CN106370776B - A method of the uptake for detecting ethanol amine absorbing carbon dioxide - Google Patents
A method of the uptake for detecting ethanol amine absorbing carbon dioxide Download PDFInfo
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- CN106370776B CN106370776B CN201610756954.4A CN201610756954A CN106370776B CN 106370776 B CN106370776 B CN 106370776B CN 201610756954 A CN201610756954 A CN 201610756954A CN 106370776 B CN106370776 B CN 106370776B
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- Prior art keywords
- carbon dioxide
- ethanol amine
- caco
- sodium hydroxide
- absorbing carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Abstract
The present invention relates to a kind of methods for detecting the uptake of ethanol amine absorbing carbon dioxide, absorbing carbon dioxide is removed by multistage sodium hydroxide, to the last level-one calcium chloride titration does not occur turbidity and precipitation or muddy especially small, then it is precipitated again with excess calcium chloride solution, finally the sediment CaCO to obtaining3Carry out calculating of weighing.The carbon dioxide absorption amount of ethanol amine can with accurate stable be measured by multistage detection titration.This multistage sodium hydroxide is apparent and smaller by gravimetry error in the method measurement effect of test in laboratory ethanol amine absorbing carbon dioxide uptake, and experimental result is stable and accurate.
Description
Technical field
The present invention relates to boiler smoke carbon dioxide absorptions and detecting system field, specifically, being related to a kind of for more
Sodium hydroxide absorbs the carbon dioxide that ethanol amine does not fully absorb to detect ethanol amine absorption efficiency.
Background technology
Currently, in view of its harmfulness of carbon dioxide gas and utility value, seem particularly to the detection of CO2 emission
It is important, effective etection theory and method are further explored, and develop the detection device adapted at this stage also to seem extremely important.Though
So with the rapid development of computer technology, microelectric technique, gas concentration lwevel detection is gradually intelligent, integrated, still
Detect the branches of learning comprehensive applications such as core or chemistry, physics, electricity.
The measurement method of common carbon dioxide absorption amount has vascular unloading technique, gravimetric method and gas chromatography.Constant appearance
Area method is also known as coprecipitation, by product medicament and carrier material co-dissolve in organic solvent, after distillation removal organic solvent
Medicament is set to be precipitated simultaneously with carrier material, you can the co-precipitate that medicament is mixed with carrier material to be obtained, through being drying to obtain.
Gas chromatography is to use gas as mobile phase, and in the chromatography column, different samples is because with different physics and chemically
Matter is had different interactions from specific column packing and is driven with different rates by air-flow.When gas is from the end of column
When the outflow of end, it is detected by the detector, generates corresponding signal, and be converted into electric signal output.
Carbon dioxide absorption amount vascular unloading technique measures big, of high cost and organic using consumption of organic solvent at present
Solvent is difficult to completely remove to the greatest extent.Although it is preferable that gas chromatography detects carbon dioxide opposing gas method, in some conditions
In the laboratory of relative mistake, it is difficult to there is such a precision instrument to remove detection gas concentration lwevel, so needing to seek its other party
Method goes to measure carbon dioxide absorption amount.
Invention content
Technical problems to be solved
The efficiency of ethanol amine absorbing carbon dioxide can be detected in order to reduce experimentation cost, overcome laboratory existing without essence
Close carbon dioxide detector and the problem of can realize minimal error detection, the present invention proposes a kind of to absorb dioxy for ethanol amine
Change the multistage detection method of carbon.
Technical solution
A method of the uptake for detecting ethanol amine absorbing carbon dioxide, it is characterised in that steps are as follows:
Step 1:Carbonated mixed gas is passed through in ethanolamine solutions and is absorbed, the Ventilation Rate of carbon dioxide is
Q, duration of ventilation t;The ethanolamine solutions mass percent is 10~40%, 30~60 DEG C of temperature;
Step 2:Mixed gas after ethanol amine is absorbed, which is passed through successively in multistage sodium hydroxide solution, to be absorbed, respectively toward hydrogen
Excess chlorination calcium solution is instilled in solution after sodium oxide molybdena absorption to be precipitated, and air is completely cut off after precipitation and stands 30 minutes;It is described
Sodium hydroxide volumetric concentration be 0.1~0.2mol/L, temperature be 35~45 DEG C;The volumetric concentration of the calcium chloride solution
For 0.5~1mol/L;
Step 3:Supernatant liquid after standing is outwelled, in sediment CaCO3Middle addition distilled water isolation air stands 30
Minute outwells supernatant liquid;This step is repeated repeatedly until after distilled water is added, isolation air stands 5-10 minutes, supernatant liquid
There is not muddiness;
Step 4:To sediment CaCO3It is washed after being filtered, then heating is evaporated, and being down to room temperature after being evaporated is claimed
Amount;
Step 5:Calculating the carbon dioxide quality that sodium hydroxide solution absorbs is:
Wherein, m (CaCO3) it is every grade of sediment CaCO generated3Quality, M (CaCO3) it is CaCO3Molal weight, M
(CO2) it is CO2Molal weight;
Step 6:Calculating ethanol amine absorbing carbon dioxide quality is:
Wherein,For the gross mass of carbon dioxide, m1、m2、mnThe respectively first order, the second level, n-th
The carbon dioxide quality that sodium hydroxide solution absorbs.
The selection principle of multistage sodium hydroxide solution in step 2 is that afterbody sodium hydroxide solution is dripped using calcium chloride
It is fixed turbidity and precipitation do not occur.
Advantageous effect
A kind of multistage detection method for ethanol amine absorbing carbon dioxide proposed by the present invention, passes through multistage sodium hydroxide
Absorbing carbon dioxide is removed, to the last level-one calcium chloride titration does not occur turbidity and precipitation or muddy especially small, ensures error
No more than 0.5%, show that carbon dioxide has been fully absorbed by multistage sodium hydroxide.It can be with accurate stable by multistage detection titration
Measure the carbon dioxide absorption amount of ethanol amine in ground.
Meanwhile the uptake of ethanol amine absorbing carbon dioxide, hydrogen-oxygen are detected with multistage sodium hydroxide absorbing carbon dioxide method
The source limitation for changing sodium absorbent is relatively small, is readily transported, stores.There is no absorbents to volatilize and ammonia mist is asked in washing process
Topic;Multistage test experience device is not likely to produce structure blockage problem, moreover, compared with other absorbents, soda abundance and
And it is cheap;The absorbability of soda absorbent is big, and dosage is few, and absorption efficiency is higher.This multistage sodium hydroxide is being tested
The method measurement effect that ethanol amine absorbing carbon dioxide uptake is detected in room is apparent and smaller by gravimetry error,
Experimental result is stable and accurate.
Description of the drawings
The hierarchical detection experimental provision schematic diagram of Fig. 1 ethanol amine absorbing carbon dioxides
In figure:
1 nitrogen gas cylinder, 2 dioxide bottle 3 carries the mixer of gas flowmeter
4 thermometer, 5 three-necked flask, 6 thermostat water bath
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described:
The multistage detection method of ethanol amine absorbing carbon dioxide is as follows:
In order to make experiment there is apparent phenomenon, the time that mixed gas is passed through to be set as t, wherein the ventilation speed of carbon dioxide
Rate is q.
Wherein ethanol amine absorbs CO2Reaction mechanism it is as follows:
2HOC2H4NH2+H2O+CO2——→(HOC2H4NH3)2CO3 (1)
But according to the reaction mechanism of ethanolamine solutions absorbing carbon dioxide, the detection method of product is relatively very complicated.Institute
With by this method by multistage sodium hydroxide behind absorption plant, the reaction mechanism of sodium hydroxide absorbing carbon dioxide is as follows:
2NaOH+CO2=Na2CO3+H2O (2)
This method mainly determines the uptake of carbon dioxide using gravimetric method, i.e., by the solution after absorbing carbon dioxide into
Row precipitation weighs the quality of deposit, then the quality of precipitation is become CO by the principle conversion of the conservation of matter2Quality.
This method is using calcium chloride solution to absorbing CO2Solution afterwards is titrated, and titration mechanism is as follows:
CaCl2+Na2CO3=Ca C3O↓+2Na Cl (3)
According to conservation of mass principle, then the carbon dioxide quality that sodium hydroxide solution absorbs is:
In logical carbon dioxide time t, the carbon dioxide gross mass being passed through is:
The carbon dioxide quality that multistage sodium hydroxide absorbs is calculated according to formula (4) and is recorded as m respectively1、m2、
m3、……、mn, according to the CO of poor quality for calculating ethanolamine solutions absorption2Quality, Computing Principle is:
Embodiment 1:With a concentration of 10% ethanol amine at a temperature of 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C absorbing carbon dioxide,
This experiment uses hierarchical detection, experiment implementation steps as follows.
(1) in conjunction with attached drawing 1, experimental provision connection is finished according to experimental provision schematic diagram, and the gas of test experience device
Whether close property is good;
(2) control valve of nitrogen gas cylinder and dioxide bottle is opened, it is respectively 3.6L/min and 0.6L/ to adjust its flow velocity
Min simulates the gas for being closer to flue gas composition in the lab, and a period of time of ventilating excludes the sky in experimental provision
Gas;
(3) the control switch of water-bath is opened, the temperature for adjusting water-bath is heated to set temperature value;
(4) ethanolamine solutions of certain volume are added into first three-necked flask, to second and three mouthfuls of third
300mL sodium hydroxide solutions are added in flask and are recorded as the first order and the second level, connects experimental provision, makes carbon dioxide and nitrogen
Gas is passed through in the three-necked flask equipped with ethanolamine solutions by the mixing of gas to react, duration of ventilation 5min;
(4) after reaction time 5min, the rubber stopper for taking out three-necked flask stops reaction, is then shut off gas cylinder control valve;
(5) by the sodium hydroxide absorbing liquid in the first order and second level three-necked flask be transferred to weighed quality and record
In beaker, prepared excess chlorination calcium solution in advance is added into the beaker and is precipitated, beaker preservative film is sealed anti-
Only it is contacted with air, stands 30 minutes;
Beaker is opened after (6) 30 minutes, the supernatant in beaker is poured out, enough distilled water is added into beaker again with guarantor
Fresh film seals beaker, stands 30 minutes;
(7) it repeats step (6) repeatedly, pours out supernatant, washing is filtered with filter paper to the sediment in beaker, then
By filtered filter paper, it is placed in curer and carries out heating and be evaporated, wait in filter paper that sediment temperature is down to room temperature progress after being evaporated
It weighs and records data such as table 1;
(8) step (1)~(7) are repeated to be tested three times;
1 ethanol amine of table absorbs CO2Experimental data
The matter for the carbon dioxide that sodium hydroxide absorbs at different temperatures can be calculated separately out according to formula (4) and formula (6)
The quality for the carbon dioxide that amount and ethanol amine absorb, result of calculation record such as table 2.
The quality for the carbon dioxide that 10% ethanol amine absorbs under 2 different temperatures of table
Claims (1)
1. a kind of method for detecting the uptake of ethanol amine absorbing carbon dioxide, it is characterised in that steps are as follows:
Step 1:Carbonated mixed gas is passed through in ethanolamine solutions and is absorbed, the Ventilation Rate of carbon dioxide is q, is led to
The gas time is t;The ethanolamine solutions mass percent is 10~40%, 30~60 DEG C of temperature;
Step 2:Mixed gas after ethanol amine is absorbed, which is passed through successively in multistage sodium hydroxide solution, to be absorbed, respectively toward hydroxide
Excess chlorination calcium solution is instilled in solution after sodium absorption to be precipitated, until afterbody sodium hydroxide solution uses calcium chloride
There is not turbidity and precipitation in titration;Completely cut off air after precipitation and stands 30 minutes;The volumetric concentration of the sodium hydroxide be 0.1~
0.2mol/L, temperature are 35~45 DEG C;The volumetric concentration of the calcium chloride solution is 0.5~1mol/L;
Step 3:Supernatant liquid after standing is outwelled, in sediment CaCO3Middle addition distilled water isolation air stands 30 minutes and falls
Fall supernatant liquid;This step is repeated repeatedly until after distilled water is added, isolation air stands 5-10 minutes, and supernatant liquid does not occur
It is muddy;
Step 4:To sediment CaCO3It is washed after being filtered, then heating is evaporated, and being down to room temperature after being evaporated is weighed;
Step 5:Calculating the carbon dioxide quality that sodium hydroxide solution absorbs is:
Wherein, m (CaCO3) it is every grade of sediment CaCO generated3Quality, M (CaCO3) it is CaCO3Molal weight, M (CO2)
For CO2Molal weight;
Step 6:Calculating ethanol amine absorbing carbon dioxide quality is:
Wherein,For the gross mass of carbon dioxide, m1、m2、mnThe respectively first order, the second level, n-th grade of hydrogen-oxygen
Change the carbon dioxide quality that sodium solution absorbs.
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CN112539978A (en) * | 2020-12-17 | 2021-03-23 | 三门核电有限公司 | Method for obtaining absorption efficiency of nuclear island chimney C-14 sampling device of nuclear power station |
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CN103097000A (en) * | 2010-07-20 | 2013-05-08 | 鲍尔斯潘公司 | Absorption media for scrubbing co2 from a gas stream and methods using the same |
CN102350368A (en) * | 2011-06-22 | 2012-02-15 | 河北科技大学 | Potassium carbonate solution based catalytic system used for removing CO2 in fume |
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