CN1945259A - Coal slurry reactant sampling device - Google Patents
Coal slurry reactant sampling device Download PDFInfo
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- CN1945259A CN1945259A CN 200610138048 CN200610138048A CN1945259A CN 1945259 A CN1945259 A CN 1945259A CN 200610138048 CN200610138048 CN 200610138048 CN 200610138048 A CN200610138048 A CN 200610138048A CN 1945259 A CN1945259 A CN 1945259A
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Abstract
The coal slurry reactant sampling device includes one sampling container connected through pipes with valves to the material conveying pipeline; solvent oil pipes with valve; hydrogen pipes; one gas sampling pipe in the upper part of the sampling container; one sampling pipe in the lower part of the sampling container; and one inert gas pipe communicated to the sampling container. The coal slurry reactant sampling device is accurate and reliable in sampling, convenient and safe in operation, and can sampling repeatedly.
Description
Technical field
The present invention relates to a kind of coal slurry reactant sampling device, more particularly, is a kind of coal slurry reactant sampling device that is used for the coal liquefaction process.
Background technology
The coal liquefaction reaction is the coal generation pyrolysis that makes under high temperature, high pressure in the high concentration coal slurry, carries out hydrogenation and further decomposition under the effect of catalyzer, finally becomes stable fluid molecule.Because each factors of coal liquefaction craft condition such as coal-water fluid concentration, pressure, temperature, the residence time, gas liquid ratio all have the influence of the pros and cons to the economy of coal liquefaction reaction and liquefying plant, must be by a large amount of experiments and economy relatively come to determine suitable process conditions repeatedly.Therefore, when coal liquefaction is reacted, be the monitoring reaction state, determine the optimal operations parameter, the gas, the liquid that need regularly to take out reactant from the coal liquefaction reactor carry out constituent analysis, obtain basic technological parameter.
Yet because the coal liquefaction reaction is all carried out under high temperature, high pressure conditions, will be from direct sample operation in the reactor, not only dangerous, operation inconvenience, and because the sample of being got is the gas, liquid, solid three-phases, when it became atmospheric pressure state from high pressure conditions, the medium of being taken a sample can produce serious wearing and tearing to sampling equipment; And because of the installation site and the structure thereof of sampling equipment often has the dead angle, thereby easily cause the medium of being taken a sample to stop up sampling equipment, feasible sub-sampling again.For this reason, in the coal liquefaction course of reaction, just need a kind of safe and easy to operate sampling method and device of exploitation.
The patent No. is that the Chinese patent that the name of ZL90214227.5 is called " a kind of high temperature, high-pressure sampling container " discloses a kind of sampling equipment that can be used for high temperature, high pressure and deep well sampling, but this sampling equipment only is applicable to the steam sampling of high temperature, high pressure and deep well, do not contain solid particle in its sample of getting, can not cause wearing and tearing to sampler, and it is simple in structure, therefore, in the coal liquefaction course of reaction, can't take a sample with described sampling container.
The patent No. be Chinese patent that the name of ZL96193860.9 is called " sampling method and equipment " disclose a kind of from olefinic polymerization polymer beads and the streaming suspension that constitutes of hydrocarbon diluent in the method and apparatus of taking a sample, but this method only is applicable to the situation that temperature and pressure is lower, be not suitable for the situation of high temperature, high pressure, therefore, in the coal liquefaction course of reaction, can't take a sample with described sampling method and equipment equally.
Summary of the invention
The purpose of this invention is to provide a kind of sampler that from high temperature, high-pressure reactor, takes out gas, liquid, solid phase reaction thing.
Coal slurry reactant sampling device provided by the present invention comprises:
One sampling container 31, this sampling container links to each other with mass transport pipeline 3 between first reactor 1 and second reactor 30 by pipeline 36 and 37, and valve 4,5 and 6 is set on the described pipeline 36, and valve 7,8 and 9 is set on the described pipeline 37;
One solvent oil pipeline 27, this pipeline links to each other with pipeline 37 and this pipeline is provided with valve 14; Also branch out the solvent oil pipeline 39 that another links to each other with pipeline 36 on this pipeline, and pipeline 39 is provided with valve 17;
One hydrogen gas lines 28, this pipeline links to each other with pipeline 37 and this pipeline is provided with valve 15; Also branch out the hydrogen gas lines 41 that another links to each other with pipeline 36 on this pipeline, and pipeline 41 is provided with valve 16;
The one gas sample pipeline 33 that is positioned at sampling container 31 tops and is connected with sampling container, this pipeline is provided with valve 10;
One sampling line 35 that is positioned at sampling container 31 bottoms and is connected with sampling container, this pipeline is provided with valve 13; And described pipeline 37 is connected with this sampling line;
One inert gas pipeline 34, this pipeline is connected with sampling container 31, and this pipeline is provided with valve 11.
In order to make those skilled in the art understand the present invention better, further describe sampler provided by the present invention below.
In device of the present invention, described sampling container 31 is preferably a container that can bear high temperature, high pressure, and for example, temperature can reach about 500 ℃, and pressure can reach about 20Mpa.For preventing the adhesion of coal slurry reactant on chamber wall, make this container easy cleaning, can polish container inner wall, for example, the roughness of polishing back vessel surface is 0.8-0.2 μ m, preferred 0.4-0.2 μ m.
But the outside of described sampling container 31 preferably is provided with the but chuck of medium circulation of cooling, by flowing through the heat eliminating medium of this chuck, the temperature of sampling container and this container internal reaction thing is minimized.Described heat eliminating medium can be selected chilled water, cold oil or other heat eliminating medium commonly used for use.
In order to prevent that coal slurry reactant enters hydrogen gas lines and solvent oil pipeline in operating process, valve on hydrogen gas lines and solvent oil pipeline 14,15,16 and 17 downstream respectively, promptly, retaining valve 18,19,20 and 21 is set respectively preferably near a side of pipeline 36 or 37.
On the mass transport pipeline 3 that connects first reactor 1 and second reactor 30, valve 2 is set.For the valve 4,5 and 6 that is provided with on described valve 2 and the pipeline 36, the valve 7,8 and 9 that is provided with on the pipeline 37, be the high High Temperature High Pressure coal slurry of solid content owing to flow through the medium of these valves, this medium can produce more serious wearing and tearing to valve body, therefore, need satisfy for the Material Selection of these valves resistance to wear, the requirement of high temperature resistant and high pressure.Because the spheroid of ball valve has wiping in opening-closing process, can be used in the medium with suspended solids, metal o-ring can high temperature resistant and high pressure, therefore above-mentioned valve preferably adopts metal seal ball valve, and it is inclined to one side by the valve rod spiral that the Vehicle Processing of area of computer aided numerical control machine is made, make metal seal ball valve in opening-closing process, not have scratch and wearing and tearing, thus the sealing and the serviceable life of improving valve greatly.Wherein, valve 4 and valve 7 are preferably pneumatic valve.
In order to reduce the impact of gases at high pressure to sampling system as much as possible, the valve 15 and 16 on the high pressure hydrogen pipeline is preferably selected the valve that open degree such as stop valve, needle valve are little, adjusting is more convenient for use.In addition, described hydrogen gas lines 28 and 41 the endpiece that preferably is positioned as close to valve 4 and 7 is set so that it is clean that reactant residual on the pipeline is purged as much as possible, avoid deposition because of solid particle to produce and stop up.
Generally speaking, preferably be furnished with tensimeter PG and thermometer TG on the sampling container 31.The described gas sample pipeline 33 that is positioned at sampling container 31 tops and is connected with sampling container is provided with valve 10.In order to provide more convenience, on described pipeline 33, two valves 10 can be set to sampling operation; In like manner, on the described sampling line that is connected with sampling container 35, also can be provided with two valves 13.In addition, on pipeline 33 and pipeline 35, can also be provided with online flowmeter commonly used, on-line analysis equipment etc.
In device of the present invention, described pipeline 36 and 37 is connected with mass transport pipeline 3 respectively, and valve 2 pipeline 36 and 37 and two tie points of pipeline 3 between.
Compared with prior art, because the characteristics of coal slurry reactant sampling device provided by the present invention are mainly reflected in following aspect:
1, can take a sample to high temperature, high pressure and the coal slurry reactant that contains gas, liquid, solid three phase materials, the sample of being got is representative, can truly reflect the variation of coal slurry reactant in the reactor, sampling accurately, reliable;
2, can take a sample under high-temperature and high-pressure conditions, temperature can reach 500 ℃ or higher, and pressure can reach 20Mpa or higher;
3, whole sampling process is easy to operate, and is safe, and sampling the time do not influence reactive system, and sampling process is relatively independent;
4, sampler of the present invention can make things convenient for, compactly salvage stores be purged and cleans, and therefore, this device can repeatedly repeat sampling.
Description of drawings
Fig. 1 is the synoptic diagram of a kind of preferred implementation of device of the present invention.
Embodiment
Further specify the working method of sampler provided by the present invention below in conjunction with accompanying drawing, but therefore the present invention is not subjected to any restriction.
Adopt the sampling process of device of the present invention can be divided into sampling and prepare, take a sample, clean and purge three steps.
Sampling is prepared:
1, shut-off valve 4 and valve 7, shut-off valve 15 and valve 16;
2, open valve 5,6,8 and 9, if the pressure in the sampling container 31 is lower than the pressure of reactive system, for example, 20MPa, open valve 14 and 17, make the high pressure solvent oil inject sampling container 31 and corresponding pipeline 36 and 37, when pressure reaches reacting system pressure, pneumatic valve 4 and 7 both sides pressure equilibriums, shut-off valve 14 and 17;
3, remote opening pneumatic valve 4 and 7 cuts out the valve 2 on the pipeline 3 then;
4, the flow direction of reaction mass changes, and through pipeline 36 and valve 4,5 and 6, enters high-pressure sampling container 31, is delivered to pipeline 37 through pipeline 35 then, the valve 9,8 and 7 of flowing through, and return line 3, and further be delivered to second reactor 30; This sampling set-up procedure generally continues 1-10 minute, and the Optimal Control time is 2-5 minute, and the displacement of the solvent oil in the sampling container 31 is finished, and makes to be full of reaction product in the sampling container.
Sampling:
1, opens valve 2;
2, shut-off valve 4 and 7, the flow direction of change reaction mass makes the material from first reactor directly enter second reactor through pipeline 3;
3, shut-off valve 5,6,8,9;
4, sampling container cooling by inject chilled water or cooling wet goods medium in the sampling container chuck, makes the temperature of sampling container reduce to 50-100 ℃ from 450 ℃; Because of being gas-liquid-solid three-phase in the sampling container,, generally be lower than reacting system pressure along with the pressure in the reduction sampling container of temperature decreases;
5, coal slurry reactant was stopped 5-10 minute in sampling container, gas phase and liquid-solid two-phase layering, gas phase is on the top of sampling container, and liquid-solid two-phase is in the bottom of sampling container;
6, slow open valve 10 carries out gas dosing by wet flow indicator or other gas measuring instrument, and measures gas composition simultaneously, and gas composition can adopt sampling to analyze or on-line analysis;
7, during liquid sampling, valve 10 is held open state, opens valve 13, and liquid-solid two-phase is discharged automatically by gravity, takes a sample and weighs, and analyzes its component; If sample can not flow out smoothly, but shut-off valve 10, the valve of opening on the pipeline 34 11 feeds inert gas, and for example, nitrogen by increasing the pressure in the sampling container, is obtained the sample of liquid-solid two-phase.
Clean and purge:
1, affirmation valve 10,11 and 13 cuts out, and opens valve 5,6,8 and 9, opens valve 15 and 16, and the coal slurry reactants in pipeline 36 and 37 are purged to sampling container; Purge time was generally 1-10 minute, preferred 5-7 minute;
2, shut-off valve 15 and 16, shut-off valve 5 and valve 8 then; Open valve 10 simultaneously, pressure in the sampling container is reduced to behind the normal pressure at shut-off valve 10;
3, slowly open valve 17 and valve 14, in sampling container, fill with solvent oil;
4, shut-off valve 17 and valve 14 are opened valve 13 solvent oil are discharged;
5, step 3 and step 4 can repeat repeatedly, observe the solvent oil that develops, and get final product shut-off valve 13 when confirming not contain coal slurry in the oil;
6, shut-off valve 6 and valve 9 are opened valve 10, open valve 11 simultaneously, carry out nitrogen purging, and the air displacement in the sampling container is clean;
7, affirmation valve 10,11 and 13 cuts out, and opens valve 5,6,8 and 9, opens valve 14 and 17, makes in sampling container 31 and the pipeline thereof to be full of solvent oil, and the pressure of its pressure and reactive system is basic identical;
8, shut-off valve 14 and 17, shut-off valve 5,6,8 and 9;
9, open valve 15 and 16, open valve 4 and 7 then, maintain hydrogen stream and cross valve 4 and 7.
Embodiment
This embodiment explanation: the applicable cases of sampler provided by the present invention in the DCL/Direct coal liquefaction reactive system.
The coal slurry of the raw material of DCL/Direct coal liquefaction device for forming by 100 purpose coal dusts (content 45 heavy %), solvent oil and Preparation of Catalyst.Coal slurry and hydrogen enter first reactor, react after 45 minutes, enter second reactor by valve 2 and pipeline 3.The concrete operations step is as follows:
1, open valve 5,6,8,9,10 and 11, with the gas in the nitrogen replacement sampler, shut-off valve 5,6,8,9,10 and 11 then;
2, shut-off valve 4 and 7, shut-off valve 15 and 16;
3, open valve 5,6,8 and 9,, open valve 14 and 17, make in the high pressure solvent oil injection sampling container and in the pipeline if the pressure in the sampling container 31 is lower than 20MPa, when pressure reaches 20.0MPa, pneumatic valve 4 and 7 both sides pressure equilibriums, shut-off valve 14 and 17;
4, remote opening pneumatic valve 4 and 7, shut-off valve 2 then;
5, behind reactant streams process valve 4,5,6 and the sampling container 31,, keep this operation 2-5 minute, make to be full of reaction product in the sampling container through valve 9,8 and 7 return lines 3;
6, open valve 2;
7, shut-off valve 4 and 7, the flow direction of change reaction mass;
8, shut-off valve 5,6,8 and 9;
9, make sampling container cooling by the chilled water in the sampling container chuck, temperature is reduced to 50-80 ℃ from 450 ℃, and its pressure decreases to the 16Mpa;
10, coal slurry reactant stopped in sampling container 5-10 minute, gas phase and liquid-solid two-phase layering;
11, slow open valve 10 carries out gas dosing by wet flow indicator, and gathers gaseous sample simultaneously, by the gas Chromatographic Determination gas composition;
12, during liquid sampling, valve 10 is held open state, opens valve 13, takes out fluid sample, and Weighing, analyzes wherein component;
13, affirmation valve 10,11 and 13 cuts out, and opens valve 5,6,8 and 9, opens valve 15 and 16, the coal slurry in the sampling container pipeline is poured in the sampling container purge time 5-7 minute;
14, shut-off valve 15 and 16, shut-off valve 5 and 8 then; Open valve 10 simultaneously, close again after the sampling container internal pressure is reduced to normal pressure;
15, slowly open valve 14 and 17, in sampling container, fill with solvent oil;
16, shut-off valve 14 and 17 is opened valve 13 solvent oil is discharged;
17, step 15 and step 16 repeat 3 times, do not contain coal slurry in the solvent oil that sampling container is discharged, shut-off valve 13;
18, shut-off valve 6 and 9 is opened valve 10, opens valve 11 simultaneously, carries out nitrogen purging, and air displacement in the sampling container is clean;
19, affirmation valve 10,11 and 13 cuts out, and opens valve 5,6,8 and 9, opens valve 14 and 17, makes in sampling container and the pipeline thereof to be full of solvent oil, and pressure is 20Mpa;
20, shut-off valve 14 and 17, shut-off valve 5,6,8 and 9;
21, open valve 15 and 16, open valve 4 and 7 then, maintain hydrogen stream and cross valve 4 and 7; So far, the cleaning of sampling container purges and finishes, for sub-sampling is ready again.
Claims (9)
1. coal slurry reactant sampling device, this device comprises:
One sampling container (31), this sampling container links to each other with the mass transport pipeline (3) that is positioned between first reactor (1) and second reactor (30) by pipeline (36) and (37), and valve (4,5 and 6) is set on the described pipeline (36), valve (7,8 and 9) is set on the described pipeline (37);
One solvent oil pipeline (27), this pipeline links to each other with pipeline (37) and this pipeline is provided with valve (14); Also branch out the solvent oil pipeline (39) that another links to each other with pipeline (36) on this pipeline, and pipeline (39) is provided with valve (17);
One hydrogen gas lines (28), this pipeline links to each other with pipeline (37) and this pipeline is provided with valve (15); Also branch out the hydrogen gas lines (41) that another links to each other with pipeline (36) on this pipeline, and pipeline (41) is provided with valve (16);
The one gas sample pipeline (33) that is positioned at sampling container (31) top and is connected with sampling container, this pipeline is provided with valve (10);
One sampling line (35) that is positioned at sampling container (31) bottom and is connected with sampling container, this pipeline is provided with valve (13); And described pipeline (37) is connected with this sampling line;
One inert gas pipeline (34), this pipeline is connected with sampling container (31), and this pipeline is provided with valve (11).
2. reactant sampling device according to claim 1 is characterized in that, the surfaceness of described sampling container (31) inwall is 0.8-0.2 μ m, but and the outside of this sampling container be provided with the but chuck of medium circulation of cooling.
3. reactant sampling device according to claim 2 is characterized in that, the surfaceness of described sampling container (31) inwall is 0.4-0.2 μ m, and adopts chilled water or the cold oil heat eliminating medium as this sampling container.
4. according to claim 1 or 3 described reactant sampling devices, it is characterized in that the downstream of the valve on hydrogen gas lines and solvent oil pipeline (14,15,16 and 17) is provided with retaining valve (18,19,20 and 21) respectively.
5. reactant sampling device according to claim 4 is characterized in that, described pipeline (36) and (37) are connected with mass transport pipeline (3) respectively, and valve (2) is arranged between two tie points of pipeline (36) and (37) and pipeline (3).
6. reactant sampling device according to claim 5 is characterized in that, described valve (4) and valve (7) are pneumatic valve; Described valve (15) and (16) are stop valve or needle valve; Described valve (4,5,6,7,8 and 9) is a metal seal ball valve.
7. according to claim 1 or 6 described reactant sampling devices, it is characterized in that the setting of described hydrogen gas lines (28 and 41) is positioned as close to the endpiece of valve (4 and 7).
8. reactant sampling device according to claim 7 is characterized in that, two valves (10) are set on the described pipeline (33); At described pipeline (35) two valves (13) are set also.
9. reactant sampling device according to claim 8 is characterized in that, described pipeline (33) and pipeline (35) are provided with online flowmeter and in-line analyzer.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101380484A CN100533111C (en) | 2006-11-03 | 2006-11-03 | Coal slurry reactant sampling device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101380484A CN100533111C (en) | 2006-11-03 | 2006-11-03 | Coal slurry reactant sampling device |
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| CN1945259A true CN1945259A (en) | 2007-04-11 |
| CN100533111C CN100533111C (en) | 2009-08-26 |
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| CNB2006101380484A Active CN100533111C (en) | 2006-11-03 | 2006-11-03 | Coal slurry reactant sampling device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101975038A (en) * | 2010-10-09 | 2011-02-16 | 东北石油大学 | Device for sampling mud rock by cooling air and rock sample sampling method thereof |
| CN102435463A (en) * | 2011-10-31 | 2012-05-02 | 神华集团有限责任公司 | Online acquisition system and method for catalyst slurry |
| CN103334742A (en) * | 2013-06-08 | 2013-10-02 | 原子高科股份有限公司 | Water sample extraction device for oilfield well-to-well tracer technology |
| CN104251788A (en) * | 2014-09-22 | 2014-12-31 | 清华大学 | Sampling device for gas-liquid-solid-composed black water for coal gasification system |
| CN105527126A (en) * | 2015-12-23 | 2016-04-27 | 陕西华电榆横煤化工有限公司 | Catalyst on-line sampling system and method for aromatization process |
| CN105571906A (en) * | 2014-11-06 | 2016-05-11 | 中国石油天然气股份有限公司 | Fixed bed hydrogenation device sampler and sampling method thereof |
| US10287522B2 (en) | 2013-01-31 | 2019-05-14 | General Electric Company | System and method for preparing coal water slurry |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5065416A (en) * | 1987-12-04 | 1991-11-12 | Process Technology, Inc. | On-line slurry ash monitoring system |
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2006
- 2006-11-03 CN CNB2006101380484A patent/CN100533111C/en active Active
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101975038A (en) * | 2010-10-09 | 2011-02-16 | 东北石油大学 | Device for sampling mud rock by cooling air and rock sample sampling method thereof |
| CN101975038B (en) * | 2010-10-09 | 2013-01-16 | 东北石油大学 | Device for sampling mud rock by cooling air and rock sample sampling method thereof |
| CN102435463A (en) * | 2011-10-31 | 2012-05-02 | 神华集团有限责任公司 | Online acquisition system and method for catalyst slurry |
| CN102435463B (en) * | 2011-10-31 | 2014-05-21 | 神华集团有限责任公司 | Online acquisition system and method for catalyst slurry |
| US10287522B2 (en) | 2013-01-31 | 2019-05-14 | General Electric Company | System and method for preparing coal water slurry |
| CN103334742A (en) * | 2013-06-08 | 2013-10-02 | 原子高科股份有限公司 | Water sample extraction device for oilfield well-to-well tracer technology |
| CN103334742B (en) * | 2013-06-08 | 2016-09-14 | 原子高科股份有限公司 | A kind of water sample extraction element of tracer technique between oil well |
| CN104251788A (en) * | 2014-09-22 | 2014-12-31 | 清华大学 | Sampling device for gas-liquid-solid-composed black water for coal gasification system |
| CN105571906A (en) * | 2014-11-06 | 2016-05-11 | 中国石油天然气股份有限公司 | Fixed bed hydrogenation device sampler and sampling method thereof |
| CN105527126A (en) * | 2015-12-23 | 2016-04-27 | 陕西华电榆横煤化工有限公司 | Catalyst on-line sampling system and method for aromatization process |
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| Publication number | Publication date |
|---|---|
| CN100533111C (en) | 2009-08-26 |
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