CN103349999A - Oil-soluble self-vulcanizing molybdenum catalyst, and preparation method, use method and application of oil-soluble self-vulcanizing molybdenum catalyst - Google Patents
Oil-soluble self-vulcanizing molybdenum catalyst, and preparation method, use method and application of oil-soluble self-vulcanizing molybdenum catalyst Download PDFInfo
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- CN103349999A CN103349999A CN2013103175145A CN201310317514A CN103349999A CN 103349999 A CN103349999 A CN 103349999A CN 2013103175145 A CN2013103175145 A CN 2013103175145A CN 201310317514 A CN201310317514 A CN 201310317514A CN 103349999 A CN103349999 A CN 103349999A
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Abstract
The invention provides an oil-soluble self-vulcanizing molybdenum catalyst, and a preparation method, a use method and an application of the oil-soluble self-vulcanizing molybdenum catalyst. The preparation method comprises the following steps of (1) sequentially putting a molybdenum source, water, sodium sulfide, a solvent and inorganic acid in a container under the protection of nitrogen, uniformly mixing and stirring, cooling to 5-50 DEG C for reaction for 10-150min, (2) adding alkylamine and carbon disulfide, uniformly stirring, heating to 60-200 DEG C for reaction for 3-10h, and (3) after reaction, sufficiently cooling a product, performing suction filtration, sufficiently washing with methanol, and drying to obtain the oil-soluble self-vulcanizing molybdenum catalyst. The oil-soluble self-vulcanizing molybdenum catalyst can be vulcanized and decomposed to form a molybdenum disulfide active component in situ, is used for a slurry reactor hydrocracking technology for poor heavy oil with a high metal content, a high carbon residue content and a high sulfur content, can reduce the coke yield, and keeps long-period operation of a device.
Description
Technical field
The present invention relates to the catalyst of the heavy oil lighting technical process in the PETROLEUM PROCESSING technique, relate in particular to a kind of oil-soluble autovulcanization molybdenum catalyst, its preparation method, using method and application that is applicable to inferior heavy oil.
Background technology
The cracking of heavy oil slurry attitude bed hydroprocessing is that the heavy oil under high temperature, high hydrogen pressure faces the hydrogen thermocracking process.A small amount of catalyst fully contacts in reactor with hydrogen with raw material residual oil, is full back-mixing state, and the Main Function of catalyst is to suppress the green coke of residual oil in cracking process, thereby realizes the hydrogenation process of high conversion, low green coke amount.Along with the ratio of China's domestic and imported inferior heavy oil constantly increases, how to process the difficulties that these high metals (nickel, vanadium, calcium etc.), high carbon residue, full-bodied inferior heavy oil become heavy oil deep processing field face.
The domestic Heavy Oil Processing Technology that adopts mainly contains RFCC, heavy oil fixed bed hydrogenating cracking and delayed coking at present.Heavy oil catalytic cracking process and heavy oil fixed bed hydrogenating technique all have requirement to metal and the carbon residue content of raw material, are not suitable for processing high metal (nickel, vanadium, calcium etc.), high carbon residue, full-bodied inferior heavy oil; Although delay coking process can adapt to high carbon residue inferior heavy oil processing, for high-sulfur and high metal heavy oil, owing to generating a large amount of gases and lean coke, liquid yield is not high, causes economy to descend.Compare with above-mentioned heavy oil lighting process technology, the inferior heavy oil that heavy oil slurry attitude bed hydroprocessing cracking technology then can be processed high metal, high carbon residue, high-sulfur, and light oil yield is high, and especially the diesel oil distillate yield is high, good product quality.At present, the catalyst that is used for the cracking of heavy oil slurry attitude bed hydroprocessing mainly comprises two kinds of water-soluble catalyst and oil-soluble catalysts, wherein because the water-soluble catalyst dispersing technology is complicated, energy consumption is high, the industrial applications difficulty, therefore, the highly active oil-soluble catalyst of development of new, the further popularization of counterweight slurry oil attitude bed hydroprocessing cracking technology and important.
Yet, according to related documents and patent report, in the use procedure of existing heavy oil slurry attitude bed hydroprocessing cracked oil molybdenum catalyst, need to add suitable vulcanizing agent and the molybdenum in the catalyst could be changed into the molybdenum bisuphide active component, there are 2 point defects in this sulfidation: (1) has increased the mixing apparatus of vulcanizing agent and catalyst in sulfidation, increases energy consumption; (2) vulcanizing agent needs to generate hydrogen sulfide with hydrogen reaction first, hydrogen sulfide generates metal sulphide with catalyst vulcanization again, this process time is longer, can cause the catalyst granules particle diameter to become large, can not guarantee that metallic element all is converted into metal sulphide in the catalyst, reduced catalytic activity, thereby so that in the hydrogenation catalyst cracking process productive rate of coke not low.Therefore, the new oil-soluble autovulcanization molybdenum catalyst of a kind of energy of exploitation decomposition in situ formation metal sulphide is very necessary.
Summary of the invention
The object of the invention is to solve the defective that above-mentioned prior art exists, a kind of oil-soluble molybdenum catalyst that can the autovulcanization decomposition in situ forms the molybdenum bisuphide active component is provided, be oil-soluble autovulcanization molybdenum catalyst of the present invention, this catalyst can reduce the coke yield in the heavy oil slurry attitude bed hydroprocessing cracking technique.
For achieving the above object, the present invention adopts following technical scheme:
A kind of oil-soluble autovulcanization molybdenum catalyst has following formula:
R in the formula
1, R
2, R
3, R
4Be selected from identical or not identical C
4-C
15Direct-connected or branched alkyl group, x+y=3～7.
Preferably, oil-soluble autovulcanization molybdenum catalyst provided by the invention has following formula:
R is C in the formula
4-C
15Direct-connected or branched alkyl group, x=2, y=2.
A kind of oil-soluble autovulcanization molybdenum catalyst preparation method, may further comprise the steps: (1), under nitrogen protection, in order with molybdenum source, water, vulcanized sodium, solvent, inorganic acid as in the container, mixing and stirring and the cooling at 5-50 ℃, the reaction 10-150min; (2), add alkylamine and carbon disulfide, stir, be heated to 60-200 ℃ of reaction 3-10h; (3), reaction fully cools off rear suction filtration with product after finishing, and fully washs with methyl alcohol, drying obtains oil-soluble autovulcanization molybdenum catalyst.
Further, described molybdenum source is the combination of one or more materials in molybdenum trioxide, sodium molybdate or the amine molybdate.
Further, described alkylamine is the combination of one or both materials in primary amine, the secondary amine class material.
Further, described alkylamine, carbon disulfide, molybdenum source, three's mol ratio is 0.5-2.5: 0.5-3.0: 1.
Further, described solvent is one or more the combination wherein of methyl alcohol, toluene, isopropyl alcohol, benzene, benzinum.
The present invention also provides a kind of application of oil-soluble autovulcanization molybdenum catalyst, and described oil-soluble autovulcanization molybdenum catalyst is used for containing the inferior heavy slurry oil attitude bed hydroprocessing cracking technique of high metal, high carbon residue, high-sulfur.
The present invention also provides a kind of using method of oil-soluble autovulcanization molybdenum catalyst, described oil-soluble autovulcanization molybdenum catalyst adds the inferior heavy oil that contains high metal, high carbon residue, high-sulfur, and wherein the metal in the oil-soluble autovulcanization molybdenum catalyst is 50-2000 μ gg in the ratio of heavy oil feedstock
-1
Technical advantage of the present invention is as follows:
(1) oil-soluble autovulcanization molybdenum catalyst involved in the present invention is a kind of organic-molybdenum based material of catalytic performance excellence, there is no at present this material and be applied to the cracking of heavy oil slurry attitude bed hydroprocessing, use oil-soluble autovulcanization molybdenum catalyst of the present invention as inferior heavy slurry oil attitude bed hydroprocessing Cracking catalyst, can reduce coke yield, the holdout device long-term operation is (if coke yield is high, then easy occluding device shortens the cycle of operation of device).
(2) because oil-soluble autovulcanization molybdenum catalyst provided by the present invention has good dispersiveness, in the dispersing technology process, do not need to add any vulcanizing agent and can decomposition in situ form the molybdenum bisuphide active component, on the one hand, avoid the use of the mixing apparatus of vulcanizing agent and catalyst, thereby reduced energy consumption; On the other hand, reduced the reaction time of metal sulphide, make the catalyst granules particle diameter can not become large, and can guarantee that metallic element all is converted into metal sulphide in the catalyst, so that catalytic activity can not reduce, and then reduced coke yield in the heavy oil slurry attitude bed hydroprocessing cracking technique, and greatly simplified the dispersing technology of catalyst in the heavy oil slurry attitude bed hydroprocessing cracking technique, improved the whole economic efficiency of technique.
(3) oil-soluble autovulcanization molybdenum catalyst synthesis technique provided by the present invention is simple, mild condition, and the raw materials such as alkylamine are easy to get, low price, thus greatly reduce production cost.
(4) oil-soluble autovulcanization molybdenum catalyst provided by the present invention and synthetic method meet the green chemistry process route, do not relate to the environomental pollution sources such as P element, are a kind of environmentally friendly heavy oil slurry attitude bed hydroprocessing Cracking catalyst.
Description of drawings
Fig. 1 is the infrared spectrogram of the oil-soluble autovulcanization molybdenum catalyst for preparing of the present invention, by finding out 2966cm in the infrared spectrogram of synthetic product
-1For-CH
3Asymmetric stretching vibration, 2868cm
-1For-CH
3Symmetrical stretching vibration; 2927cm
-1For-CH
2-asymmetric stretching vibration; 1384cm
-1, 145.6cm
-1Flexural vibrations peak for methyl, methylene; 1175cm
-1Be the C-N stretching vibration; 1536cm
-1Be the C=S asymmetric stretching vibration; 1228cm
-1Be the C=S symmetrical stretching vibration; 966.95cm
-1Be the Mo=O characteristic absorption; 476.3cm
-1For molybdenum sulphur characteristic of a ring absorbs.Comprehensive above analysis result thinks that synthetic material is target product.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, the below is clearly and completely described the technical scheme among the present invention, and obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Embodiment 1:
0.05mol MoO under nitrogen protection
3Powder joins in the 100ml water, adds the Na of 0.05mol 15%
2Then S solution add 0.5mol toluene, and the sulfuric acid acidation with 0.01mol35% is cooled to 25 ℃, reaction 10min; Add 0.05mol di-n-butylamine and 0.05mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 85 ℃ of reaction 4h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 66%.
Embodiment 2:
Under nitrogen protection, with 0.05mol NaMoO
42H
2The O powder joins in the 100ml water, adds the Na of 0.05mol 15%
2Then S solution add 0.63mol methyl alcohol, and the sulfuric acid acidation with 0.01mol35% is cooled to 15 ℃, reaction 150min; Add 0.06mol di-n-butylamine and 0.06mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 90 ℃ of reaction 3h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 75%.
Embodiment 3:
Under nitrogen protection, with 0.05mol MoO
3Powder joins in the 100ml water, adds the Na of 0.05mol15%
2Then S solution add 0.7mol methyl alcohol, and the sulfuric acid acidation with 0.01mol35% is cooled to 10 ℃, reaction 60min; Add 0.1mol di-n-butylamine and 0.15mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 95 ℃ of reaction 5h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 80%.
Embodiment 4:
Under nitrogen protection, with 0.5mol MoO
3Powder joins in the 1000ml water, adds the Na of 0.5mol15%
2Then S solution add the 5mol isopropyl alcohol, and the sulfuric acid acidation with 0.1mol35% is cooled to 5 ℃, reaction 150min; Add 0.25mol n-dodecylamine and 0.8mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 60 ℃ of reaction 8h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 64%.
Embodiment 5:
Under nitrogen protection, with 0.05mol NaMoO
42H
2The O powder joins in the 100ml water, adds the Na of 0.05mol15%
2Then S solution add the mixture of 0.63mol methyl alcohol and isopropyl alcohol, and the sulfuric acid acidation with 0.01mol 35% is cooled to 50 ℃, reaction 10min; Add 0.125mol two cocoyl amine and 0.06mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 60 ℃ of reaction 10h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 83%.
Embodiment 6:
Under nitrogen protection, with 0.05mol MoO
3, NaMoO
42H
2O, H
8MoN
2O
4Mix powder join in the 100ml water, add the Na of 0.05mol 15%
2Then S solution add the mixed liquor of 0.7mol methyl alcohol and toluene, and the sulfuric acid acidation with 0.01mol35% is cooled to 25 ℃, reaction 60min; Add 0.1mol di-n-butylamine and 0.025mol carbon disulfide under room temperature, behind the stirring 30min, heating up is heated to 200 ℃ of reaction 10h again, after reaction finishes with product cooling, suction filtration, fully use methanol wash, get the yellow solid of oil-soluble autovulcanization molybdenum catalyst after the drying, productive rate is 70%.
Buy and execute example 7:
Getting 15g molybdenum mass fraction and be 20% oil-soluble autovulcanization molybdenum catalyst and 10g residual oil and mix, add 7g diesel oil and be in harmonious proportion, is under the 1500r/min condition in mechanical agitation speed, stirs 10min, preparation catalyst mother liquor system.This catalyst mother liquor system is added in the 15kg heavy oil feedstock, and molybdenum is 200 μ gg at the mass fraction of heavy oil feedstock
-1
Embodiment 8:
Getting 15g molybdenum mass fraction and be 20% oil-soluble autovulcanization molybdenum catalyst and 10g residual oil and mix, add 7g diesel oil and be in harmonious proportion, is under the 1500r/min condition in mechanical agitation speed, stirs 10min, preparation catalyst mother liquor system.This catalyst mother liquor system is added in the 60kg heavy oil feedstock, and molybdenum is 50 μ gg at the mass fraction of heavy oil feedstock
-1
Embodiment 9:
Getting 150g molybdenum mass fraction and be 20% oil-soluble autovulcanization molybdenum catalyst and 10g residual oil and mix, add 7g diesel oil and be in harmonious proportion, is under the 1500r/min condition in mechanical agitation speed, stirs 10min, preparation catalyst mother liquor system.This catalyst mother liquor system is added in the 15kg heavy oil feedstock, and molybdenum is 2000 μ gg at the mass fraction of heavy oil feedstock
-1
Embodiment 10-13:
Following examples use raw material to be the reduced crude of the super viscous crude of Kelamayi Feng Cheng, and its character sees Table 1.Embodiment 10,12 is respectively the conversion situation of raw material when using oil-soluble autovulcanization molybdenum catalyst, and embodiment 11,13 is the conversion situation of raw material during as catalyst with the molybdenum naphthenate that uses in the prior art.As shown in Table 2, compare with molybdenum naphthenate, oil-soluble autovulcanization molybdenum catalyst provided by the invention has advantages of that catalytic activity is high, it is good to press down burnt performance, in the situation of addition (in metal)≤200 μ of catalyst g/g, can control coke yield about 1.0%,＜500 ℃ of liquid product yields reach 70%-80%.
The reduced crude character of the super viscous crude of table 1 Kelamayi Feng Cheng
Table 2 autoclave evaluation result
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (9)
1. oil-soluble autovulcanization molybdenum catalyst is characterized in that having following formula:
R in the formula
1, R
2, R
3, R
4Be selected from identical or not identical C
4-C
15Direct-connected or branched alkyl group, x+y=3～7.
2. oil-soluble autovulcanization molybdenum catalyst according to claim 1 is characterized in that having following formula:
R is C in the formula
4-C
15Direct-connected or branched alkyl group, x=2, y=2.
3. oil-soluble autovulcanization molybdenum catalyst preparation method, it is characterized in that, may further comprise the steps: (1), under nitrogen protection places container with molybdenum source, water, vulcanized sodium, solvent, inorganic acid in order, mixing and stirring and cooling are reacted 10-150min at 5-50 ℃; (2), add alkylamine and carbon disulfide, stir, be heated to 60-200 ℃ of reaction 3-10h; (3), reaction fully cools off rear suction filtration with product after finishing, and fully washs with methyl alcohol, drying obtains oil-soluble autovulcanization molybdenum catalyst.
4. oil-soluble autovulcanization molybdenum catalyst preparation method according to claim 3 is characterized in that, described molybdenum source is the combination of one or more materials in molybdenum trioxide, sodium molybdate or the amine molybdate.
5. oil-soluble autovulcanization molybdenum catalyst preparation method as claimed in claim 3 is characterized in that, described alkylamine is the combination of one or both materials in primary amine, the secondary amine class material.
6. oil-soluble autovulcanization molybdenum catalyst preparation method as claimed in claim 3 is characterized in that, described alkylamine, carbon disulfide, molybdenum source, and three's mol ratio is 0.5-2.5: 0.5-3.0: 1.
7. oil-soluble autovulcanization molybdenum catalyst preparation method as claimed in claim 3 is characterized in that, described solvent is one or more the combination wherein of methyl alcohol, toluene, isopropyl alcohol, benzene, benzinum.
8. the application of an oil-soluble autovulcanization molybdenum catalyst is characterized in that, described oil-soluble autovulcanization molybdenum catalyst is used for containing the inferior heavy slurry oil attitude bed hydroprocessing cracking technique of high metal, high carbon residue, high-sulfur.
9. the using method of an oil-soluble autovulcanization molybdenum catalyst, it is characterized in that, described oil-soluble autovulcanization molybdenum catalyst adds the inferior heavy oil that contains high metal, high carbon residue, high-sulfur, and wherein the molybdenum in the oil-soluble autovulcanization molybdenum catalyst is 50-2000 μ gg in the ratio of heavy oil feedstock
-1
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