CN107462669A - A kind of amine liquid for desulphurization sparger and method - Google Patents
A kind of amine liquid for desulphurization sparger and method Download PDFInfo
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- CN107462669A CN107462669A CN201610391287.4A CN201610391287A CN107462669A CN 107462669 A CN107462669 A CN 107462669A CN 201610391287 A CN201610391287 A CN 201610391287A CN 107462669 A CN107462669 A CN 107462669A
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- China
- Prior art keywords
- desulphurization
- amine liquid
- experiment
- cup
- kuppe
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- 239000007788 liquid Substances 0.000 title claims abstract description 47
- 150000001412 amines Chemical class 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title description 8
- 238000002474 experimental method Methods 0.000 claims abstract description 41
- 238000009826 distribution Methods 0.000 claims abstract description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 47
- 239000006260 foam Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 13
- 238000011156 evaluation Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000011109 contamination Methods 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims 1
- 238000005187 foaming Methods 0.000 description 18
- 101100441413 Caenorhabditis elegans cup-15 gene Proteins 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 4
- 230000023556 desulfurization Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- -1 amine salt Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 235000019157 thiamine Nutrition 0.000 description 1
- 150000003544 thiamines Chemical class 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a kind of amine liquid for desulphurization sparger,For determining,Assess petrochemical industry specialty amine liquid for desulphurization frothing capacity,It has disclosed exhaust outlet,And it is provided centrally with gas distribution head connecting rod,There is a cylinder type kuppe,The iron hoop that the A-frame that kuppe is set by the closely upper head end of connecting rod supports is installed on middle part in experiment cup,One gas distribution head kept flat is set at link end,Kuppe top surface opens wide with bottom surface,Gas distribution head is in kuppe center and is mutually not in contact with each other,Flowermeter of the gas distribution head connecting rod other end to outside experiment cup is connected,The side in experiment bottom of a cup portion is provided with the port that sample inlet and outlet device pipe are led,Experiment cup top is provided with constant temperature and humidity gas blowout head,Top of piece constant temperature and humidity gas inlet tube into experiment cup is set at experiment cup lower through-ports,The described constant temperature and humidity gas inlet tube connection flow gauge and pressure gauge to outside experiment cup.
Description
Technical field
The invention belongs to petroleum chemical industry laboratory analytical instrument, for determining, assessing desulfurization
The device of amine liquid frothing capacity, the invention further relates to tote-box of factory's research and development etc..
Background technology
Methyl diethanolamine (MDEA) is widely used in petroleum refining sulfur removal technology as desulfurizing agent,
Its aqueous solution, i.e. amine liquid for desulphurization, in use, due to bringing impurity or mass change into
Etc. factor, easily cause situations below：(1) amine liquid for desulphurization foaming, race damage, cause economic damage
Lose, increase production cost；(2) increase desulfurizer and run unstable factor, accumulate potential safety hazard,
Even trigger work safety accident；(3) desulfurized effect is reduced, causes the hydrogen sulfide content of product
It is exceeded.
At present, domestic and international amine liquid for desulphurization frothing capacity measure is mainly used in petroleum gas, oil
Chemical industry and Utilities Electric Co., but without unified execution standard.Petroleum chemical industry or electricity
Power company is substantially the method provided using amine liquid for desulphurization manufacturer and is measured, that is, is used
Nitrogen makes amine liquid for desulphurization be bubbled in foaming tube by gas distribution head, determines at the appointed time
Foaming height and foam time, but do not do related rule for the parameters in assay method
It is fixed.In oil and gas industry, although having formulated foam performance measure relevant criterion SY/T
6538-2002 " Compound Type Selective Desulfurization Solvent ", but also not to the items in continuous mode
Specification index does clear stipulaties, and it is to be limited to 30 DEG C of constant temperature to test, amine liquid for desulphurization quality point
Number is carried out under conditions of being 40%.In existing patent, gas distribution head typically uses glass
Core makes, and because the micro-pore diameter of glass core, quantity and distribution are uncontrollable, causes gas
Distribution head individual difference is big, and experimental repeatability is poor, and glass material is easily by the desulfurization amine of alkalescence
Corrosion, gas distribution head is caused to be damaged.Certain difference be present using method in above-mentioned industry,
But during actual analysis, problems be present：(1) gas distribution head, is not provided
Make material, specification and performance rating standard；(2), formed using raw glass grains of sand sintering
Gas distribution head, individual between size heterogeneity it is big；(3), glass microporous is easily dirty by amine liquid for desulphurization
Dye and corrosion, and be difficult to clean, repair；(4), do not consider that ambient temperature and humidity produces to foam
With shattered to pieces influence.Above mentioned problem, causes that experimental accuracy is low, poor repeatability, unfavorable
The running status of amine liquid for desulphurization is accurately monitored in desulfurizer operating personnel.
The content of the invention
It is an object of the invention to provide a kind of amine liquid for desulphurization sparger and method, and it is steady to be formed
Determine the frothing capacity of the minimum nitrogen flow evaluation amine liquid for desulphurization of hemispherical foam, stable foam
State is reproducible, and the degree of accuracy is high, can be that desulfurizer operating personnel monitor amine liquid for desulphurization operation
State provides accurate analyze data.
The technical solution of the present invention is that have an experiment cup with a scale, and experiment cup is using saturating
Bright resistant material is made, and bottom is circular arc, and top is cylinder open container, there is lid,
There is exhaust outlet at the center of lid, and be provided centrally with gas distribution head connecting rod, there is a cylinder type
Kuppe, the iron hoop that the A-frame that kuppe is set by the closely upper head end of connecting rod supports are installed on
Middle part in cup is tested, a gas distribution head kept flat, kuppe top are set at link end
Face is opened wide with bottom surface, and gas distribution head is in kuppe center and is mutually not in contact with each other, the gas
Flowermeter of the distribution head connecting rod other end to outside experiment cup is connected, and one in experiment bottom of a cup portion
Side is provided with the port that sample inlet and outlet device pipe are led, and experiment cup top is provided with constant temperature
Constant humidity gas blowout head, a constant temperature and humidity gas inlet tube is set at experiment cup lower through-ports to experiment
Top in cup, the described constant temperature and humidity gas inlet tube connection flow gauge and pressure to outside experiment cup
Table.
Gas distribution head described above is that special material is diameter 15mm, thick 0.2mm, material
For 316L stainless steel disk thin slices, through-hole diameter 0.15mm；Through hole is distributed as from the inside to surface,
Number is followed successively by 3,4,8,8 totally 23；2,5,8,11 are followed successively by for circular diameter；Institute
There is hole laser boring.
Inventive flow counter device is to load onto high-flow meter respectively at four-way connection, middle flow
Meter, Low-flow meter.
Sample inlet and outlet device described above are in the three-pronged connector both sides punishment for having switch
Sample inlet pipe, sample export pipe are not loaded onto.
The present invention is that the air nozzle that goes out of constant temperature and humidity gas blowout head is the hole on annulus tubulose.
Above inventive desulfurization amine liquid frothing capacity evaluation method, stable half is formed on kuppe
The minimum of spherical foam advertises the frothing capacity of nitrogen flow evaluation amine liquid for desulphurization, hemispherical foam
Formed, do not contacted with other solid matters above kuppe upper surface, surface tension can be avoided
With the interference of surface contamination, repeat experiment more preferable.
The present invention operation principle be：It is real that the present invention devises a set of brand-new amine liquid for desulphurization foaming
Experiment device.Wherein, the gas distribution head as core component, made using laser boring,
With particular via diameter, quantity and the stainless steel disk of distribution thin slice, corrosion-resistant, easy cleaning
And individual difference is small, the repeatability of experiment can be ensured.Gas distribution head and the plastics with lid
The foaming experimental situation that cup forms closing is tested, gas is advertised and is introduced from experiment bottom of a cup portion, outfit
Different range flow meters can switch easily, make the optional scope of gas flow wider, be easy to measure not
With the horizontal amine liquid for desulphurization of foaming；Experiment cup top is passed through the nitrogen after outside Constant Temperature and Humidity Chambers processing
Gas, reach the purpose of control foaming ambient temperature and humidity, reduce foaming experiment interference factor, make reality
Test reproducible, result stabilization.In addition, the present invention is no longer with foaming height and foam time,
But to form the foaming characteristic that the minimum nitrogen flow of stable hemispherical foam evaluates amine liquid for desulphurization
Can, stable foam state makes experimental repeatability more preferable.
Foam refers to the scattered dispersion in a liquid of gas.Foam, which produces, needs two bars
Part, first, continuously gas is fully filled with into liquid, second, expansion rate is higher than brokenly bubble speed.
Fresh, clean amine liquid for desulphurization (aqueous alkanolamine), due to lacking surface reactive material, bubble
Foam is not likely to produce, and is also easy to vanish even if producing, thus bubble problem is not present.But
In sweetening process, as organic amine salt is formed, aliphatic acid, fatty alcohol and organic salt etc. are miscellaneous
Matter is accumulated, and surface reactive material gradually increases in amine liquid for desulphurization, not only make foaming become it is easy and
And expansion rate exceedes brokenly bubble speed, so as to cause amine liquid for desulphurization easily to produce foam.
The amine liquid for desulphurization foaming experimental provision and method that the present invention designs, with nitrogen as foam cone
Blow, after flowmeter regulation reaches particular flow rate, through in stainless steel disk gas distribution head
Micropore dispersion be filled with amine liquid for desulphurization sample interior.Gas-liquid two-phase is continuously in abundant contact process,
If the impurity of surface-active action in sample be present, then be likely to form by polyhedron
The foam that bubble is mutually accumulated, they are by along the cylindrical shape centered on gas distribution head
Kuppe is accumulated upwards, and hemispherical foam is finally formed above kuppe upper surface.By steeping
Condition caused by foam, it is bigger to advertise throughput, and gas-liquid two-phase contact is more abundant, and then foam
Also easier generation；The impurity that surface-active action is played in sample is more advantageous to foam generation, i.e.,
Expansion rate surmounts brokenly bubble speed, then it is smaller that what foam generation was required advertises throughput can.
Based on this, determine the minimum required for stable hemispherical foam is formed above kuppe and advertise gas
Flow value, can be as the index of evaluation amine liquid for desulphurization frothing capacity.Required flow is smaller, takes off
The foaming of thiamines liquid is horizontal more serious；Required flow is bigger, and amine liquid for desulphurization foaming is horizontal slighter.
Minimum required for the present invention advertises air flow value, can be used as evaluation amine liquid for desulphurization foaming
The index of performance, can directly look into rope in practical application, amine liquid for desulphurization frothing capacity and advertise air-flow
Magnitude relation table：(such as following table)
Wherein " amine liquid for desulphurization frothing capacity and advertise throughput relation table " by enterprise according to itself
The factor such as equipment ability to bear and cost control requirement is voluntarily formulated, and does not have national standard or row at present
Mark specifically defines to this work.
Closed it is an advantage of the invention that gas distribution head is formed with the plastics experiment cup with lid
Foaming environment, its humiture can be controlled by by introducing constant temperature and humidity gas, and it is dry to reduce foaming
Factor is disturbed, gas distribution head is the stainless steel disk thin slice for having special diameter through hole, corrosion-resistant,
Easy cleaning, thoroughly abolish with foaming height and foam time, but stablized with formation hemispherical
The minimum of foam advertises the frothing capacity of nitrogen flow evaluation amine liquid for desulphurization, reproducible.
Brief description of the drawings
Fig. 1 is organigram of the present invention.
Specific embodiment
According to Fig. 1, the present invention has an experiment cup 15 with a scale, and experiment cup uses
Transparent resistant material is made, and bottom is circular arc, and top is cylinder open container, there is lid,
There is exhaust outlet 6 at the center of lid, and be provided centrally with gas distribution head connecting rod, there is a cylinder
Type kuppe 13, the A-frame 25 that kuppe 13 is set by the closely upper head end of connecting rod support
Iron hoop 24 be installed on experiment cup 15 in middle part, at link end set the gas kept flat
Body distribution head 14, gas distribution head 14 are discoid, and the gas distribution head is special material
For diameter 15mm, thick 0.2mm, material is 316L stainless steel disk thin slices, through-hole diameter
For 0.15mm；Through hole is distributed as from the inside to surface, and number is followed successively by 3,4,8,8 totally 23；
2,5,8,11 are followed successively by for circular diameter；All hole laser borings.The top surface of kuppe 13 with
Bottom surface is opened wide, and gas distribution head 14 is in the center of kuppe 13 and is mutually not in contact with each other, the gas
Flowermeter of the connecting rod other end of body distribution head 14 to outside experiment cup 15 is connected, the flow
Counter device is by loading onto high stream respectively again by two pass ball valves 20 at four-way connection 23 in nitrogen
Gauge 10, middle flowmeter 11, Low-flow meter 12 and pressure gauge 18.In experiment cup 15 bottom
Side be provided with the port that sample inlet and outlet device pipe are led, the sample inlet and outlet
Device is to load onto sample inlet 1 and the dress of outlet 2 respectively at the three-pronged connector both sides for having switch 7
Pipe is put to lead.Experiment cup top is provided with constant temperature and humidity gas blowout head 8, the constant temperature and humidity gas blowout
First 8 air nozzle that goes out is annulus tubulose, there is multiple ventholes on annulus tubulose.In experiment cup
Top of piece pipe of constant temperature and humidity gas entrance 3 into experiment cup 15 is set at 15 lower through-ports,
The described pipe of constant temperature and humidity gas entrance 3 is to the outer connection flow gauge 9 of experiment cup 15 and pressure gauge 16.
The present invention amine liquid for desulphurization frothing capacity evaluation method be on kuppe formed stablize it is hemispherical
The minimum of foam advertises the frothing capacity of nitrogen flow evaluation amine liquid for desulphurization, and hemispherical foam is being led
Stream cover is formed above upper surface, is not contacted with other solid matters, can be avoided surface tension and table
The interference of face pollution, repeat experiment more preferable.
Claims (6)
1. a kind of amine liquid for desulphurization sparger, it is characterized in that there is an experiment cup with a scale, test
Cup is made of transparent resistant material, and bottom is circular arc, and top is cylinder open container,
There is lid, have exhaust outlet at the center of lid, and be provided centrally with gas distribution head connecting rod, there is one
Cylinder type kuppe, the iron hoop that the A-frame that kuppe is set by the closely upper head end of connecting rod supports
Middle part in experiment cup is installed on, a gas distribution head kept flat is set at link end, led
Stream cover top surface opens wide with bottom surface, and gas distribution head is in kuppe center and is mutually not in contact with each other, institute
State flowermeter of the gas distribution head connecting rod other end to outside experiment cup to be connected, in experiment bottom of a cup
The side in portion is provided with the port that sample inlet and outlet device pipe are led, and is set on experiment cup top
There is constant temperature and humidity gas blowout head, a constant temperature and humidity gas inlet tube is set at experiment cup lower through-ports
Top into experiment cup, described constant temperature and humidity gas inlet tube connection flow gauge to outside experiment cup
And pressure gauge.
A kind of 2. amine liquid for desulphurization sparger according to claim 1, it is characterized in that gas point
The special material of the leftover of bolt of cloth is diameter 15mm, and thick 0.2mm, material is 316L stainless steel disks
Thin slice, through-hole diameter 0.15mm；Through hole is distributed as from the inside to surface, and number is followed successively by 3,4,
8,8 totally 23；2,5,8,11 are followed successively by for circular diameter；All hole laser borings.
A kind of 3. amine liquid for desulphurization sparger according to claim 1, it is characterized in that flowmeter
Device is to load onto high-flow meter respectively at four-way connection, middle flowmeter, Low-flow meter.
A kind of 4. amine liquid for desulphurization sparger according to claim 1, it is characterized in that sample enters
Mouth and outlet device are to load onto sample inlet pipe, sample respectively at the three-pronged connector both sides for having switch
Product outlet.
A kind of 5. amine liquid for desulphurization sparger according to claim 1, it is characterized in that constant temperature is permanent
Moisture shower nozzle goes out air nozzle for the hole on annulus tubulose.
6. a kind of amine liquid for desulphurization frothing capacity evaluation method of amine liquid for desulphurization sparger, it is characterized in that
The minimum that stable hemispherical foam is formed on kuppe advertises nitrogen flow evaluation amine liquid for desulphurization
Frothing capacity, hemispherical foam formed above kuppe upper surface, not with other solids
Matter contacts, and can avoid the interference of surface tension and surface contamination, repeats experiment more preferable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610391287.4A CN107462669A (en) | 2016-06-03 | 2016-06-03 | A kind of amine liquid for desulphurization sparger and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610391287.4A CN107462669A (en) | 2016-06-03 | 2016-06-03 | A kind of amine liquid for desulphurization sparger and method |
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| Publication Number | Publication Date |
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| CN107462669A true CN107462669A (en) | 2017-12-12 |
Family
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610391287.4A Pending CN107462669A (en) | 2016-06-03 | 2016-06-03 | A kind of amine liquid for desulphurization sparger and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111089935A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | On-site natural gas dry desulfurizing agent sulfur capacity testing method |
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| JPH0862206A (en) * | 1994-08-18 | 1996-03-08 | Nippon Oil Co Ltd | Simplified foaming-test method and apparatus for lubricating oil |
| JPH10230128A (en) * | 1997-02-17 | 1998-09-02 | Chiyoda Corp | Flue gas desulfurization method and flue gas desulfurizing device |
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2016
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|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111089935A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | On-site natural gas dry desulfurizing agent sulfur capacity testing method |
| CN111089935B (en) * | 2018-10-24 | 2023-01-03 | 中国石油化工股份有限公司 | On-site natural gas dry desulfurizing agent sulfur capacity testing method |
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Application publication date: 20171212 |
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| RJ01 | Rejection of invention patent application after publication |