CN103100446A - Startup sulfuration method of hydrogenation unit - Google Patents
Startup sulfuration method of hydrogenation unit Download PDFInfo
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- CN103100446A CN103100446A CN2011103524518A CN201110352451A CN103100446A CN 103100446 A CN103100446 A CN 103100446A CN 2011103524518 A CN2011103524518 A CN 2011103524518A CN 201110352451 A CN201110352451 A CN 201110352451A CN 103100446 A CN103100446 A CN 103100446A
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Abstract
The invention relates to a startup sulfuration method of a hydrogenation unit. According to the invention, a part of recycle gas is heated by using a heating furnace at first, then a vulcanizing agent is introduced, and hydrogen sulfide is obtained after decomposition of the vulcanizing agent; then recycle gas rich in hydrogen sulfide is mixed with a second part of recycle gas, and obtained mixed gas passes through a catalyst bed after an expected temperature requirement is met; heating is continued after a great amount of hydrogen sulfide penetrates the catalyst bed, and injection amount of the vulcanizing agent is adjusted according to requirements on the content of hydrogen sulfide; the ratio of the two parts of recycle gas is adjusted according to requirements on temperature, and sulfuration is finished according to a heating rate and constant temperature conditions; and temperature is decreased after sulfuration is finished, startup oil is introduced for wetting of the catalyst bed, heating is carried out, and then raw oil is introduced instead. Compared with the prior art, the method provided by the invention enables performance of a catalyst to be effectively brought into play and realizes safe and smooth startup.
Description
Technical field
The invention belongs to the processing method of oil Refining Technologies, particularly relate to a kind of start-up vulcanization method of hydrogenation plant hydrogenation catalyst.
Background technology
Along with the protection to environment; environmental regulation increasingly stringent in global range, this just needs to produce a large amount of clean light clean fuels, and hydrogen addition technology is the effective means of cleaning products; therefore hydrogenation plant has become the standard configuration of oil plant, and the hydrogenation plant in oil refining enterprise is on the increase.
In hydrogen addition technology, the hydrogenation metal of the catalyst that uses is divided into two kinds of noble metal and base metals usually, and base metal mainly comprises VI B and VIII family metal (as Mo, W, Ni and Co etc.) element, in the commodity hydrogenation catalyst, these metals normally exist with the form of oxidation state.Because the Hydrogenation of oxidation state metal and metallic atom is very low, only be translated into sulphided state and just there is higher Hydrogenation, therefore for the performance that makes hydrogenation catalyst reaches best, need to be vulcanized (sometimes also claiming presulfurization) to catalyst before use.
US4177136 discloses the hydrotreatment process of hydrogenation catalyst being vulcanized with elementary sulfur, with elementary sulfur, catalyst is vulcanized.The method shortcoming is that solid element sulphur all is converted into hydrogen sulfide at a lower temperature, but catalyst can not vulcanize fully at low temperatures, can not supply with the enough sulphur of catalyst during high temperature, the feed speed of hydrogen sulfide can not be controlled accurately, makes the cure efficiency of catalyst poor.
CN1082591A discloses a kind of processing hydrocarbons catalyst vulcanization method, and the method adds vulcanizing agent by solvent, and all or part of a kind of component or the similar components that contains alkene and alkene cut (for example plant oil) of this solvent.Its shortcoming makes the chain olefinic constituent separately added in solvent be difficult to obtain in refinery, and when sulfuration easy polymerization coking on hydrotreating catalyst, affect the activity of catalyst.
CN1362289A discloses a kind of vulcanization process of hydrogenation catalyst, and the method by arranging the one or more sulfurations of the hydrogen sulfide generator of the sulphur-containing substances such as troilite or elemental sulfur for catalyst of having loaded before hydrogenation reactor.Its shortcoming is to need to build separately a reactor, need to be purified hydrogen sulfide gas, needs the make-up hydrogen compressor of hydrogen sulfide corrosion resistant, and sulphur iron ore also needs subsequent treatment simultaneously.
The catalyst vulcanization method has liquid phase sulfuration and gas phase to vulcanize two kinds, and gas phase is vulcanized because not reacting with hydrocarbon molecules in sulfidation, and can at higher temperature, carry out catalyst vulcanization, generally good than the liquid phase cure efficiency.In the catalyst vulcanization process, two important indicators of vulcanizing system are temperature and concentration of hydrogen sulfide, but in actual mechanical process, and these two important indicators are not with the operator, to adjust arbitrarily, particularly at initial stage of sulfidation.For example, at the initial stage of sulfidation, catalyst is at lower temperature, just need certain density hydrogen sulfide, to prevent being difficult to again full cure after some component reduction or decomposition, but now, because temperature is lower, the vulcanizing agent of introducing can not be converted into hydrogen sulfide, therefore can cause catalyst performance not give full play to.Simultaneously, in existing catalyst vulcanization method, generally need to use the lower vulcanizing agent of hydrogenolysis temperature, also caused the vulcanizing agent range of choice limited, and the low vulcanizing agent of hydrogenolysis temperature in general volatile, toxicity is large, so potential safety hazard is larger.
Summary of the invention
For the deficiencies in the prior art, in order to reach better catalyst vulcanization effect, the invention provides a kind of start-up vulcanization method of hydrogenation plant, can guarantee in the cryogenic vulcanization stage, contain appropriate hydrogen sulfide in vulcanizing system, improve the catalyst vulcanization effect, and then improve reactivity worth.
The start-up vulcanization method of hydrogenation plant of the present invention comprises the steps:
(a), when hydrogenation plant goes into operation sulfuration, the circulating air of hydrogenation plant is divided into to two parts, i.e. first's circulating air and second portion circulating air;
(b) more than first's circulating air is heated to through heating furnace temperature that the vulcanizing agent hydrogenolysis is hydrogen sulfide, vulcanizing agent is introduced before heating furnace or after heating furnace in this part circulating air, preferably after heating furnace, introduces vulcanizing agent;
(c) second portion circulating air is through the heating of heating furnace only, and mixes through heating furnace first's circulating air of introducing vulcanizing agent, and mixed gas enters in reactor the hydrogenation catalyst in reactor is vulcanized;
(d), before hydrogen sulfide penetrates the hydrogenation catalyst bed, the beds inlet temperature, lower than 160 ℃, is preferably 80 ℃～155 ℃;
(e) after hydrogen sulfide penetrates the hydrogenation catalyst bed, conditions of vulcanization is adjusted the temperature of circulating air routinely, and the injection rate of vulcanizing agent and heating rate complete the sulfidation of catalyst.
In the inventive method, the circulating air used when hydrogenation plant goes into operation is the gases at high pressure that are rich in hydrogen in start-up process, and hydrogen purity (volume) is not less than 50%, preferably is not less than 60%, preferably is not less than 75%.In step (a), the volume ratio of the first portions circulating air and second portion circulating air is generally 1:10～10:1, and the beds inlet temperature that concrete ratio can penetrate before the hydrogenation catalyst bed according to the hydrogenolysis temperature of using vulcanizing agent and hydrogen sulfide requires to be adjusted.
In the inventive method, vulcanizing agent is the conventional vulcanizing agent used of hydrogenation process, is generally liquid sulfur-containing compound, requires the hydrogenolysis temperature for higher than 140 ℃, is generally 150 ℃～400 ℃, concrete as CS
2, the DMDS(dimethyl disulfide), SulfrZol
?54(C
8h
18s
4), the diethyl disulfide, dipropyl disulfides etc. can be also transportations and store other safer polysulfide etc.First's circulating air temperature by heating furnace by surpass the hydrogenolysis temperature of use vulcanizing agent, usually be greater than 140 ℃, preferably 150 ℃～400 ℃.Generally need to be higher than used vulcanizing agent hydrogenolysis temperature more than 10 ℃, preferably higher than vulcanizing agent hydrogenolysis temperature more than 30 ℃, being beneficial to the abundant hydrogenolysis of vulcanizing agent is hydrogen sulfide.The sulfuration dosage of introducing in step (b) is that 500～6000 μ L/L determine by beds entrance hydrogen sulfide content.
In the inventive method, the pressure of sulfidation can be operating pressure, also can be low than operating pressure, be preferably 50%～100% of operating pressure.
In the inventive method, hydrogen sulfide penetrates beds, more than the concentration of hydrogen sulfide that refers to reactor outlet reaches 1000 μ L/L.
In this forwarding method, hydrogenation plant can be Naphtha hydrofining unit, gasoline hydrogenation device, kerosene hydrogenation device, diesel hydrotreating unit, Wax Oil Hydrogenation Unit, residual hydrogenation equipment etc.
In the inventive method, the sulfidation that step (e) hydrogen sulfide penetrates after the hydrogenation catalyst bed adopts this area conventional process and condition to carry out catalyst vulcanization.Other technology contents of concrete hydrogenation plant start-up vulcanization method is well known to those skilled in the art, can specifically determine according to the type of device, as pressed suitable programming rate, progressively improve the vulcanization reaction temperature, adjust on demand concentration of hydrogen sulfide simultaneously, when the reactor bed inlet temperature, when using the hydrogenolysis temperature of vulcanizing agent, two parts recycle hydrogen can be merged into to normal recycle hydrogen, all by after heating furnace, then enter hydrogenation reactor.Common conditions of vulcanization is: under 50%～100% condition of design pressure, after hydrogen sulfide penetrates in a large number (concentration of hydrogen sulfide is greater than 1000 μ L/L), with ≯ 8 ℃/h(≯ expression, be not more than, being less than or equal to) speed is increased to 220～240 ℃ by the temperature of beds, and at least constant temperature sulfuration 8 hours at this temperature, control concentration of hydrogen sulfide 1000～7000 μ L/L around here, then ≯ 8 ℃/h speed is increased to 290 ℃ by the temperature of beds, control concentration of hydrogen sulfide 5000～12000 μ L/L around here, in order to make reaction bed temperature reach steadily and to be to reach the requirement of controlling concentration of hydrogen sulfide in next stage circulating air, can consider at this temperature constant temperature 0.1～4 hour, with ≯ 15 ℃/h speed, the temperature of beds is increased to 330～380 ℃ again, and at the temperature finally be raised to constant temperature at least 8 hours, control during this period concentration 10000～30000 μ L/L of hydrogen sulfide, complete above-mentioned steps, completed the pre-vulcanization process of catalyst.
In prior art in hydrogenation catalyst dry method sulfidation, circulating air only has a pipeline, inject vulcanizing agent when temperature is high, can't produce at a lower temperature hydrogen sulfide, sulfidation under low temperature does not occur in catalyst, for hydrogenation catalyst, can affect the performance of catalyst performance, the catalyst that particularly contains easy decomposition components is larger to the activity influence of catalyst.In addition, conventional hydrogenation catalyst sulfidation, inject vulcanizing agent when temperature is low, vulcanizing agent does not decompose, not only do not reach catalyst needs the requirement of hydrogen sulfide atmosphere when low temperature, and, along with the raising of temperature, vulcanizing agent decomposes in a large number and forms higher temperature wave, sulfidation to catalyst causes adverse influence, when serious, can cause because temperature rise is too high security incident.The present invention is by being divided into recycle hydrogen high temperature and low temperature two parts, it is hydrogen sulfide that high-temperature part can make the effective hydrogenolysis of vulcanizing agent of injecting, then with low temperature, partly mix, can obtain the hydrogen sulfide containing circulating air of lower temperature, guarantee to have the sulfidation of a low temperature during for the hydrogenation catalyst sulfidation, by the temperature of different circulating air and the injection rate of vulcanizing agent, can realize preferably the catalyst vulcanization effect and vulcanize stably start-up process.
The specific embodiment
Method of the present invention is specific as follows: at first the part of circulating air is passed through heating furnace, introduce vulcanizing agent at furnace outlet after reaching certain temperature, the vulcanizing agent hydrogenolysis obtains hydrogen sulfide gas, then this part circulating air mixes with another part circulating air, pass through beds after reaching the temperature requirement of expection, treat that hydrogen sulfide penetrates the follow-up temperature of continuing rising of beds, adjust the injection rate of vulcanizing agent according to the requirement of hydrogen sulfide content, be warming up to 230 ℃ with ≯ 3 ℃/h speed simultaneously, constant temperature sulfuration 8 hours, then 3～5 ℃/h speed is warming up to 290 ℃, be warming up to 370 ℃ with 4～6 ℃/h speed again, and at this temperature constant temperature 8 hours, complete the pre-vulcanization process of catalyst.Then introduce the glossy moist catalysis bed that goes into operation, then heat up and swap-in feedstock oil.
Further illustrate concrete condition of the present invention below by embodiment.The wax oil cut fraction hydrogenation that catalyst FF-46 is China Petroleum and Chemical Corporation Fushun Petrochemical Research Institute's development and production is processed catalyst.
Table 1 feedstock oil main character.
| Feedstock oil | Iran VGO |
| Density (20 ℃)/gcm -3 | 0.9135 |
| Boiling range/℃ | 350~545 |
| Sulfur content, wt% | 1.74 |
| Nitrogen content, μ gg -1 | 1535 |
| Aromatic hydrocarbons, wt% | 43.8 |
Table 2 embodiment process conditions and result of the test.
| Process conditions | Embodiment 1 | The reference example | Embodiment 2 | Embodiment 3 |
| Catalyst | FF-46 | FF-46 | FF-46 | FF-46 |
| The sulfidation parameter | ? | ? | ? | ? |
| Vulcanizing agent | DMDS | DMDS | DMDS | CS 2 |
| Pressure/MPa | 15.0 | 15.0 | 13.0 | 10.0 |
| The furnace outlet temperature/℃ | 180 | 180 | 190 | 175 |
| Hydrogen sulfide penetrate front reactor inlet temperature/℃ | 80 | 180 | 140 | 110 |
| Maximum bed temperature rise/℃ | 15 | 300 | 15 | 16 |
| Final curing temperature/℃ | 370 | 370 | 370 | 370 |
| Sulfuration rear catalyst activity rating condition and result | ? | ? | ? | ? |
| Feedstock oil | Iran VGO | Iran VGO | Iran VGO | Iran VGO |
| Reaction pressure/MPa | 15.7 | 15.7 | 15.7 | 15.7 |
| Volume space velocity/h -1 | 1.0 | 1.0 | 1.0 | 1.0 |
| Hydrogen to oil volume ratio | 1000 | 1000 | 1000 | 1000 |
| Average reaction temperature/℃ | 385 | 389 | 385 | 385 |
| Generate oily nitrogen content/μ gg -1 | 5.0 | 8.4 | 5.3 | 5.7 |
Can be found out by embodiment, adopt the catalyst start-up method of the inventive method, not only can effectively bring into play the activity of catalyst, but also realize the quiet run of start-up process.
Claims (10)
1. the start-up vulcanization method of a hydrogenation plant, is characterized in that comprising the steps:
(a), when hydrogenation plant goes into operation sulfuration, the circulating air of hydrogenation plant is divided into to two parts, i.e. first's circulating air and second portion circulating air;
(b) more than first's circulating air is heated to through heating furnace temperature that the vulcanizing agent hydrogenolysis is hydrogen sulfide, vulcanizing agent is introduced in this part circulating air before heating furnace or after heating furnace;
(c) second portion circulating air is through the heating of heating furnace only, and mixes through heating furnace first's circulating air of introducing vulcanizing agent, and mixed gas enters in reactor the hydrogenation catalyst in reactor is vulcanized;
(d), before hydrogen sulfide penetrates the hydrogenation catalyst bed, the beds inlet temperature, lower than 160 ℃, is preferably 80 ℃～155 ℃;
(e) after hydrogen sulfide penetrates the hydrogenation catalyst bed, conditions of vulcanization is adjusted the temperature of circulating air routinely, and the injection rate of vulcanizing agent and heating rate complete the sulfidation of catalyst.
2. in accordance with the method for claim 1, it is characterized in that: the circulating air used when hydrogenation plant goes into operation is the gases at high pressure that are rich in hydrogen in start-up process, and hydrogen purity is not less than 50% by volume.
3. it is characterized in that in accordance with the method for claim 1: in step (a), the volume ratio of the first portions circulating air and second portion circulating air is 1:10～10:1.
4. in accordance with the method for claim 1, it is characterized in that: vulcanizing agent is liquid sulfur-containing compound, and the hydrogenolysis temperature of sulfur-containing compound, higher than 140 ℃, is preferably 150 ℃～400 ℃.
5. according to the described method of claim 1 or 4, it is characterized in that: the first's circulating air temperature by heating furnace by surpass the hydrogenolysis temperature of use vulcanizing agent, need to be higher than used vulcanizing agent hydrogenolysis temperature more than 10 ℃, preferably higher than vulcanizing agent hydrogenolysis temperature more than 30 ℃.
6. by according to the power profit, wanting the described method of Ao 1 or 3, it is characterized in that: the sulfuration dosage of introducing in step (b) is that 500～6000 μ L/L determine by beds entrance hydrogen sulfide content, preferably 1000～5000 μ L/L.
7. it is characterized in that in accordance with the method for claim 1: the pressure of sulfidation is operating pressure 50%～100%.
8. in accordance with the method for claim 1, it is characterized in that: hydrogenation plant is Naphtha hydrofining unit, gasoline hydrogenation device, kerosene hydrogenation device, diesel hydrotreating unit, Wax Oil Hydrogenation Unit or residual hydrogenation equipment.
9. it is characterized in that in accordance with the method for claim 1: the sulfidation that step (e) hydrogen sulfide penetrates after the hydrogenation catalyst bed adopts this area conventional process and condition to carry out catalyst vulcanization.
10. in accordance with the method for claim 9, it is characterized in that: the sulfidation that step (e) hydrogen sulfide penetrates after the hydrogenation catalyst bed is: be warmed up to 220～240 ℃, the constant temperature sulfuration is not less than 8 hours, then continue to be warmed up to 330～380 ℃, the constant temperature sulfuration is not less than 8 hours, completes the pre-vulcanization process of catalyst.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104338565A (en) * | 2013-08-09 | 2015-02-11 | 中国石油天然气股份有限公司 | Method for presulfurizing catalytic gasoline hydrogenation catalyst |
| CN104593051A (en) * | 2013-11-03 | 2015-05-06 | 中国石油化工股份有限公司 | startup method of sulfuration type hydrogenation catalyst |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
| CN110694696A (en) * | 2019-09-11 | 2020-01-17 | 河北华丰能源科技发展有限公司 | System and method for vulcanizing heating furnace and drying furnace synchronous hydrogenation catalyst |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104338565A (en) * | 2013-08-09 | 2015-02-11 | 中国石油天然气股份有限公司 | Method for presulfurizing catalytic gasoline hydrogenation catalyst |
| CN104338565B (en) * | 2013-08-09 | 2016-08-10 | 中国石油天然气股份有限公司 | Method for presulfurizing catalytic gasoline hydrogenation catalyst |
| CN104593051A (en) * | 2013-11-03 | 2015-05-06 | 中国石油化工股份有限公司 | startup method of sulfuration type hydrogenation catalyst |
| CN104593051B (en) * | 2013-11-03 | 2016-06-22 | 中国石油化工股份有限公司 | A kind of start-up method of sulfurized hydrogenation catalyst |
| CN109913252A (en) * | 2017-12-13 | 2019-06-21 | 中国石油化工股份有限公司 | A kind of coal tar combined hydrogenation technique start-up method |
| CN109913252B (en) * | 2017-12-13 | 2020-12-08 | 中国石油化工股份有限公司 | Coal tar combined hydrogenation process starting method |
| CN110694696A (en) * | 2019-09-11 | 2020-01-17 | 河北华丰能源科技发展有限公司 | System and method for vulcanizing heating furnace and drying furnace synchronous hydrogenation catalyst |
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