CN102659077B - High-pressure fixed bed recycle hydrogen dry desulphurization device and method - Google Patents

High-pressure fixed bed recycle hydrogen dry desulphurization device and method Download PDF

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CN102659077B
CN102659077B CN 201210155019 CN201210155019A CN102659077B CN 102659077 B CN102659077 B CN 102659077B CN 201210155019 CN201210155019 CN 201210155019 CN 201210155019 A CN201210155019 A CN 201210155019A CN 102659077 B CN102659077 B CN 102659077B
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recycle hydrogen
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air cooler
pressure separator
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CN102659077A (en
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刘超
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HAINAN HANDI SUNSHINE PETROCHEMICAL CO Ltd
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Abstract

The invention discloses a high-pressure fixed bed recycle hydrogen dry desulphurization device and a method. The device comprises an air cooler, a high-pressure separator, a hydrogen sulfide-removal tower and a recycle hydrogen knock-out drum, wherein the air cooler, the high-pressure separator, the hydrogen sulfide-removal tower and the recycle hydrogen knock-out drum are connected through a pipeline; the outer end of the air cooler is connected with a desulphurization inlet; the outer side of the air cooler is provided with a refrigeration controller; the top part of the high-pressure separator is provided with a pressure controller; the middle part of the high-pressure separator is provided with a liquid level controller; the lower part of the high-pressure separator is connected with a liquid outlet pipeline; the liquid outlet pipeline is provided with a liquid level control valve; the top part of the recycle hydrogen knock-out drum is provided with a recycle hydrogen outlet; and the bottom part of the recycle hydrogen knock-out drum is provided with a condensate outlet. The invention has the beneficial effects that as the dry desulphurization method is adopted, any impurities are not generated in the desulphurization process. Moreover, the device is long in service life and easy in maintenance; a desulphurization effect can reach 100 percent; the sulfur content of the recycle hydrogen can be controlled to be under 2ppm all along, so that the service life of a catalyst and the service life of equipment are prolonged, and the running cost of the device is further reduced. Moreover, no secondary pollution is generated, and the problem of environment treatment does not exist.

Description

A kind of high pressure fixed bed recycle hydrogen dry desulfurization device and method
Technical field
The present invention relates to a kind of high pressure fixed bed recycle hydrogen dry desulfurization device and method.
Background technology
At present, do not have design cycle hydrogen desulfurizer in domestic existing High-pressure Hydrogenation Unit.And, in order to solve the excessive problem of sulphur content in recycle hydrogen, can only constantly supplement highly purified hydrogen (99.99%) by useless hydrogen line discharge cycle hydrogen the while at high-pressure separator top, in the mode of constantly being replaced, realize.And existing medium pressure hydrogenation unit adopts, be that the reverse absorption-hydrometallurgic recovery of ammoniacal liquor realizes removing of hydrogen sulfide, principle is to allow oil gas through the device of ammoniacal liquor is housed, and with ammoniacal liquor, absorbs sulphur, and then ammonia recycles after desulfurization again; Although ammoniacal liquor can recycling use, this kind of method still will be built a set of solvent reclamation device again, and all will be designed to the high-tension apparatus system, domesticly in high-pressure hydrogenation, also can't apply.
For the shortcoming of above-mentioned prior art, if just simply solve by continuous dilution sulphur purity, certainly will cause hydrogen loss, and plant energy consumption increases, generally can increase by 5 ~ 10% hydrogen gas consumption in actually operating, and sweetening effectiveness is poor, can't accomplish 100% desulfurization; And the Technology absorbed with ammoniacal liquor, although effect is better, but ammoniacal liquor will have corresponding high-tension apparatus and pipeline when the use of solvent reclamation matched with devices and ammoniacal liquor desulfurization must be arranged, and build a set of corollary apparatus more, must there be personnel to carry out management operating, plant investment is large, and operation more complicated and running cost are higher, and also there is the problem of environmental protection treatment at present in the ammoniacal liquor that has absorbed in addition sulphur.
Summary of the invention
The purpose of this invention is to provide a kind of high pressure fixed bed recycle hydrogen dry desulfurization device and method, to solve above technical barrier.
A kind of high pressure fixed bed recycle hydrogen dry desulfurization device of the present invention, comprise that the air cooler, high-pressure separator, de-hydrogen sulfide column and the recycle hydrogen that are connected by pipeline divide flow container; The air cooler outer end is connected with the desulfurization entrance, and the air cooler outside is provided with refrigeration controler; Described high-pressure separator top is provided with pressure controller, and middle part is provided with fluid level controller, and the high-pressure separator bottom is connected with the fluid pipeline, and the fluid pipeline is provided with level control valve; Described recycle hydrogen separatory tank top is provided with the recycle hydrogen outlet, and bottom is provided with condensate outlet.
A kind of high pressure fixed bed recycle hydrogen dry desulfurizing process of the present invention, it comprises the following steps:
1) the recycle hydrogen gas that is mixed with hydrogen sulfide enters in air cooler cooling by the desulfurization entrance, and controls gas space velocity/h -1:≤3000, and the temperature of controlling the gas in air cooler by refrigeration controler is in 45-55 ℃ of scope;
2) circulating hydrogen enters high-pressure separator and carries out gas-liquid separation, and controls liquid level and high-pressure separator internal pressure in the 14.5-16.5MPa scope by fluid level controller and level control valve;
3) circulating hydrogen enters the de-hydrogen sulfide column desulfurization, fill successively diameter 15mm porcelain ball layer, diameter 6mm porcelain ball layer, adsorbent layer, diameter 6mm porcelain ball layer and diameter 15mm porcelain ball layer in de-hydrogen sulfide column from top to bottom, and make its working pressure be controlled at 15.0-18.9MPa, service temperature≤50 ℃;
4) circulating hydrogen after desulfurization enters recycle hydrogen and divides flow container to get rid of phlegma to enter the circulating hydrogen compressor recycle hydrogen and recycle.
Beneficial effect of the present invention is: the present invention adopts dry desulfurizing process, do not produce any impurity in sweetening process, and device long service life, be easy to safeguard, sweetening effectiveness can reach 100%, and the sulphur content of recycle hydrogen can be controlled at below 2ppm all the time, make extend the work-ing life of catalyzer, equipment, further reduce the cost of device operation, and there is no secondary pollution, do not had the environmental protection treatment problem.
The accompanying drawing explanation
Below with reference to the accompanying drawings the present invention is described in further detail.
The structural representation of a kind of high pressure fixed bed recycle hydrogen dry desulfurization device that Fig. 1 is the embodiment of the present invention;
In figure:
1, air cooler; 2, high-pressure separator; 3, de-hydrogen sulfide column; 4, recycle hydrogen divides flow container; 5, refrigeration controler; 6, fluid level controller; 7, pressure controller; 8, level control valve; 9, desulfurization entrance; 10, condensate outlet; 11, recycle hydrogen outlet.
Embodiment
As shown in Figure 1, the of the present invention a kind of high pressure fixed bed recycle hydrogen dry desulfurization device shown in the embodiment of the present invention, comprise that the air cooler 1, high-pressure separator 2, de-hydrogen sulfide column 3 and the recycle hydrogen that are connected by pipeline divide flow container 4; Air cooler 1 outer end is connected with desulfurization entrance 9, and air cooler 1 outside is provided with refrigeration controler 5; Described high-pressure separator 2 tops are provided with pressure controller 7, and middle part is provided with fluid level controller 6, and high-pressure separator 2 bottoms are connected with the fluid pipeline, and the fluid pipeline is provided with level control valve 8; Described recycle hydrogen divides flow container 4 tops to be provided with recycle hydrogen outlet 11, and bottom is provided with condensate outlet 10.
The method of utilizing the described a kind of high pressure fixed bed recycle hydrogen dry desulfurization device of the embodiment of the present invention to carry out desulfurization, it comprises the following steps:
1) the recycle hydrogen gas that is mixed with hydrogen sulfide enters in air cooler 1 cooling by desulfurization entrance 9, and controls gas space velocity/h -1:≤3000, and control the temperature of the gas in air cooler 1 in 45-55 ℃ of scope by refrigeration controler 5;
2) circulating hydrogen enters high-pressure separator 2 and carries out gas-liquid separation, and controls liquid levels and high-pressure separator 2 internal pressures in the 14.5-16.5MPa scope by fluid level controller 6 and level control valve 8;
3) circulating hydrogen enters de-hydrogen sulfide column 3 desulfurization, fill successively diameter 15mm porcelain ball layer, diameter 6mm porcelain ball layer, adsorbent layer, diameter 6mm porcelain ball layer and diameter 15mm porcelain ball layer in de-hydrogen sulfide column 3 from top to bottom, and make its working pressure be controlled at 15.0-18.9MPa, service temperature≤50 ℃;
Filling situation during actual the use is as shown in the table:
Figure 966026DEST_PATH_IMAGE001
Wherein, JX-4A type sweetening agent is developed by Sanju Environment Protection New Material Co., Ltd., Beijing, and its concrete technical parameter is as follows:
Figure 932714DEST_PATH_IMAGE002
4) circulating hydrogen after desulfurization enters recycle hydrogen and divides flow container 4 to get rid of phlegmas to enter the circulating hydrogen compressor recycle hydrogen and recycle.
A kind of high pressure fixed bed recycle hydrogen dry desulfurization device and method shown in the China Chemical Industry company application embodiment of the present invention, significantly reduced the hydrogen usage quantity of device, calculate by annual hydrogen usage in 2011 the new hydrogen consumption that this technological transformation has reduced 72 tons, close 1,670,000 yuan of Renminbi.
Although below only described the specific embodiment of the present invention example, it will be understood by those of skill in the art that these only illustrate, protection scope of the present invention is limited by appended claims.Those skilled in the art, under the prerequisite that does not deviate from principle of the present invention and essence, can make various changes or modifications to these embodiments, but these changes or modification all fall into protection scope of the present invention.

Claims (1)

1. a high pressure fixed bed recycle hydrogen dry desulfurization device, comprise that the air cooler (1), high-pressure separator (2), de-hydrogen sulfide column (3) and the recycle hydrogen that are connected by pipeline divide flow container (4); It is characterized in that: air cooler (1) outer end is connected with desulfurization entrance (9), and air cooler (1) outside is provided with refrigeration controler (5); Described high-pressure separator (2) top is provided with pressure controller (7), and high-pressure separator (2) middle part is provided with fluid level controller (6), and high-pressure separator (2) bottom is connected with the fluid pipeline, and this fluid pipeline is provided with level control valve (8); Described recycle hydrogen divides flow container (4) top to be provided with recycle hydrogen outlet (11), and recycle hydrogen divides flow container (4) bottom to be provided with condensate outlet (10), and wherein, the method for utilizing described high pressure fixed bed recycle hydrogen dry desulfurization device to carry out desulfurization comprises the following steps:
1) the recycle hydrogen gas that is mixed with hydrogen sulfide enters in air cooler (1) cooling by desulfurization entrance (9), and controls gas space velocity/h -1:≤3000, and control the temperature of the gas in air cooler (1) in 45-55 ℃ of scope by refrigeration controler (5);
2) circulating hydrogen enters high-pressure separator (2) and carries out gas-liquid separation, and by fluid level controller (6) and level control valve (8) control liquid level and high-pressure separator (2) internal pressure in the 14.5-16.5MPa scope;
3) circulating hydrogen enters de-hydrogen sulfide column (3) desulfurization, fill successively diameter 15mm porcelain ball layer, diameter 6mm porcelain ball layer, adsorbent layer, diameter 6mm porcelain ball layer and diameter 15mm porcelain ball layer in de-hydrogen sulfide column (3) from top to bottom, and make its working pressure be controlled at 15.0-18.9MPa, service temperature≤50 ℃; And
4) circulating hydrogen after desulfurization enters recycle hydrogen and divides flow container (4) to get rid of phlegma to enter the circulating hydrogen compressor recycle hydrogen and recycle.
CN 201210155019 2012-05-18 2012-05-18 High-pressure fixed bed recycle hydrogen dry desulphurization device and method Active CN102659077B (en)

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CN101721861A (en) * 2009-12-18 2010-06-09 上海华畅环保设备发展有限公司 Method and device for desulphurization of recycle hydrogen
CN202594773U (en) * 2012-05-18 2012-12-12 海南汉地阳光石油化工有限公司 High-pressure fixed bed circulating hydrogen dry desulfurization device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101721861A (en) * 2009-12-18 2010-06-09 上海华畅环保设备发展有限公司 Method and device for desulphurization of recycle hydrogen
CN202594773U (en) * 2012-05-18 2012-12-12 海南汉地阳光石油化工有限公司 High-pressure fixed bed circulating hydrogen dry desulfurization device

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Denomination of invention: A high-pressure fixed bed circulating hydrogen dry desulfurization device and method

Effective date of registration: 20230823

Granted publication date: 20131225

Pledgee: Industrial Bank Co.,Ltd. Haikou Branch

Pledgor: HAINAN HANDI SUNSHINE PETROCHEMICAL Co.,Ltd.

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