CN201397320Y - Experimental device for desorbing H2S and CO2 in alcohol amine solution - Google Patents

Experimental device for desorbing H2S and CO2 in alcohol amine solution Download PDF

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Publication number
CN201397320Y
CN201397320Y CN2009201060381U CN200920106038U CN201397320Y CN 201397320 Y CN201397320 Y CN 201397320Y CN 2009201060381 U CN2009201060381 U CN 2009201060381U CN 200920106038 U CN200920106038 U CN 200920106038U CN 201397320 Y CN201397320 Y CN 201397320Y
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tube
pipe
acid gas
gas desorption
acid
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颜晓琴
熊钢
常宏岗
何金龙
温崇荣
胡天友
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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Abstract

An experimental device for desorbing H2S and CO2 in alcohol amine solution is used for pretreatment before sample injection of gas chromatographic analysis and comprises an trapping tube, a drying tube, an acid gas desorption tube, a sintered glass plate, a solution control switch, a capillary tube and a reaction tube. The acid gas desorption tube is a vertical glass tube and is filled with strongly acid solution therein. The inner end of a vent glass tube is positioned inside the acid gas desorption tube and is vertically and upwardly bent. A glass tube is fixed at the top end of the acid gasdesorption tube and is connected with the reaction tube. Other glass tubes are fixed on the side wall of the top of the acid gas desorption tube and are both communicated with the top of a communicating cup and are communicated with the drying tube. The trapping tube is connected with the lower part of the drying tube. The experimental device has the effect that the acid solution in the acid gasdesorption tube can uniformly circulate inside the device. After connecting the trapping tube on the rear side of the acid gas desorption tube and the drying tube, the water mist and acid mist in thegas can be eliminated, so as to prevent a chromatographic column and a detector from being contaminated.

Description

H in the desorb alkanolamine solution 2S and CO 2Experimental provision
Technical field
The utility model relates to a kind of chemical analysis experimental provision, and the experimental provision that particularly a kind of gas chromatographic analysis sample introduction is used is used for the H of desorb hydramine desulfurization and decarburization solution 2S and CO 2, utilize its content of gas Chromatographic Determination.This device can cooperate gas chromatograph to be used for analyzing H dissimilar, the variable concentrations alkanolamine solution 2S and CO 2
Background technology
Alkanolamine solution is widely used in the H in the industrial gasses such as removing rock gas, refinery gas 2S and CO 2In the gas purification production run, device operator extremely is concerned about the CO in the amine liquid 2And H 2S content is because this is one of important monitoring parameter that guarantees product makings amount and device even running.Design one cover amine method desulfurization and decarburization device, for certain makings condition and treatment capacity, needing one of definite main technologic parameters is exactly the solution internal circulating load, and reasonably the solution internal circulating load just need be with H under the working condition 2S and CO 2Content in amine liquid is according to determining.In service at device as if makings condition generation marked change, also must be according to H under the New Terms 2S and CO 2Content in amine liquid redefines the solution internal circulating load.So,, measure H in the alkanolamine solution no matter be gas purification production or the design of amine method desulfurization and decarburization device 2S and CO 2Content all be crucial work.
At present, the sampling device of most of gas chromatographs all is by the mode that heats fluid sample to be gasified, and then brings the sample of gasification into chromatogram column analysis with carrier gas.The hydramine desulfurization and decarburization solution example because the mode of employing heating gasifies is not only with H 2S and CO 2Changed into gas, also the hydramine in the solution has been changed into gas, the boiling point of hydramine is all than higher (＞200 ℃), at H 2S and CO 2Analysis condition down can condensation and then pollute chromatographic column and chromatographic detector.If the temperature of chromatographic column and chromatographic detector is brought up to more than 200 ℃ H 2S and CO 2Detection sensitivity then can reduce greatly, can't detect the H of low content 2S and CO 2In view of red, orange, green, blue, yellow (ROGBY) has such limitation, oil and gas industry standard SY/T 6537 " Gas Purification Factory gas and liquor analysis method ", employing be that two kinds of chemical analysis methods are measured the H in the hydramine desulfurization and decarburization solution respectively 2S and CO 2Content, the accuracy of these two kinds of methods and precision all can satisfy the requirement of production and scientific research, but complicated operation, very time-consuming, and analyzing a sample approximately needs 1 hour, and some reducing substanceses can disturb H 2S and CO 2Determination on content causes measurement result inaccurate.
The utility model content
The purpose of this utility model is: H in a kind of desorb alkanolamine solution is provided 2S and CO 2Experimental provision, be implemented in the H that detects quickly and accurately on the chromatograph in the hydramine desulfurization and decarburization solution 2S and CO 2Content.Overcoming existing gas chromatographic sampling device all is by the mode that heats fluid sample to be gasified, and is not suitable for the H that analyzes in the alkanolamine solution 2S and CO 2SY/T 6537.13 " mensuration of hydrogen sulfide content in the desulfuration solution " and SY/T 6537.14 " mensuration of carbon dioxide content in the desulfuration solution ", and overcome reducing substances interference H 2S and CO 2Determination on content causes the inaccurate deficiency of measurement result.
The technical solution adopted in the utility model is: H in the desorb alkanolamine solution 2S and CO 2Experimental provision, comprise trap tube, drying tube, inlet, blow vent, tap hole, acid gas desorption pipe, sintering glass plate, solution gauge tap, kapillary, sample feeding mouth pipe and reaction tube.Sample feeding mouth pipe is the glass three-way pipe, and sample feeding mouth Guan Yiduan is an air intake opening, and carrier gas can enter by sample inlet tube.Sample feeding mouth Guan Yiduan is connected with kapillary by the rubber connecting pipe.The other end capillaceous is in series with second kapillary by rubber connecting pipe, glass tube, solution gauge tap.Second other end capillaceous is connected with the cloche that has sintering glass plate in the acid gas desorption pipe by glass tube.The acid gas desorption pipe is upright glass tube, in the acid gas desorption pipe strong acid solution is housed.Tap hole is arranged at the bottom at the acid gas desorption pipe, and the rubber connecting pipe is arranged on the tap hole, and the rubber connecting pipe can be pricked and be bolted.A glass tube and cup UNICOM of UNICOM are arranged at the top of acid gas desorption pipe.Be fixed with a blow vent glass tube on acid gas desorption pipe top, there is the rubber connecting pipe outer end of blow vent glass tube, and the rubber connecting pipe can be pricked and be bolted.Bend in the acid gas desorption pipe and vertically upward the inner of blow vent glass tube.Be fixed with glass tube on the top of acid gas desorption pipe and be connected with reaction tube, the other end of reaction tube is connected with the glass three-way pipe of injection port pipe.On the sidewall at acid gas desorption pipe top, be fixed with glass tube, glass tube by the rubber connecting pipe respectively with the top UNICOM of UNICOM's cup, with drying tube UNICOM.The bottom of drying tube is connected with trap tube.Carrier gas is carried sample by trap tube, can enter chromatograph.Be fixed with an inlet at the top of UNICOM's cup, can be UNICOM's cup and acid gas desorption pipe liquid make-up.
Desiccant-filled in the drying tube, as phosphorus pentoxide, lime chloride, silica gel, scribble the Chromosorb G/AW (ChromosorbG/AW) of phosphoric acid.
Fill the chemical powder that captures acid mist in the trap tube, chemical powder comprises sodium bicarbonate, sodium tetraborate.
In the acid gas desorption pipe strong acid solution is housed, strong acid solution comprises that massfraction is 10%～50% phosphoric acid solution, sulfuric acid solution or hydrochloric acid solution.
The acid gas desorption pipe is provided with inlet, tap hole and blow vent; In the acid gas desorption pipe strong acid solution is housed.When in the acid gas desorption pipe, adorning acid solution, earlier tap hole is clamped with the stainless steel folder, open inlet and blow vent, with glass syringe acid solution is slowly injected in the desorption pipe then and (should be put on the protective gloves of acid corrosion-resistant when injecting acid solution), the loading height of acid solution as shown in Figure 1.Change once the acid solution half a year in the desorption pipe, opens inlet and blow vent during replacing and earlier old solution is emitted, again by the above-mentioned steps new soln of packing into.When not changing solution, inlet, blow vent and tap hole are all used the stainless steel folder and are clamped.
Before the sample analysis, should check inlet, blow vent, tap hole, sample feeding mouth pipe (11), and whether each junction leak gas, and get rid of the gas leakage situation.
During analytic sample, the solution gauge tap should be in open mode; If analytic sample not clamps the solution gauge tap with the stainless steel folder for a long time.
The utlity model has following function:
That this experimental provision and chromatograph coupling can be measured is dissimilar, the H in the variable concentrations alkanolamine solution 2S content and CO 2Content.
The beneficial effects of the utility model: H in the utility model desorb alkanolamine solution 2S and CO 2Experimental provision with after chromatographic carrier gas is connected, the acid solution in the acid gas desorption pipe can circulate in device evenly.The trap tube and the drying tube that are connected behind the acid gas desorption pipe can be removed water smoke in the gas and acid mist, guarantee that thus chromatographic column and detecting device are not contaminated.
The chromatogram analysis method that adopts this experimental provision and chromatograph coupling to set up, simple to operate; Measurement range is wide, can measure the CO of mass ratio greater than 1ppm 2And H 2S; Analysis time is short, can finish sample analysis in five minutes one time; Disturb for a short time, can not be subjected to the interference of other component in the sample solution.
H in the desorb alkanolamine solution 2S and CO 2Experimental provision, can satisfy and produce and the needs of scientific research, detect the H in the alkanolamine solution quickly and accurately 2S and CO 2Content.The sampling device of this device as chromatogram is connected with chromatograph.The acid gas desorption pipe in strong acid solution is housed, behind the sample access to plant, the hydramine in the sample and acid reaction generate salt, dissolve and are strapped in H in the alkanolamine solution 2S and CO 2Under this strong acidic condition, desorbed.The H that desorbs 2S and CO 2, the reaction salt and the acid solution that generate, these gas-liquid mixtures in device can because of action of gravity through twice gas-liquid separation, liquid (comprising salt that acid solution, reaction generate and the water in the sample) turns back in the acid solution in the device, and gas (comprises H 2S, CO 2And carrier gas) enters chromatographic column analysis.The chromatogram analysis method that adopts this device and chromatograph coupling to set up, simple to operate, can in five minutes, finish one time sample analysis, shortened sample analysis time greatly, and H 2S and CO 2Mensuration can not be subjected to the interference of other component in the sample.
Description of drawings
Fig. 1 is H in the desorb alkanolamine solution 2S and CO 2The structural representation of experimental provision.
Among the figure, 1. trap tube, 2. drying tube, 3. connecting pipe, 4. inlet, 5. blow vent, 6. tap hole, 7. acid gas desorption pipe, 8. sintering glass plate, 9. solution gauge tap, 10. kapillary, 11. sample feeding mouth pipes, 12. reaction tubes.
Embodiment
Embodiment 1: with H in the desorb alkanolamine solution 2S and CO 2Experimental provision be example, the utility model is described in further detail.
Consult Fig. 1.H in the desorb alkanolamine solution 2S and CO 2Experimental provision, be a kind of glass apparatus, comprise trap tube 1, drying tube 2, inlet 4, blow vent 5, tap hole 6, acid gas desorption pipe 7, sintering glass plate 8, solution gauge tap 9, kapillary 10, sample feeding mouth pipe 11 and reaction tube 12.Sample feeding mouth pipe 11 is that internal diameter is 5 millimeters a glass three-way pipe, and it is air intake opening that the sample feeding mouth is managed 11 1 ends, and carrier gas can enter by sample inlet tube 11.The sample feeding mouth is managed 11 1 ends and is connected with kapillary 10 by rubber connecting pipe 3.The other end of kapillary 10 is in series with second kapillary 10 by rubber connecting pipe 3, glass tube, solution gauge tap 9.The other end of second kapillary 10 is connected by the cloche that has sintering glass plate 8 in glass tube and the acid gas desorption pipe 7.Acid gas desorption pipe 7 is upright glass tube, and the diameter of acid gas desorption pipe 7 is 25 millimeters, height 270 millimeter.In the acid gas desorption pipe 7 strong acid solution is housed.In the bottom of acid gas desorption pipe 7 tap hole 6 is arranged, rubber connecting pipe 3 is arranged on the tap hole 6, rubber connecting pipe 3 can be pricked and be bolted.A glass tube and cup UNICOM of UNICOM are arranged at the top of acid gas desorption pipe 7.30 millimeters of the diameters of glass UNICOM cup, 80 millimeters of height.Be fixed with blow vent 5 glass tubes on acid gas desorption pipe 7 tops, there is rubber connecting pipe 3 outer end of blow vent 5 glass tubes, and rubber connecting pipe 3 can be pricked and be bolted.Bend in acid gas desorption pipe 7 and vertically upward the inner of blow vent 5 glass tubes.Be fixed with glass tube on the top of acid gas desorption pipe 7 and be connected with reaction tube 12, the other end of reaction tube 12 is connected with the glass three-way pipe of injection port pipe 11.On the sidewall at acid gas desorption pipe 7 tops, be fixed with glass tube, glass tube by rubber connecting pipe 3 respectively with the top UNICOM of UNICOM's cup, with drying tube 2 UNICOMs.The bottom of drying tube 2 is connected with trap tube 1.Be fixed with an inlet 4 at the top of UNICOM's cup.
The drying agent of 2 li fillings of drying tube is phosphorus pentoxides.
Filling the chemical powder that captures acid mist in the trap tube 1 is sodium bicarbonate.
In the acid gas desorption pipe 7 strong acid solution is housed, strong acid solution is that massfraction is 10%～50% sulfuric acid solution.
By shown in Figure 1 connect experimental provision after, press SY/T 6537.8 " H in the gas purifying technique process gas 2S and CO 2Determination on content (vapor-phase chromatography) " the setting chromatographiccondition.After opening solution gauge tap 9, the acid solution in the acid gas desorption pipe 7 can flow to the carrier gas inlet place by sintering glass plate 8, kapillary 10 successively, and upwards arrives reaction tube 12 through sample inlet tube 11 with carrier gas.Inject sample 10 microlitres with syringe at sample inlet tube 11, sample enters reaction tube 12 and fully reacts the H in the sample at this and acid solution with carrier gas 2S and CO 2From solution, desorb, and, enter chromatographic column analysis at last along with carrier gas enters trap tube 1, drying tube 2 successively; Hydramine, water and acid solution then flow back in the acid solution in the acid gas desorption pipe 7 in the sample.
Under assigned temperature, investigate H 2S, CO 2Dividing potential drop and H 2S, CO 2The relation of solubleness in alkanolamine solution.H 2S, CO 2Solubleness in alkanolamine solution adopts chromatography and chemical determination simultaneously.The measurement result of chromatography and chemical method is consistent as can be seen from table 1 and table 2.H according to these experimental datas works 2S dividing potential drop and H 2Graph of a relation, the CO of S solubleness in alkanolamine solution 2Dividing potential drop and CO 2The graph of a relation of solubleness in alkanolamine solution, all with data on curve map coincide.
The equilibrium solubility experimental data of table 1 carbon dioxide in the sulfone amine aqueous solution
CO 2Dividing potential drop (kPa) CO in the desulfurization of chromatography determination 2Content (mol/mol) CO in the desulfurization of chemical determination 2Content (mol/mol)
3.212 0.02376 0.02377
8.444 0.05416 0.05413
18.076 0.0836 0.0830
39.275 0.1432 0.1439
57.011 0.2205 0.2210
132.262 0.3096 0.3095
161.017 0.4015 0.4017
235.88 0.4998 0.4990
323.593 0.5503 0.5507
409.384 0.6062 0.6070
537.007 0.6646 0.6648
Table 2 H 2The equilibrium solubility experimental data of S in certain desulfuration solution
Hydrogen sulfide sectional pressure (kPa) H in the desulfurization of chromatography determination 2S content (mol/mol) H in the desulfurization of chemical determination 2S content (mol/mol)
2.138 0.0317 0.0314
1.749 0.0325 0.0323
14.674 0.1365 0.1371
39.035 0.3297 0.3289
84.341 0.5079 0.5076
215.346 0.8121 0.8125
320.198 0.9291 0.9288
463.121 1.0831 1.0830
537.804 1.1404 1.1400
577.995 1.2328 1.2322
589.784 1.2323 1.2327
。

Claims (1)

1, H in a kind of desorb alkanolamine solution 2S and CO 2Experimental provision, comprise trap tube (1), drying tube (2), inlet (4), blow vent (5), tap hole (6), acid gas desorption pipe (7), sintering glass plate (8), solution gauge tap (9), kapillary (10), sample feeding mouth pipe (11) and reaction tube (12), sample feeding mouth pipe (11) is the glass three-way pipe, sample feeding mouth pipe (11) one ends are air intake opening, it is characterized in that: sample feeding mouth pipe (11) one ends are connected with kapillary (10) by rubber connecting pipe (3), the other end of kapillary (10) is by rubber connecting pipe (3), glass tube, solution gauge tap (9) is in series with second kapillary (10), the other end of second kapillary (10) is connected by the interior cloche that has sintering glass plate (8) of glass tube and acid gas desorption pipe (7), acid gas desorption pipe (7) is upright glass tube, the acid gas desorption pipe is equipped with strong acid solution in (7), in the bottom of acid gas desorption pipe (7) tap hole (6) is arranged, rubber connecting pipe (3) is arranged on the tap hole (6), rubber connecting pipe (3) can be pricked and be bolted, a glass tube and cup UNICOM of UNICOM are arranged at the top of acid gas desorption pipe (7), be fixed with a blow vent (5) glass tube on acid gas desorption pipe (7) top, there is rubber connecting pipe (3) outer end of blow vent (5) glass tube, bend in acid gas desorption pipe (7) and vertically upward the inner of blow vent (5) glass tube, be fixed with glass tube is connected with reaction tube (12) on the top of acid gas desorption pipe (7), the other end of reaction tube (12) is connected with the glass three-way pipe of injection port pipe (11), on the sidewall at acid gas desorption pipe (7) top, be fixed with glass tube, glass tube by rubber connecting pipe (3) respectively with the top UNICOM of UNICOM's cup, with drying tube (2) UNICOM, the bottom of drying tube (2) is connected with trap tube (1), is fixed with an inlet (4) at the top of UNICOM's cup.
CN2009201060381U 2009-03-04 2009-03-04 Experimental device for desorbing H2S and CO2 in alcohol amine solution Expired - Lifetime CN201397320Y (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103185755A (en) * 2011-12-28 2013-07-03 中国石油天然气股份有限公司 Sample pre-treatment device for analyzing anions in alkanolamine solution
CN103185756A (en) * 2011-12-28 2013-07-03 中国石油天然气股份有限公司 Sample pretreatment method for analysis of anions in alkanolamine solution
CN107621449A (en) * 2017-02-13 2018-01-23 中国石油天然气股份有限公司 CO in a kind of gas purification amine liquid2The Continuous Flow Analysis method of content
CN113049332A (en) * 2021-03-19 2021-06-29 中海石油化学股份有限公司 Analytical determination method for chromium ions in pre-decarbonization liquid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103185755A (en) * 2011-12-28 2013-07-03 中国石油天然气股份有限公司 Sample pre-treatment device for analyzing anions in alkanolamine solution
CN103185756A (en) * 2011-12-28 2013-07-03 中国石油天然气股份有限公司 Sample pretreatment method for analysis of anions in alkanolamine solution
CN103185756B (en) * 2011-12-28 2014-06-04 中国石油天然气股份有限公司 Sample pretreatment method for analysis of anions in alkanolamine solution
CN103185755B (en) * 2011-12-28 2014-06-04 中国石油天然气股份有限公司 Sample pre-treatment device for analyzing anions in alkanolamine solution
CN107621449A (en) * 2017-02-13 2018-01-23 中国石油天然气股份有限公司 CO in a kind of gas purification amine liquid2The Continuous Flow Analysis method of content
CN107621449B (en) * 2017-02-13 2020-12-01 中国石油天然气股份有限公司 CO in gas purification amine liquid2Continuous flow analysis method of content
CN113049332A (en) * 2021-03-19 2021-06-29 中海石油化学股份有限公司 Analytical determination method for chromium ions in pre-decarbonization liquid
CN113049332B (en) * 2021-03-19 2022-09-27 中海石油化学股份有限公司 Analytical determination method for chromium ions in pre-decarbonization liquid

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C14 Grant of patent or utility model
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Assignee: Chengdu Tianke Oil and Gas Engineering Co.,Ltd.

Assignor: China Petroleum & Natural Gas Co., Ltd.

Contract record no.: 2011510000221

Denomination of utility model: Experimental device for desorption of H[sub]2[/sub]S and CO[sub]2[/sub] in ethanolamine solution

Granted publication date: 20100203

License type: Exclusive License

Record date: 20110828

CX01 Expiry of patent term
CX01 Expiry of patent term

Granted publication date: 20100203