g modified montmorillonoid and add the 20ml morpholine, after stirring 1 hour under 50 ℃ of conditions, slowly drip 19.2ml formaldehyde solution while stirring, stir observe phenomena after 2 hours, drip the 46ml dicyclohexyl amine, observe phenomena, stir and add benzoic acid solution (the 28g phenylformic acid is dissolved in the 40ml deionized water) after 3 hours again, observe phenomena continues to stir after 4 hours and carries out suction filtration, put into oven for drying, promptly get 75g vapour-phase inhibitor 2.
Embodiment 3
Take by weighing an amount of polynite, be scattered in the ethanolic soln, making beating is about to the polynite activation, after stirring 24 hours, get the suspension of solution, the monoethanolamine of 5g is added in the above-mentioned solution, mix and stir, the 12g phenylformic acid is dissolved in the ethanolic soln, with two kinds of solution intermingling under constantly stirring, promptly produce the precipitation of white, suction filtration promptly gets 15g vapour-phase inhibitor 3.
Embodiment 4
Taking by weighing the 0.5g organo montmorillonite adds in the ethanolic soln, the monoethanolamine of 4.7g is added in the above-mentioned solution, stirred 12 hours, 20 laurostearic acids are dissolved in the ethanolic soln, with two kinds of solution intermingling under constantly stirring, promptly produce the precipitation of white, mix and stir, suction filtration promptly gets 21g vapour-phase inhibitor 4.
Simultaneous test 1
Embodiment 1 and 2 gained target products are carried out the vapour-phase inhibitor volatile loss test of modification front and back.Vapour-phase inhibitor is used in enclosed space or semi closed space mostly, should have certain saturated vapor pressure, guarantee that there is certain density vapour-phase inhibitor in the space under the certain temperature condition, can be adsorbed onto the metallic surface and play rust inhibition, the vapour-phase inhibitor that vapour pressure is big can volatilize fast and be adsorbed onto the metallic surface and restrain corrosion process in advance in general, and the vapour-phase inhibitor that vapour pressure is little then has persistent rust-proof effect.(under the normal temperature 0.133～0.013Pa), use general instrument to be difficult for measurement but usually the vapour pressure of vapour-phase inhibitor is very little.The gasification performance that compares vapour-phase inhibitor by the volatile loss test indirectly.Preparation embodiment 1 gained target product is carried out the vapour-phase inhibitor volatile loss test of modification front and back: the vapour-phase inhibitor of weighing 0.5g places 5cm diameter surface ware, evenly spread out, the baking oven of putting into 50 ℃ heats 72h continuously, every 24h weighing once, calculate rate of weight loss, the results are shown in Figure enclosed space volatile loss test (the common synthetic vapour-phase inhibitor of 1-of 1 vapour-phase inhibitor; 2-vapour-phase inhibitor 1; 3-vapour-phase inhibitor 2).The volatilization weight-loss ratio of vapour-phase inhibitor in 72 hours is to reduce gradually along with the prolongation of time, and this is owing to the concentration that reaches capacity gradually of vapour-phase inhibitor in enclosed space causes evaporation rate to slow down.From experimental result, the initial volatile weight loss rate of the vapour-phase inhibitor after imvite modified is obviously greater than the vapour-phase inhibitor that there is not modification, this shows organic imvite modified vapour-phase inhibitor, can increase the volatilization ability of vapour-phase inhibitor, thereby influences the application performance of vapour-phase inhibitor.The more common vapour-phase inhibitor of volatile weight loss rate of the vapour-phase inhibitor of method preparation of the present invention is big, shows that the vapour-phase inhibitor of method preparation of the present invention has the ability of volatilizing preferably.
Simultaneous test 2
Embodiment 1, embodiment 2, embodiment 3 and embodiment 4 gained target products are carried out volatile rust prevention differentiation test: will fill the weighing bottle that changes 1g modified gas phase corrosion inhibitor and place Erlenmeyer flask, hang two of the Q235 steel of 50mm * 25mm * 2mm respectively, a slice does not add inhibiter and contrasts, the saturated 2h. of constant temperature injects the distilled water of 15ml then with transfer pipet in 50 ℃ of baking ovens, be stored in and keep 50 ℃ of temperature in the thermostat container, heat 8h every day, every 24h is an one-period, observe every day 1 time, carry out 7 periodic tests altogether, volatile rust prevention differentiation test-results sees Table 1.Corrosion does not take place in the vapour-phase inhibitor of the present invention's preparation in 7 cycles.
Table 1 volatile rust prevention discrimination test result
Figure C20061011831000081
Simultaneous test 3
Embodiment 1, embodiment 2, embodiment 3 and embodiment 4 gained target products are carried out vapor inhibitability test: the good test piece concave surface of will polishing is pressed in No. 9 soft rubber balls, test is showed out part and is no more than 3mm, the dehydrated alcohol degreasing of test piece test face after press-fiting, hot blast drying, experimental installation is with reference to Machinery Ministry standard JB/T 6071-92.Inject 35% aqueous glycerin solution 10ml in the wide-necked bottle of 1000ml bottom, adjusting relative humidity is 90%, is even spreading 0.5g vapour-phase inhibitor in the vessel of 40 ± 2mm at diameter; Testing apparatus placed under 20 ± 2 ℃ the temperature, in aluminum pipe, fill with temperature behind the 20h and be 2.0 ± 0.5 ℃ frozen water, keep down pouring out behind the 3h at 20 ± 2 ℃ again, take off the cotton sample of cleaning of paper, dry up the back and check that there is non-corroding on the test piece surface with what be soaked with dehydrated alcohol.The result shows that the modified gas phase corrosion inhibitor that the present invention prepares can make metal testing plate that corrosion does not take place.
Simultaneous test 4
Embodiment 2 gained target products are simulated the electrochemical tests of the carbon steel electrode in the atomospheric corrosion solution and measure, and compare with common synthetic vapour-phase inhibitor.Electrochemical tests is measured and is carried out on three-electrode system, saturated calomel electrode is a reference electrode, Pt is a supporting electrode, and carbon steel electrode is a work electricity electrode, and adopting simulation atomospheric corrosion water (0.1g/L NaCl, 0.1g/L NaHCO3,0.1g/L Na2SO4) is supporting electrolyte.Surveying instrument is the CHI660B electrochemical workstation of Shanghai occasion China instrument company, and sweep limit is-1200 ± 400mv, and sweep velocity is 2mV/s.Use the epoxy encapsulation carbon steel electrode, exposed area is 1cm2, and abrasive paper for metallograph is polished step by step, the alcohol degreasing, and deionized water rinsing is clean.Given current potential is the current potential with respect to saturated calomel electrode (SCE), the results are shown in Figure 2 electrochemical tests (1-blank, 2～0.5% common synthetic gas phase corrosion inhibitors, 3～0.5% vapour-phase inhibitors 2).Fig. 2 shows: common synthetic vapour-phase inhibitor all has restraining effect to the negative electrode and the anode electrochemical process of carbon steel electrode, and is comparatively speaking bigger for the restraining effect of anode electrochemical process.Adopt the inventive method synthetic vapour-phase inhibitor 2, further increased the anode of counter electrode and the restraining effect of electrochemical cathode process.

Claims (3)

1. the preparation method of a vapour-phase inhibitor comprises the following steps:
A. polynite is scattered in the deionized water, pulls an oar, stirred 24 hours, the suspension of getting solution then is warming up to 80 ℃ to wherein adding morpholine, constant temperature 4-5 hour, has precipitation to separate out in the solution;
B. in the solution of step a, add formaldehyde, left standstill 4 hours, add dicyclohexyl amine, stirring reaction 3 hours, the mixing solutions of adding phenylformic acid and acetone in solution then, leave standstill and generated white slurry in 8 hours, at last slurry is scattered in the deionized water, suction filtration obtains white powder, 80 ℃ of forced air dryings, obtain described vapour-phase inhibitor.
2. according to the preparation method of the described a kind of vapour-phase inhibitor of claim 1, it is characterized in that: before being scattered in polynite in the deionized water among the described step a modification is carried out in polynite, described modification is with the polynite wiring solution-forming, get upper strata suspension after leaving standstill and be warmed up to 80 ℃, add 30% cetyl trimethylammonium bromide solution then, stir the back suction filtration, reduce Br 3～4 times as far as possible with deionized water rinsing -, put into 120 ℃ of dryings of baking oven and grind to form 500 order powder after 4 hours, obtain montmorillonite modified.
3. according to the preparation method of claim 1 or 2 described a kind of vapour-phase inhibitors, it is characterized in that the consumption of polynite or montmorillonite modified accounts for the 1%-10% of entire reaction thing weight.
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CN104098984B (en) * 2014-06-27 2016-05-11 国家电网公司 A kind of imvite/epoxy self-healing coatings that loads corrosion inhibiter
CN105316687A (en) * 2014-07-01 2016-02-10 蒋寿悟 Improved gas-phase antirust agent and preparation method thereof
CN110004446A (en) * 2019-03-15 2019-07-12 吉林三鑫工贸有限责任公司 Vapor phase inhibitor and preparation method thereof
CN110804388A (en) * 2019-10-11 2020-02-18 中航百慕新材料技术工程股份有限公司 Inorganic alkene zinc coating and preparation method and application thereof
CN111172543A (en) * 2019-12-27 2020-05-19 国网浙江平湖市供电有限公司 Preparation method of humidity-regulating controlled-release type vapor phase corrosion inhibitor
CN111088497A (en) * 2019-12-27 2020-05-01 国网浙江平湖市供电有限公司 Humidity-regulating controlled-release type vapor phase corrosion inhibitor
CN114959712B (en) * 2021-02-25 2024-02-23 中国石油化工股份有限公司 Vapor phase corrosion inhibitor and preparation method thereof

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Publication number Priority date Publication date Assignee Title
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Publication number Priority date Publication date Assignee Title
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