CN103215071A - Fischer-Tropsch oil catalyzing and upgrading method - Google Patents
Fischer-Tropsch oil catalyzing and upgrading method Download PDFInfo
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Abstract
The invention discloses a Fischer-Tropsch oil catalyzing and upgrading technology which belongs to the fields of chemical technologies and heterogeneous catalysis. The Fischer-Tropsch oil catalyzing and upgrading method comprises two parts of reaction distillation and catalytic hydrogenation upgrading. The Fischer-Tropsch oil catalyzing and upgrading technology comprises the following steps that: firstly Fischer-Tropsch oil is preheated and is injected into a flash tank; steamed oil gas enters a reaction distillation tower filled with molecular sieve and an alumina composite catalyst to undergo catalytic cracking reaction and be distilled to obtain light distillate oil, and the ratio of catalyst to oil is controlled at 1-20; the light distillate oil is pressurized again and enters a catalytic hydrogenation upgrading tower together with hydrogen, the light distillate oil and the hydrogen react under the conditions that the temperature is 240-360 DEG C, the liquid hourly space velocity is 0.3-2.0h<-1> and the ratio of hydrogen to oil is (300-1200):1 at the hydrogen pressure of 3-10Mpa, thus water-white clean flue oil with stable performance and without peculiar smell is obtained, and gasoline and diesel distillate oil is obtained through distillation. The Fischer-Tropsch oil catalyzing and upgrading technology is also suitable for heavy oil. The Fischer-Tropsch oil catalyzing and upgrading technology has the advantages that the raw material range is wide, the technological process is simple, the conversion rate and the selectivity of products are high, the production operating flexibility is large, and therefore, the Fischer-Tropsch oil catalyzing and upgrading technology has good industrial application prospect.
Description
Technical field
The invention belongs to heterogeneous catalysis field, relate to a kind of Fischer-Tropsch oil and produce the clean fuel oil tech through catalytic reaction distillation and shortening upgrading.
Background technology
Along with society and economic sustained and rapid development, the international energy demand increases substantially.Simultaneously, the energy is as the grand strategy goods and materials, and it is very big that its supply and price are influenced by International Politics, economy and military affairs.Chinese crude oil import reached 1.99 hundred million tons in 2009, and externally interdependency reaches more than 51.3%.Therefore, the exploitation oil replacement energy is one of feasible measure that solves oil shortage and national energy security.Fischer-Tropsch synthesis oil is meant the synthetic oil of the similar petroleum based fuels of producing by " Fischer-Tropsch synthetic " technology of character.At present, Fischer-Tropsch oil is mainly used in low side primary fuels such as boiler oil.No matter from the utilization of resources and environment protection angle, or economic benefit and social sustainable development all are irrational.And Fischer-Tropsch oil catalysis upgrading can not only improve the level of resources utilization, protection environment, but also can produce the clean fuel of urgent need, increases substantially economic benefit.
Fischer-Tropsch synthesis oil has no sulphur, do not have nitrogen and do not have the characteristics of aromatic hydrocarbons, is eco-friendly oil fuel and chemical.But contain a large amount of alkene and a certain amount of oxygenatedchemicals in the synthetic thick oil product, especially acid oxygenatedchemicals, serious dress ornament equipment is unfavorable for the further processing and the utilization of synthetic thick oil product.So must adopt appropriate means Fischer-Tropsch synthesis oil is carried out hydrogenation deoxidation and alkene saturated.According to the chemical constitution and the character of Fischer-Tropsch synthesis oil, we have successfully developed the new technology that clean fuel oil is produced in catalytic distillation-hydrofining-distillation.Following known technology all comes with some shortcomings:
Chinese patent CN102380391A carries out hydrogenation deacidification to Fischer-Tropsch synthesis oil, and catalyzer is CuO/ZnO/Al
2O
3, temperature of reaction is 205-245
oC, mean pressure are 0.1MPa.The content of this complete processing weak point alkene behind hydrogenation deacidification is also very high.
Chinese patent CN10133119A has introduced a kind of Fischer-Tropsch synthesis oil and has carried out hydrogenation catalyst.Catalyzer is NiWMo, and temperature of reaction is 180-390
oC, pressure are 2-10MPa.This complete processing weak point needs to introduce the stability that non-metallic element increases catalyzer, catalyst preparation process complexity, poor repeatability in the process of preparation catalyzer.And main products lubricating oil and base oil.
Chinese patent CN1884446A has introduced the hydrocracking catalyst that is used for Tscher-Topsch synthesis of heavy wax.Catalyzer is NiWMo/HY/SAPO-11, and temperature of reaction is 320-400
oC, pressure are 3-10MPa.This complete processing has good selectivity to middle distillate, and good isomerization performance is arranged.Weak point is that temperature and pressure is higher in the reaction process, and the yield of oil product is low.
Chinese patent CN1597859A has introduced a kind of hydrogenation of Fischer-Tropsch synthesis oil deoxidation and olefins hydrogenation.Catalyzer is NiCoCuFe, and contains a lot of auxiliary agents, and temperature of reaction is 240-380
oC, pressure are 2-15MPa.This complete processing weak point needs to introduce rare earth element in the process of preparation catalyzer increase activity of such catalysts and stability, catalyst preparation process complexity, poor repeatability.And hydrogenation conditions harshness, hydrogen consumption height, the oil product light component that obtains is low, product quality is poor.
Summary of the invention
At the problem of deficiency in the Fischer-Tropsch synthesis oil course of processing and existence, the present invention is target product with the clean fuel oil, by the high-efficiency cleaning upgrading conversion of technology realization Fischer-Tropsch oil under mild conditions of reaction distillation-catalytic hydrofinishing.Specifically, Fischer-Tropsch synthesis oil catalysis upgrading technology comprises catalytic reaction distillation and shortening upgrading two portions.The at first preheating and inject flash tank of Fischer-Tropsch oil adopts the cinder and the dry gas that produce in the Fischer-Tropsch synthesis oil conversion process to heat, and the flash tank temperature is controlled at 300-600
oBetween the C.The oil gas that flash distillation is come out enters and carries out catalytic cracking reaction in the reactive distillation column that molecular sieve and aluminum oxide composite catalyst are housed and distillation obtains light ends oil, and agent-oil ratio is controlled between the 1-20; Light ends oil pressurizes and enters the shortening upgrading tower of the sulfide catalyst that oxide compound and molecular sieve composite carrier load are housed with hydrogen, at 240-360
oC, 3-10MPa hydrogen pressure, liquid air speed 0.3-2.0h
-1With hydrogen to oil volume ratio is to carry out reactions such as hydrogenation deoxidation and alkene are saturated under the 300-1200:1, obtains the oil fuel cut of color water-white, stable performance, free from extraneous odour, obtains gasoline and diesel oil distillate respectively through distillation.
Technical scheme of the present invention is as follows:
Fischer-Tropsch oil among the present invention comprises the various thick oil product that various Fischer-Tropsch synthesis obtain.Technological method of the present invention also is applicable to mink cell focus simultaneously.
The employed catalyzer of reaction distillation is molecular sieve and aluminum oxide composite catalyst among the present invention, wherein the molecular sieve molecular sieve comprises ZSM-5, y-type zeolite, mordenite and β zeolite or their mixture, molecular sieve content is determined according to the selectivity to product, is generally 1-95wt%.The size of preformed catalyst determines that according to the diameter of reaction fractionating tower the equivalent diameter of general granules of catalyst should be less than 0.1 with the ratio of reaction fractionating tower diameter.The main effect of catalyzer is macromolecular cpd and the dehydration in the selective splitting Fischer-Tropsch oil, and carries out isomerization reaction simultaneously and obtain corresponding light fuel cut.Catalyzer also is the filler of rectifying tower, is used for reacting separating of product and product cut.The sulfide catalyst that the shortening upgrading is used is loading type NiMo, NiW, and CoMo, CoW, NiMoW and CoMoW sulfide catalyst, carrier are oxide compound and the molecular sieve complex carriers with high mesopore volume, oxide compound comprises SiO
2, Al
2O
3, TiO
2, SiO
2-Al
2O
3Or Al
2O
3-TiO
2Molecular sieve is ZSM-5, y-type zeolite, mordenite and β zeolite; Oxide compound is between the 20-100% at oxide compound and molecular sieve complex carrier percentage composition.The main effect of sulfide catalyst is that hydrogenation deoxidation and alkene are saturated, oxide compound and molecular sieve complex carrier be mainly used in disperse and the stable sulfide activity mutually, simultaneously the macromole in the Fischer-Tropsch synthesis oil is carried out cracking and isomerization, and then produce the oil fuel cut that obtains color water-white, stable performance, free from extraneous odour, obtain gasoline and diesel oil distillate respectively through distillation.
The present invention generates light ends oil by reaction distillation selective splitting on oxide compound and molecular sieve composite catalyst, with light ends oil again on the sulfide catalyst of oxide compound and molecular sieve composite carrier load hydrogenation deoxidation and alkene saturated, produce the oil fuel cut of cleaning, finally obtain the technology of gasoline and diesel oil distillate respectively through distillation.The at first preheating and inject flash tank of Fischer-Tropsch oil adopts the waste residue and the combustion gas that produce in the shale oil conversion process to heat, and flash distillation still temperature is controlled between 300-600 ℃.The oil gas that distills enters and reacts in the reactive distillation column that oxide compound and molecular sieve composite catalyst are housed and distill, and agent-oil ratio is controlled between the 1-20.Technique scheme may be carried out batchwise, and also can carry out continuous operation by the switching between many stills.The mixed fraction that reaction distillation goes out enters shortening upgrading system by feedstock pump, mixes with hydrogen after interchanger and process furnace enter the shortening upgrading tower of the sulfide catalyst that oxide compound and molecular sieve composite carrier load are housed, at 240-360
oC, 3-10MPa hydrogen pressure, liquid air speed 0.3-2.0h
-1With hydrogen to oil volume ratio be that 300-1200:1 carries out reactions such as hydrogenation deoxidation and alkene are saturated, obtain the oil fuel cut of color water-white, stable performance, free from extraneous odour, obtain gasoline and diesel oil distillate respectively through distillation.
By method production of the present invention obtain gasoline fraction (＜150 ℃〉yield at 10-25%, octane value is 75-85, density 0.70-0.76g/cm
3, can be used as the blend component of gasoline.The yield of diesel oil distillate is at 75-90%, and cetane value is 55, density 0.83-0.86g/cm
3, condensation point is lower than-10 ℃, can be used as low-coagulation diesel oil No. 10.Combustion gas and cinder productive rate are not higher than 8%.
The mode of operate continuously, flexible operation, easy are adopted in catalytic distillation of the present invention, hydrofining and air distillation.
The invention has the beneficial effects as follows:
1) adopt air distillation to combine with the gas phase catalysis cracking process, the combustion gas and the cinder that make full use of process have reduced energy consumption, non-secondary pollution;
2) improve the transformation efficiency of balanced reaction by air distillation and catalytic rectification process, improved the selectivity of reaction, prolonged the Hydrobon catalyst life-span, reduced catalyst levels simultaneously;
3) first fractionation repeated hydrogenation has reduced the hydrogen consumption;
4) product yield height, wide scope of material.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Among the figure: 1 flash tank; 2 reactive distillation columns; 3 shortening upgrading towers; 4 distillation towers.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Fischer-Tropsch oil is injected the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed to react and the rectifying distillation tower, catalyzer is made up of the aluminum oxide that contains 30% ZSM-5 and 10% β zeolite, obtain the columnar product of 2.0-3.0 mm by molding bonded, length 3-8 mm, bulk density 0.65-0.80 g/mL, intensity is greater than 40 N/mm.Adopt the waste residue and the combustion gas that produce in the Fischer-Tropsch oil conversion process to heat, agent-oil ratio is controlled between the 1-20.The combustion gas that produces is used for the heating of distillation tower.Following table 1 is seen catalytic distillation material balance test-results
Following table 2 is seen catalytic distillation front and back oil property
Fischer-Tropsch oil is injected the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed to react and the rectifying distillation tower, catalyzer is made up of the aluminum oxide that contains 30% ZSM-5 and 10%Y zeolite, obtain the columnar product of 2.0-3.0 mm by molding bonded, length 3-8 mm, bulk density 0.65-0.80 g/mL, intensity is greater than 40 N/mm.Adopt the waste residue and the combustion gas that produce in the Fischer-Tropsch oil conversion process to heat, agent-oil ratio is controlled between the 1-20.The combustion gas that produces is used for the heating of distillation tower.Following table 3 is seen catalytic distillation material balance test-results
Supported cobalt molybdenum sulphide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Cobalt molybdenum sulphide precursor adopts Xiao Suangu or Cobaltous diacetate or acetylacetone cobalt and ammonium thiomolybdate.Adopt equi-volume impregnating to prepare supported cobalt molybdenum sulphide catalyzer through dipping-drying-steps such as roasting.Following table 4 is seen reaction process condition and product composition.
As shown in Table 4, oil distillate on supported cobalt molybdenum sulphide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Load-type nickel molybdenum sulphide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Nickel molybdenum sulphide precursor adopts nickelous nitrate or nickel acetate or acetylacetonate nickel and ammonium thiomolybdate.Adopt equi-volume impregnating to prepare load-type nickel molybdenum sulphide catalyzer through dipping-drying-steps such as roasting.Following table 5 is seen reaction process condition and product composition.
As shown in Table 5, oil distillate on supported cobalt molybdenum sulphide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 5
Load-type nickel tungsten sulfide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Nickel tungsten sulfide precursor adopts nickelous nitrate or nickel acetate or acetylacetonate nickel and sulfo-ammonium tungstate.Adopt equi-volume impregnating to prepare load-type nickel tungsten sulfide catalyzer through dipping-drying-steps such as roasting.Following table 6 is seen reaction process condition and product composition.
As shown in Table 6, oil distillate on load-type nickel tungsten sulfide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 6
Supported cobalt tungsten sulfide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Cobalt tungsten sulfide precursor adopts Xiao Suangu or Cobaltous diacetate or acetylacetone cobalt and sulfo-ammonium tungstate.Adopt equi-volume impregnating to prepare supported cobalt tungsten sulfide catalyzer through dipping-drying-steps such as roasting.Following table 7 is seen reaction process condition and product composition.
As shown in Table 7, oil distillate on supported cobalt molybdenum sulphide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 7
Load-type nickel molybdenum tungsten sulfide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Nickel molybdenum tungsten sulfide precursor adopts nickelous nitrate or nickel acetate or acetylacetonate nickel and ammonium thiomolybdate and sulfo-ammonium tungstate.Adopt equi-volume impregnating to prepare load-type nickel molybdenum tungsten sulfide catalyzer through dipping-drying-steps such as roasting.Following table 8 is seen reaction process condition and product composition.
As shown in Table 8, oil distillate on load-type nickel molybdenum tungsten sulfide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 8
Supported cobalt molybdenum tungsten sulfide catalyzer is a Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Cobalt molybdenum tungsten sulfide precursor adopts Xiao Suangu or Cobaltous diacetate or acetylacetone cobalt and ammonium thiomolybdate and sulfo-ammonium tungstate.Adopt equi-volume impregnating to prepare supported cobalt molybdenum tungsten sulfide catalyzer through dipping-drying-steps such as roasting.Following table 9 is seen reaction process condition and product composition.
As shown in Table 9, oil distillate on supported cobalt molybdenum tungsten sulfide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 9
Product after the hydrofining enters atmospheric distillation tower and cuts into 150 ℃ of gasoline (＜150 ℃) and diesel oil (〉 according to recovered temperature).10 tables are seen vapour, diesel oil character down
As shown in Table 10, oil distillate obtains the petrol and diesel oil distillate through atmospheric distillation.The product free from extraneous odour that obtains, gasoline that quality is high and diesel oil.
Embodiment 10
With the catalytic distillation distillate is raw material, on the basis of embodiment 1,3,10 in 3.0MPa and 280
oC carries out stability experiment, and following table 11 is seen the reaction process condition of operation in 200 hours and obtained product property at last.
200 hours experimental result as shown in Table 11, on supported cobalt molybdenum sulphide catalyzer in 280
oC hydrofining, bromine valency and acid number reduce greatly in the product that obtains, and show that supported cobalt molybdenum sulphide catalyzer has the saturated deoxy performance of good hydrogenation of olefins.The product water-white that obtains, free from extraneous odour, gasoline that quality is high and diesel oil.Meet national petrol and diesel oil standard, show the product free from extraneous odour that this technology obtains, have good stability the vapour that quality is high, diesel oil.The above results shows that technology of the present invention has satisfactory stability.
Claims (5)
1. Fischer-Tropsch oil catalysis upgrading method, comprise reaction distillation and shortening upgrading two portions, it is characterized in that: the at first preheating and inject flash tank of Fischer-Tropsch oil, steam the oil gas that comes and enter and carry out catalytic pyrolysis in the reactive distillation column that molecular sieve and aluminum oxide composite catalyst are housed and distillation obtains light ends oil, agent-oil ratio is controlled between the 1-20; The light ends oil catalytic hydrogenation reaction tower that enters the sulfide catalyst that oxide compound and molecular sieve composite carrier load are housed with hydrogen that pressurizes again carries out hydrogenation upgrading tower, at 240-360
oC, 3-10MPa hydrogen pressure, liquid air speed 0.3-2.0h
-1, hydrogen to oil volume ratio is 300-1200:1, reacts, and obtains the oil fuel cut, obtains gasoline and diesel oil respectively through distillation.
2. a kind of Fischer-Tropsch oil catalysis upgrading method according to claim 1, its feature also is: Fischer-Tropsch oil comprises the various thick oil product of Fischer-Tropsch synthesis.
3. a kind of Fischer-Tropsch oil catalysis upgrading method according to claim 1 and 2, its feature also is: the employed catalyzer of reaction distillation is molecular sieve and aluminum oxide composite catalyst, wherein molecular sieve comprises ZSM-5, y-type zeolite, mordenite, β zeolite and composition thereof, and molecular sieve content is 1-95wt%; The size of preformed catalyst determines according to the diameter of reaction fractionating tower, and the ratio of the equivalent diameter of granules of catalyst and reaction fractionating tower diameter is less than 0.1.
4. a kind of Fischer-Tropsch oil catalysis upgrading method according to claim 1 and 2, its feature also is: oxide compound that the shortening upgrading is used and molecular sieve composite carrier load sulfide catalyst are loading type NiMo, NiW, CoMo, CoW, NiMoW or CoMoW, carrier is oxide compound and molecular sieve complex carrier, and oxide compound is SiO
2, Al
2O
3, TiO
2, SiO
2-Al
2O
3Or Al
2O
3-TiO
2Molecular sieve is ZSM-5, y-type zeolite, mordenite and β zeolite; The percentage composition that oxide compound accounts for oxide compound and molecular sieve complex carrier is 20-100%.
5. a kind of Fischer-Tropsch oil catalysis upgrading method according to claim 3, its feature also is: oxide compound that the shortening upgrading is used and molecular sieve composite carrier load sulfide catalyst are loading type NiMo, NiW, CoMo, CoW, NiMoW or CoMoW, carrier is oxide compound and molecular sieve complex carrier, and oxide compound is SiO
2, Al
2O
3, TiO
2, SiO
2-Al
2O
3Or Al
2O
3-TiO
2Molecular sieve is ZSM-5, y-type zeolite, mordenite and β zeolite; The percentage composition that oxide compound accounts for oxide compound and molecular sieve complex carrier is 20-100%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105749927A (en) * | 2014-12-19 | 2016-07-13 | 易高环保能源研究院有限公司 | Non-sulfide catalyst and use thereof in hydrogenation upgrading of biological oils/greases |
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| CN1665909A (en) * | 2002-07-03 | 2005-09-07 | 埃克森美孚化学专利公司 | Process for steam cracking heavy hydrocarbon feedstocks |
| CN101899326A (en) * | 2010-05-14 | 2010-12-01 | 大连理工大学 | Shale oil catalytic upgrading method |
| CN102041067A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Hydrofining method for Fischer-Tropsch oil |
-
2013
- 2013-04-12 CN CN2013101300333A patent/CN103215071A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1665909A (en) * | 2002-07-03 | 2005-09-07 | 埃克森美孚化学专利公司 | Process for steam cracking heavy hydrocarbon feedstocks |
| CN102041067A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Hydrofining method for Fischer-Tropsch oil |
| CN101899326A (en) * | 2010-05-14 | 2010-12-01 | 大连理工大学 | Shale oil catalytic upgrading method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105749927A (en) * | 2014-12-19 | 2016-07-13 | 易高环保能源研究院有限公司 | Non-sulfide catalyst and use thereof in hydrogenation upgrading of biological oils/greases |
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Application publication date: 20130724 |