CN111548806B - Method for treating carbon deposit on surface of hydrocarbon fuel cracking furnace in two-stage mode - Google Patents
Method for treating carbon deposit on surface of hydrocarbon fuel cracking furnace in two-stage mode Download PDFInfo
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- CN111548806B CN111548806B CN202010399238.1A CN202010399238A CN111548806B CN 111548806 B CN111548806 B CN 111548806B CN 202010399238 A CN202010399238 A CN 202010399238A CN 111548806 B CN111548806 B CN 111548806B
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Abstract
The invention discloses a method for treating carbon deposition on the surface of a hydrocarbon fuel cracking furnace in a two-stage mode, which comprises the following steps: two sections of coatings are designed on the inner surface of the cracking furnace according to a certain length proportion, and the coke content on the inner surface of the cracking furnace is reduced at the cracking temperature. The design of the two-stage decoking coating is put forward for the first time in order to purposefully decoke.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and particularly relates to a two-stage method for treating carbon deposition on the surface of a hydrocarbon fuel cracking furnace.
Background
The hydrocarbon fuel is cracked under the high-temperature condition, not only a large amount of heat is released, but also various coke is generated, so that the long-time effective use of the cracking furnace is limited; in addition, another problem with coking is that it can cause a reduction in the activity of, or even complete deactivation of, the catalyst in certain catalytic cracking reactions. The coke cleaning agent is added into the fuel, which is an effective way for solving the coking of the hydrocarbon fuel; such as patent CN 105950207A; the dibenzyl diselenide has the inhibition effect on the RP-3 jet fuel supercritical thermal cracking coking, Liu national column and the like, the school report of Tianjin university, 11 months in 2017 and the like. However, the addition of decoking agents to fuels has the following problems: firstly, the pressure difference of a system fluctuates, and the stability of the cracking reaction is poor; secondly, raw materials are wasted, a decoking agent needs to be added into the fuel for each cracking, and the decoking agent such as dibenzyl diselenide and the like has high price and cannot be recycled. In the prior art, a coating is coated on the inner surface of the reactor, such as CN105885486A, but the effect of coating is not ideal, because some areas of the coated coating can prevent coking, some areas of the coated coating are coked more seriously, and the overall decoking effect of the inner surface of the cracking furnace is worse.
The applicant carries out intensive research on the condition of coke generated by pyrolysis of hydrocarbon fuel, and the distribution of the coke generated by pyrolysis of the hydrocarbon fuel along the direction from the inlet to the outlet of the cracking furnace has the following two regularity: 1. the amount of carbon deposition is small at the inlet position and increases sharply at the outlet position. 2. In the aspect of carbon deposit morphology, the carbon deposit on the inner surface of the cracking furnace section which is about 30% away from the inlet length is mainly fibrous carbon, and the carbon deposit on the inner surface of the cracking furnace section which is about 70% away from the outlet length is mainly amorphous carbon or spherical carbon.
On the basis, the coke cleaning technical scheme is provided.
Disclosure of Invention
The invention aims to overcome the defects in the background technology, provides a two-section coating combination capable of removing coke in a targeted manner aiming at the problem of carbon deposition in hydrocarbon fuel cracking, and belongs to the field of first proposal.
The invention solves the problems through the following technical scheme:
the invention discloses a method for treating carbon deposition on the surface of a hydrocarbon fuel cracking furnace in a two-stage mode, which comprises the following steps: two sections of coatings are designed on the inner surface of the cracking furnace according to a certain length proportion, and the coke content on the inner surface of the cracking furnace is reduced at the cracking temperature.
Preferably, the method of the invention uses a hydrocarbon fuel in combination with a decoking agent.
Preferably, the two-stage coating length ratio is 3: 7. The first section is close to the inlet end, and occupies 30 percent of the length; the second section is close to the outlet end and occupies 70 percent of the length.
Preferably, the first section of coating contains dibenzyl diselenide, and the second section of coating contains a composite coating of barium cerate, phosphotungstic acid and calcium tungstate.
Preferably, the mass content of the dibenzyl diselenide in the first-stage coating is 10-35 wt%; the mass content of phosphotungstic acid in the second-stage coating is 0.9-12.3 wt%, and the mass content of barium cerate in the second-stage coating is 4.6-16.5 wt%; the mass content of the calcium tungstate at the second section of coating is 4.6-16.5 wt%.
Preferably, the cracking temperature is 600-800 ℃. The fuel cracking temperature is selected from the range of 600-800 ℃ because: when the temperature is lower than 600 ℃, the fuel cracking rate is very low, and the gas production rate is very low; when the temperature is higher than 800 ℃, the coking of the fuel is very serious, the time for the reaction tube to bear high temperature is greatly shortened, the cracking reaction is not facilitated to be carried out, and the high temperature can not be generally used in practical application.
Preferably, the decoking agent is ethanol.
Preferably, the decoking agent is mixed with the hydrocarbon fuel, and the mass ratio of the decoking agent to the hydrocarbon fuel is (0.1-10): 100.
The two-section coating is realized by adopting the following specific technical scheme:
pretreatment of the inner surface of the cracking furnace: dichloromethane, ethanol, hydrochloric acid solution (1 wt%) and water are sequentially pumped into the inner surface of the pyrolysis furnace by using a peristaltic pump, the inner surface wall of the pyrolysis furnace is cleaned in a circulating flow manner, each reagent is cleaned for 20min to respectively play a role in removing organic matters, dichloromethane, etching and hydrochloric acid, then high-purity nitrogen is used for purging for 10min, and finally, tetrafluoro adhesive tapes are used for sealing two ends of the tube for later use.
(1) Preparation of coating containing dibenzyl diselenide
Uniformly mixing 1-3 parts by weight of dibenzyl diselenide, 18.6-30 parts by weight of about 30 wt% of silica sol and 5-15 parts by weight of ethanol, naturally allowing a coating solution to flow downwards through the inner surface of the cracking furnace by using a coating device, purging with 0.5MPa of nitrogen for 20s, changing the direction of the inner surface of the cracking furnace, and repeating for 4-6 times. Putting the inner surface of the coated cracking furnace into a muffle furnace with an air atmosphere, heating the inner surface of the cracking furnace to 700 ℃ from room temperature after 500min, and keeping the temperature of the inner surface at 700 ℃ for 2 h; then cooling to room temperature at the same speed to obtain the coating containing the dibenzyl diselenide. The first coating is the inner surface of the cracking furnace close to the inlet end, and occupies about 30 percent of the length.
(2) Preparation of composite coating containing barium cerate, phosphotungstic acid and calcium tungstate
Adding 5-10 parts by weight of barium carbonate and 4-8 parts by weight of cerium dioxide into 20-30 parts by weight of ethanol, soaking and ball milling for 10-20 hours, roasting the mixture at 1000-1200 ℃ for 4-8 hours, cooling to obtain a perovskite-type structural substance barium cerate, drying at 100-120 ℃ for 2-4 hours, and ball milling for 60-120 min to obtain barium cerate powder;
respectively dissolving 10-20 parts by weight of calcium chloride dihydrate and 20-25 parts by weight of sodium tungstate dihydrate in 100-200 parts by weight of deionized water, fully stirring, adding the prepared sodium tungstate solution into the calcium chloride solution, aging for 150-200 min, filtering the solution, respectively washing for 3 times by using deionized water and ethanol, then drying in an oven at 100-120 ℃ for 10-12 h, and performing ball milling for 30-60 min to obtain calcium tungstate powder;
mixing 1-3 parts by weight of barium cerate powder and 1-3 parts by weight of calcium tungstate powder, adding 0.2-2 parts by weight of phosphotungstic acid, 45-55 parts by weight of about 30 wt% alkaline silica sol, 15-25 parts by weight of ethanol and 15-25 parts by weight of deionized water into the mixture, and pouring all the mixture into a ball milling tank to perform ball milling for 30-60 min at the rotating speed of 150-300 rpm to prepare a composite coating liquid;
and (3) naturally enabling the coating liquid to flow downwards through the inner surface of the cracking furnace by using a coating device, purging for 20s with 0.5MPa of nitrogen, changing the direction of the inner surface of the cracking furnace, and repeating for 4-6 times. Curing for 30-60 min at the temperature of 100-150 ℃, then placing the material into a muffle furnace, and roasting for 2-6 h at the roasting temperature range of 500-1000 ℃ at the heating rate of 1-3 ℃/min; and then cooling to room temperature at the same speed to obtain the composite coating containing barium cerate, phosphotungstic acid and calcium tungstate. The second section is the inner surface of the cracking furnace close to the outlet end, and the occupied length proportion is about 70%.
The invention has the beneficial effects that:
1. the invention discloses a method for treating carbon deposition on the surface of a hydrocarbon fuel cracking furnace in a two-stage mode for the first time. According to a great deal of research in the early stage, aiming at the problem of carbon deposition generated by cracking of hydrocarbon fuel, the invention designs a two-section coating scheme containing different substances, and the carbon deposition generation in a cracking furnace is reduced in a targeted manner.
2. The method for treating the carbon deposition on the surface of the hydrocarbon fuel cracking furnace in the two-stage mode has three effects. The second section coating component adopted by the invention comprises perovskite and phosphotungstic acid, and the decoking agent is ethanol. On the one hand, the coating is capable of inhibiting coke deposition; on the other hand, the phosphotungstic acid can promote the ethanol to be decomposed into water vapor under the high-temperature condition, and the perovskite coating can catalyze coke and the water vapor to generate carbon vaporization reaction, so that the content of the coke is further reduced; thirdly, the addition of a proper amount of ethanol also contributes to improving the heat absorption capacity of fuel cracking.
3. The two-stage method for treating the carbon deposition on the surface of the hydrocarbon fuel cracking furnace can be used for specifically removing coke. The selenium compound in the dibenzyl diselenide contained in the first-stage coating has the function of stably combining with metal active sites such as iron, nickel and the like at high temperature so as to inhibit coking of fiber carbon; the barium cerate coating contained in the second-stage coating can effectively reduce the generation of spherical carbon.
Drawings
FIG. 1 is a schematic representation of a two-stage coating of the present invention.
FIG. 2 is a coke yield comparison of examples and comparative examples.
FIG. 3 is a gas production rate comparison of examples and comparative examples.
Wherein the abscissas of fig. 2 and 3 correspond respectively: 1-example 1; 2-example 2; 3-example 3; 4-blank test; 5-comparative example 1; 6-comparative example 2; 7-comparative example 3; 8-comparative example 4; 9-comparative example 5; 10-comparative example 6; 11-comparative example 7.
Detailed Description
The invention is further illustrated by the following examples and figures, which are intended to give a better understanding of the invention, but are not intended to limit the invention.
Example 1
(1) Preparation of the coating containing dibenzyl diselenide:
1.4 parts by weight of dibenzyldiselenide, 20 parts by weight of 30 wt% silica sol and 10.5 parts by weight of ethanol were uniformly mixed to obtain a coating solution. Enabling the coating liquid to naturally flow downwards through the inner surface of the cracking furnace by using a coating device, and replacing the inner surface direction of the cracking furnace with the coating liquid by purging with 0.5MPa nitrogen for 20 s; the coating was repeated 6 times. Putting the inner surface of the coated cracking furnace into a muffle furnace with an air atmosphere, heating the inner surface of the cracking furnace to 700 ℃ from room temperature after 500min, and keeping the temperature of the inner surface at 700 ℃ for 2 h; then cooling to room temperature at the same speed to obtain the dibenzyl diselenide coating. The mass content of dibenzyl diselenide in the coating layer was 18.9 wt%.
(2) The preparation and coating method of the barium cerate-phosphotungstic acid-calcium tungstate-containing composite coating comprises the following steps:
A. adding 6.0 parts by weight of barium carbonate and 5.2 parts by weight of cerium dioxide into 24.0 parts by weight of ethanol, soaking and ball-milling for 12 hours, roasting the mixture at 1100 ℃ for 6 hours, cooling to obtain a perovskite-type structural substance barium cerate, drying at 120 ℃ for 3 hours, and ball-milling for 60 minutes to obtain barium cerate powder;
B. respectively dissolving 17.2 parts by weight of calcium chloride dihydrate and 23.2 parts by weight of sodium tungstate dihydrate into 200 parts by weight of deionized water, fully stirring, adding the prepared sodium tungstate solution into the calcium chloride solution, aging for 180min, filtering the solution, respectively washing the solid for 3 times by using the deionized water and ethanol, then drying in an oven at 100 ℃ for 12h, and carrying out ball milling for 60min to obtain calcium tungstate powder;
C. mixing 1.7 parts by weight of the barium cerate powder obtained in the step A and 1.7 parts by weight of the calcium tungstate powder obtained in the step B, then adding 1.7 parts by weight of phosphotungstic acid, 50 parts by weight of 30 wt% alkaline silica sol, 20.0 parts by weight of ethanol and 20.9 parts by weight of deionized water, and pouring all the mixture into a ball milling tank to perform ball milling for 30min at the rotating speed of 300rpm to prepare coating liquid for later use;
D. and D, adding the coating liquid obtained in the step C into a coating device, enabling the coating liquid to naturally flow downwards through the inner surface of the cracking furnace, uniformly blowing with 0.5MPa of nitrogen, and changing the direction of the inner surface of the cracking furnace for coating. Repeating for 6 times;
E. curing the inner surface of the cracking furnace in the step D for 30min at the temperature of 100 ℃;
F. and (3) roasting the inner surface of the solidified cracking furnace in a muffle furnace at 900 ℃ for 4h, wherein the heating rate is 3 ℃/min, and then cooling to obtain the barium cerate-phosphotungstic acid-calcium tungstate composite coating.
The mass content of phosphotungstic acid in the second-stage coating is 8.5 wt%, and the mass content of barium cerate in the second-stage coating is 8.5 wt%; the mass content of the calcium tungstate in the second-stage coating is 8.5 wt%.
(3) Two-stage coating length
The total length of the reaction tube of the cracking furnace is 100 cm; the first section is a coating containing dibenzyl diselenide and is 30cm away from the inlet; the second section is a barium cerate-phosphotungstic acid-calcium tungstate composite coating which is 70cm away from the outlet.
(4) Cracking reaction results on cracking furnace
The raw materials used for cracking are all heat absorption type hydrocarbon fuels, and the flow rate is 1 g/s; the cracking temperature is 700 ℃, the pressure is 4MPa, and the cracking stabilization time is 30 min. The carbon deposit quantity in the reaction tube of the cracking furnace at the end of cracking is 0.71mg/cm2The cracking gas yield is 49.0%.
Example 2
The fuel is the same as example 1, except that ethanol is mixed with the hydrocarbon fuel, and the weight ratio of the ethanol to the hydrocarbon fuel is 5: 100. The carbon deposit quantity in the inner surface of the reaction tube of the cracking furnace at the end of cracking is 0.59mg/cm2The cracking gas yield is 52.6%.
Example 3
The fuel is similar to example 2 except that the weight ratio of ethanol to hydrocarbon fuel is 10: 100. The carbon deposit quantity in the inner surface of the reaction tube of the cracking furnace at the end of cracking is 0.78mg/cm2The cracking gas yield is 50.3%.
Blank test
The blank test is a cracking test carried out on the inner surface of the reaction tube of the cracking furnace under the conditions of no coating and no coke cleaning agent. The cracking conditions were the same as in example 1, and the amount of carbon deposited on the inner surface of the reaction tube of the cracking furnace in the cracking furnace at the end of the cracking was 59.80mg/cm2The cracking gas yield is 45.4%.
Comparative example 1
The difference of the method is that the inner surface of the reaction tube of the cracking furnace is completely provided with a first-stage coating layer, like the example 1. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 7.55mg/cm2And carbon deposits are mainly at the outlet. The cracking gas yield is 46.1%.
Comparative example 2
The difference from example 1 is that the inner surface of the cracking furnace is entirely coated with the second coating. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 2.66mg/cm2And carbon deposition is mainly at the inlet. The cracking gas yield is 47.9%.
Comparative example 3
The difference from example 1 is that the inner surface of the cracking furnace has a first coating length of 50cm and a second coating length of 50 cm. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 2.17mg/cm2And carbon deposits are mainly at the outlet. The cracking gas yield is 48.7%.
Comparative example 4
The difference from example 1 is that the first coating on the inner surface of the cracking furnace does not contain dibenzyldiselenide. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 5.09mg/cm2And carbon deposition is mainly at the inlet. The cracking gas yield is 47.9%.
Comparative example 5
Basically the same as example 1, except that the second coating on the inner surface of the cracking furnace does not contain phosphotungstic acid. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 3.60mg/cm2The cracking gas yield is 48.9%.
Comparative example 6
Basically the same as example 1, except that the second coating layer on the inner surface of the cracking furnace does not contain a calcium tungstate component. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 5.68mg/cm2The cracking gas yield is 49.0%.
Comparative example 7
Basically the same as example 1, except that the second coating layer on the inner surface of the cracking furnace does not contain barium cerate. The amount of carbon deposit on the inner surface of the cracking furnace at the end of cracking was 6.67mg/cm2The cracking gas yield is 46.1%.
Claims (5)
1. A two-stage method for treating carbon deposition on the surface of a hydrocarbon fuel cracking furnace is characterized by comprising the following steps: designing a two-section coating on the inner surface of the cracking furnace according to a certain length proportion, and reducing the coke content on the inner surface of the cracking furnace at the cracking temperature; the length ratio of the two-section type coating is 3:7, the first section coating is the inner surface of the cracking furnace close to the inlet end, and the second section coating is the inner surface of the cracking furnace close to the outlet end; the first section of coating contains dibenzyl diselenide, and the second section of coating contains a composite coating of barium cerate, phosphotungstic acid and calcium tungstate; the mass content of the dibenzyl diselenide in the first-stage coating is 10-35 wt%; the mass content of phosphotungstic acid in the second-stage coating is 0.9-12.3 wt%, and the mass content of barium cerate in the second-stage coating is 4.6-16.5 wt%; the mass content of the calcium tungstate at the second section of coating is 4.6-16.5 wt%.
2. The method of claim 1, wherein a hydrocarbon fuel is used in combination with the decoking agent.
3. The process according to claim 1 or 2, characterized in that the cracking temperature is 600-800 ℃.
4. The method of claim 2, wherein the decoking agent is ethanol.
5. The method according to claim 4, wherein the decoking agent is used by mixing the decoking agent with the hydrocarbon fuel at a mass ratio of (0.1-10): 100.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249733A (en) * | 1997-01-08 | 2000-04-05 | 赫尔克里士公司 | Metal oxide solid acids as catalysts for preparation of hydrocarbon resins |
| CN105950207A (en) * | 2016-07-07 | 2016-09-21 | 天津大学 | Method for inhibiting pipe wall coking of hydrocarbon fuel cracking furnace pipe |
| CN109777460A (en) * | 2019-01-30 | 2019-05-21 | 虞定生 | A kind of acicular petroleum coke and its processing technology |
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- 2020-05-12 CN CN202010399238.1A patent/CN111548806B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249733A (en) * | 1997-01-08 | 2000-04-05 | 赫尔克里士公司 | Metal oxide solid acids as catalysts for preparation of hydrocarbon resins |
| CN105950207A (en) * | 2016-07-07 | 2016-09-21 | 天津大学 | Method for inhibiting pipe wall coking of hydrocarbon fuel cracking furnace pipe |
| CN109777460A (en) * | 2019-01-30 | 2019-05-21 | 虞定生 | A kind of acicular petroleum coke and its processing technology |
Non-Patent Citations (2)
| Title |
|---|
| Activating ABO3-type coating by additive for coke inhibition in supercritical thermal cracking of endothermic hydrocarbon fuel;Huiying Wang等;《Fuel Processing Technology》;20191026;第1页摘要和第2页第2.3部分和第3页第2.5部分和第7页第2列第2-3段和第9页第2列第2段 * |
| 超临界条件下甲基环己烷的结焦抑制研究;王贞等;《化学推进剂与高分子材料》;20110525;摘要和第75页第2.4部分 * |
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