CN104596883A - Determination method for concentration of octadecylamine - Google Patents
Determination method for concentration of octadecylamine Download PDFInfo
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- CN104596883A CN104596883A CN201510063319.3A CN201510063319A CN104596883A CN 104596883 A CN104596883 A CN 104596883A CN 201510063319 A CN201510063319 A CN 201510063319A CN 104596883 A CN104596883 A CN 104596883A
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- octadecylamine
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Abstract
The invention provides a determination method for the concentration of octadecylamine. The determination method comprises the following steps: weighing a certain weight of a solution to be detected and drying at a constant temperature of 70-110 DEG C for 1-10 hours until the solution to be detected is cooled to a room temperature when the solution to be detected is in a colorless, clarified and transparent colloid shape; recording the mass of the solution to be detected as m0 before drying and recording the mass of the solution to be detected as m1 after drying; and calculating the weight percent concentration of the solution to be detected according to a formula (m1/m0)*100%, wherein the solution to be detected is octadecylamine emulsion for boiler shutdown protection. The method only needs to use conventional instrument equipment and is convenient to operate; the error can be controlled within 5%; and the determination method can be used for checking and accepting a purchased octadecylamine emulsion product for the boiler shutdown protection of a thermal power plant.
Description
Technical field
The present invention relates to chemical field, particularly the determination techniques of octadecylamine concentration in octadecylamine shutdown protection solution.
Background technology
The heat power equipment such as boiler, steam turbine, condenser, well heater of genset is during stopping transport, if do not take effective safeguard measure, strong corrosion can occur on its surface, and this corrosion is called the withdrawal hepatitis of heat power equipment.For many years, China's fired power generating unit often because of do not take after stopping transport anticorrosive measure or the anticorrosive measure taked improper, cause corrosion and damage, especially the corrosion of steam side, the safety and economic operation of power plant caused to having a strong impact on.
The Shut-down Protection measure generally adopted both at home and abroad at present; according to its action principle; can be divided three classes substantially: the first kind stops air to enter heat power equipment water-steam system inside, and its essence is the concentration reducing oxygen, these class methods have nitrogen method of filling, keep vapour pressure force method etc.Equations of The Second Kind is the humidity reducing heat power equipment water-steam system inside, its essence is and prevents metal surface condensation water film, forms corrosion cell.These class methods have oven drying method, Desicdant method etc.3rd class uses corrosion inhibiter (comprising vapour-phase inhibitor and high temperature film inhibitor etc.), or add the pH value of basifier, adjustment solution, makes metal surface form diaphragm; slow down the corrosion of metal surface; or use oxygen scavenger, except the dissolved oxygen DO in anhydrating, corrosion is alleviated.Institute's with medicament has vapour-phase inhibitor, high temperature film inhibitor, ammonia, diamine etc.The essence of these class methods is that the anode of corrosion cell and/or cathodic process are blocked.
According to heat power equipment in the difference of stopping residing anti-corrosion state during (standby) is used, Shut-down Protection method can be divided into dry type Protection Code and the large class of wet type Protection Code two.Dry type Protection Code has: hot stove discharge water residual heat drying method, negative pressure residual heat drying method, adjacent stove hot-air seasoning method, Desicdant method, fill nitrogen method, vapour-phase inhibitor method etc.Wet type Protection Code has: Ammonia Process, ammonia-diamine method, vapour pressure force method, feed pressure method etc.
Wherein high temperature film inhibitor method is more, the more welcome Shut-down Protection method of current domestic application.It is Moscow, Russia power institute in research in 1987 successfully, first uses on your Darius gram central-station unit of longevity, after in succession use on many power station unit of Yugoslavia, Germany and the state such as Russian.High temperature film inhibitor method is in the sliding uniform temperature of stopping in process of unit, under pressure and pH condition, disposablely in boiler feed water or condensate water in certain hour add high temperature film inhibitor, film inhibitor is by forming coordination bond between the lone pair electrons on its atom N 2P track and the 3d unoccupied orbital of Fe, and (comprise boiler at heat power equipment, steam turbine etc.) metal surface formation layer of hydrophobic film, isolated metallic matrix contacts with the direct of water with air, oxygen in anti-sealing and air and carbon dioxide are to corrosion of metal, reach the object of protection heat power equipment, the structure of film may be: iron/iron oxide layer/and containing the film forming layer of the corrosion inhibiter film forming layer/corrosion inhibiter of iron oxide.
The feature of high temperature film inhibitor method is: (1) protected effect is good; can be formed evenly in the equipment surface such as boiler, steam turbine, the diaphragm that fine and close, corrosion stability is good; certain cleaning, removal effect is had to corrosion product such as the rust etc. of metal surface; the content of copper, iron etc. when making unit starting in steam reduces, thus shortens grid-connected time when unit starts again.(2) protection domain is wide, can protect boiler (comprising drum, water-cooling wall, economizer, superheater, reheater etc.) and steam turbine simultaneously.(3) guard time is long, and after heat power equipment surface filming, the corrosion protection time in an atmosphere can reach more than 6 months.(4) protect technique simple, easy to operate; do not need newly-increased medicine system; on-the-spot feedwater or condensate water medicine system can be utilized; under sliding uniform temperature, pressure and the pH condition of stopping in process of unit, disposablely in boiler feed water or condensate water in certain hour add high temperature film inhibitor.(5) applied range, the power-equipment of running temperature more than 200 DEG C all can adopt high temperature film inhibitor method to carry out Shut-down Protection.
At present, domestic film inhibitor mainly octadecylamine (ODA) and imidazolines material stopping (standby) use Shut-down Protection for genset heat power equipment, wherein octadecylamine application is comparatively general.
Octadecylamine, has another name called octadecylamine, filming amine, belongs to fatty amines, and be a kind of organic polymer hydrocarbon compound, end group is-NH
2, molecular formula is CH
3(CH
2)
16cH
2nH
2, be white waxy solid or particulate material under normal temperature, belong to cationic surfactant, be soluble in chloroform, be dissolved in ethanol, ether and benzene, be slightly soluble in acetone, be insoluble in water, in suspension in 75 DEG C of water, density is 860kg/m, 52.9 DEG C, solidifying point, boiling point 348.8 DEG C.
Octadecylamine, by physical and chemical adsorption effect, forms one deck and can resist the unimolecular layer of oxygen and carbonic acid or the hydrophobic film of polymolecular layer, play barrier buffer action in metal surface, thus protection metal, reduce corrosion.To stop using anti-corrosion protection technology so octadecylamine is used to genset heat power equipment water-steam system.
Octadecylamine anti-corrosion protection technology of stopping using comes across USSR (Union of Soviet Socialist Republics) the earliest, and early fifties is tried out in certain cogeneration plant, and effect is better, but because of dosing technological problems, is not promoted always.The late nineteen eighties, USSR (Union of Soviet Socialist Republics) and the East Germany principal ingredient that releases one after another is the liquid preservative agent of octadecylamine, and the very fast nuclear power station in Russia and Germany, thermal power station are applied, and effect is fairly obvious.China to investigate and exchange of technology personnel take back for information about in 1993 Nian Fu Russia, and many electric power research units and universities and colleges start corresponding development, development & application.Wherein, some units such as Wuhan University have carried out system and deep research to the membrance casting condition of octadecylamine and membrane formation mechanism, think as a kind of organic inhibitor, octadecylamine has stronger superiority in high temperature film forming, and in liquid and vapor capacity all energy film forming, concentration is higher, film-formation result is better, in autoclave, the constant temperature film-formation result of hour is best, and best film-forming temperature is 220 DEG C, and the roughness of specimen surface has certain influence to film forming; Analyzed by Auger electron spectroscopy, after the process of octadecylamine film forming, iron surface has following structure: iron ∣ is oxidized the octadecylamine layer ∣ octadecylamine layer of iron layer ∣ containing iron oxide.
Common Shut-down Protection technique the cunning of octadecylamine emulsion before shutdown is stopped controlling vapor (steam) temperature in process be less than 450 DEG C, fast medicament added therrmodynamic system, shut down after circulation 1h, then after cooling, system band presses water, utilizes residual heat drying boiler.
At present, protection of boiler during shutdown period octadecylamine emulsion is more and more extensive in the application of thermal power plant, but high concentration octadecylamine emulsion, Concentration Testing namely as the protection of boiler during shutdown period octadecylamine emulsion of production marketing never has appropriate method, thus meet difficulty when thermal power plant carries out an acceptance inspection to purchased protection of boiler during shutdown period octadecylamine emulsion product, the weight can only understanding protection of boiler during shutdown period octadecylamine emulsion by weighing is enough, but do not know that the amount of the octadecylamine really shielded is enough, in the urgent need to can be used for the octadecylamine concentration detection method of actual examination protection of boiler during shutdown period octadecylamine emulsion product, to strengthen the quality supervision of protection of boiler during shutdown period octadecylamine emulsion product, ensure the safety applications of protection of boiler during shutdown period octadecylamine emulsion product.
Why " Concentration Testing as the protection of boiler during shutdown period octadecylamine emulsion of production marketing never has appropriate method "; that a lot of people thinks that the method also can as the detection method of octadecylamine concentration in the protection of boiler during shutdown period octadecylamine emulsion of production marketing because have one " a kind of assay method of octadecylamine concentration " on the one hand.The method can only survey the octadecylamine of low concentration in water in fact, detects high concentration octadecylamine and can bring very big error.Because the measurement range of the method is 10-50mg/L octadecylamine concentration; and general be a few percent as the octadecylamine concentration in the protection of boiler during shutdown period octadecylamine emulsion of production marketing; if detected by the method; octadecylamine emulsion to be diluted up to ten thousand times; add that octadecylamine is not soluble in water, octadecylamine emulsion understands layering after diluting; so just bring very big error, cause testing result and actual concentrations widely different, thus actually can not to use.Because the protection of boiler during shutdown period octadecylamine emulsion as production marketing is not also a kind of real commodity on the other hand; just selling as research products; virtually coverd with one deck mystery flavour; the buyer adding applying unit is ignorant of technology; so the buyer of applying unit measures enough by all means; and the amount being ignorant of also being unable to control or manage the octadecylamine really shielded is enough; decrease trouble to like this sellers, user, otherwise sellers, user be in a rush and muddle because can not find suitable Concentration Testing way, cannot check and accept.Based on this, we have invented the octadecylamine concentration detection method that can be used for actual examination protection of boiler during shutdown period octadecylamine emulsion product.In order to invention this method, we have changed multiple invention thinking, thousands of tests are carried out, as thought, testing, detection emulsion density, volume were to calculate octadecylamine concentration, also thought, tested real constant weight to detect octadecylamine concentration in emulsion, in order to obtain constant weight temperature, time, update invention thinking especially, constantly test, just be tending towards perfect.
Summary of the invention
The invention provides the method for octadecylamine concentration in a kind of gravimetric determination octadecylamine emulsion; the method only needs routine instrument device; easy to operate, can departure within 5%, can carry out an acceptance inspection to purchased protection of boiler during shutdown period octadecylamine emulsion product for thermal power plant.
Concrete technical scheme is as follows:
An assay method for octadecylamine concentration, takes solution to be measured freeze-day with constant temperature 1-10h under 70 ~ 110 DEG C of conditions of certain mass, and when solution to be measured is achromaticity and clarification transparent colloidal, be cooled to room temperature, the quality recorded respectively before solution drying to be measured is m
0, dried quality is m
1, according to formula (m
1/ m
0) × 100% can calculate the weight percent concentration in solution to be measured; Described solution to be measured is protection of boiler during shutdown period octadecylamine emulsion.
The drying condition of described solution to be measured is dry 4h under 90 DEG C or 100 DEG C of conditions.
Beneficial effect of the present invention is: this method is easy to operate, without the need to adding any reagent in addition, only needs routine instrument device; Can measure the octadecylamine emulsion of high concentration, and error is very little, can be controlled within 5%, can carry out an acceptance inspection to purchased protection of boiler during shutdown period octadecylamine emulsion product for thermal power plant.
Embodiment
Below in conjunction with embodiment, further detailed description is done to the present invention, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) compound concentration is the octadecylamine emulsion of 2%;
(2) open drying box power supply and drying box is warmed up to 100 DEG C and constant temperature;
(3) three surface plate priority tap water and demineralized water cleaned up, put into the drying box that temperature is tuned to 105 ± 3 DEG C and be dried to constant weight, weigh after then putting into exsiccator cooling 30min, and be M by the quality record of three surface plates
10, M
20, M
30;
(4) with glass bar dip preparation, concentration is that the octadecylamine emulsion uniform application of 2% is on surface plate, the quality controlling octadecylamine emulsion on each surface plate with electronic scales is 7.3g, then weigh the quality of these 3 surface plates (containing octadecylamine emulsion) with electronic analytical balance, and be recorded as M
11, M
21, M
31;
(5) surface plate scribbling octadecylamine emulsion is put into constant temperature to the drying box of 100 DEG C together with pallet;
(6) dry certain hour (2h ~ 4h), when to observe octadecylamine emulsion be achromaticity and clarification transparent colloidal, take out pallet and surface plate put into exsiccator drying and be cooled to room temperature, then weigh with electronic analytical balance, and be recorded as M
13, M
23, M
33; If
(7) calculate octadecylamine in octadecylamine emulsion concentration and with 2% deviation; If deviation is greater than 5%, then repeat step (5), (6), until the concentration of octadecylamine and the deviation of 2% are less than 5% in the octadecylamine emulsion calculated.
Result of implementation is as table 1.
The octadecylamine concentration corresponding from different constant temperature time recorded at 100 DEG C, table 1 and with 2% deviation
As shown in Table 1,2 batches totally 6 experimental tests show, at 100 DEG C preparation 2% octadecylamine emulsion, the octadecylamine concentration that constant temperature 4h records and the deviation of 2% are all within 5%.
Embodiment 2
(1) compound concentration is respectively the octadecylamine emulsion of 2%, 4%, 6%, 8%, 10%;
(2) open drying box power supply and drying box is warmed up to 70 DEG C or 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C and constant temperature;
(3) three surface plate priority tap water and demineralized water cleaned up, put into the drying box that temperature is tuned to 105 ± 3 DEG C and be dried to constant weight, weigh after then putting into exsiccator cooling 30min, and be M by the quality record of three surface plates
10, M
20, M
30;
(4) with glass bar dip preparation, concentration is that the octadecylamine emulsion uniform application of 2% or 4%, 6%, 8%, 10% is on surface plate, the quality controlling octadecylamine emulsion on each surface plate with electronic scales is 7.3g, then weigh the quality of these 3 surface plates (containing octadecylamine emulsion) with electronic analytical balance, and be recorded as M
11, M
21, M
31;
(5) surface plate scribbling octadecylamine emulsion is put into the drying box to 70 DEG C or 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C of constant temperature together with pallet;
(6) dry certain hour (1h ~ 10h), when to observe octadecylamine emulsion be achromaticity and clarification transparent colloidal, take out pallet and surface plate put into exsiccator drying and be cooled to room temperature, then weigh with electronic analytical balance, and be recorded as M
13, M
23, M
33; If
(7) calculate octadecylamine in octadecylamine emulsion concentration and with 2% deviation; If deviation is greater than 5%, then repeat step (5), (6), until in the octadecylamine emulsion calculated octadecylamine concentration and 2% or 4%, 6%, 8%, the deviation of 10% is less than 5%.
Result of implementation is as table 2.
The constant temperature time that the octadecylamine concentration that table 2 records is corresponding with the deviation < 5% of corresponding compound concentration
As shown in Table 2: the concentration that (1) prepares is the octadecylamine emulsion of 2% or 4%, 6%, 8%, 10%, constant temperature at 70 DEG C ~ 110 DEG C, all records the octadecylamine concentration with the deviation < 5% of corresponding compound concentration by constant temperature substantially; (2) thermostat temperature is different, and required constant temperature time is different, and along with the rising of thermostat temperature, required constant temperature time is shortening trend; (3) thermostat temperature is 90 DEG C or 100 DEG C, constant temperature time is when being 4h, deviation all < 5% of the octadecylamine concentration recorded and corresponding compound concentration (2% or 4%, 6%, 8%, 10%).
Above-described embodiment 1 and embodiment 2 are screening experiments of optimum proportioning.
Embodiment 3
Thermal power plant surveys the method for wherein octadecylamine concentration when checking and accepting purchased protection of boiler during shutdown period octadecylamine emulsion product.
(1) open drying box power supply and drying box is warmed up to 100 DEG C and constant temperature;
(2) three surface plate priority tap water and demineralized water cleaned up, put into the drying box that temperature is tuned to 105 ± 3 DEG C and be dried to constant weight, weigh after then putting into exsiccator cooling 30min, and be M by the quality record of three surface plates
10, M
20, M
30;
(4) purchased protection of boiler during shutdown period octadecylamine emulsion uniform application is dipped on surface plate with glass bar; the quality controlling octadecylamine emulsion on each surface plate with electronic scales is 7.3g; then weigh the quality of these 3 surface plates (containing octadecylamine emulsion) with electronic analytical balance, and be recorded as M
11, M
21, M
31;
(5) surface plate scribbling octadecylamine emulsion is put into the drying box to 90 DEG C or 100 DEG C of constant temperature together with pallet;
(6) dry 4h and to observe octadecylamine emulsion be achromaticity and clarification transparent colloidal time, take out pallet and surface plate put into exsiccator drying and be cooled to room temperature, then weigh with electronic analytical balance, and be recorded as M
13, M
23, M
33;
(7) calculate the weight percent concentration in solution to be measured in three surface plates respectively, get the concentration that namely its mean value obtain octadecylamine in octadecylamine emulsion.
Claims (2)
1. the assay method of an octadecylamine concentration, it is characterized in that: the solution to be measured freeze-day with constant temperature 1-10h under 70 ~ 110 DEG C of conditions taking certain mass, when solution to be measured is achromaticity and clarification transparent colloidal, be cooled to room temperature, the quality recorded respectively before solution drying to be measured is m
0, dried quality is m
1, according to formula (m
1/ m
0) × 100% can calculate the weight percent concentration in solution to be measured; Described solution to be measured is protection of boiler during shutdown period octadecylamine emulsion.
2. the assay method of octadecylamine concentration as claimed in claim 1, is characterized in that: the drying condition of described solution to be measured is dry 4h under 90 DEG C or 100 DEG C of conditions.
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| CN110239222A (en) * | 2019-05-31 | 2019-09-17 | 深圳市华星光电半导体显示技术有限公司 | Fill ink system |
| CN110805892A (en) * | 2019-11-13 | 2020-02-18 | 浙江浙能技术研究院有限公司 | Negative pressure waste heat drying maintenance method for waste heat boiler and steam turbine set |
| CN111886497A (en) * | 2018-04-03 | 2020-11-03 | 法玛通有限公司 | Method and apparatus for determining film-forming amines in liquids |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111886497A (en) * | 2018-04-03 | 2020-11-03 | 法玛通有限公司 | Method and apparatus for determining film-forming amines in liquids |
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