CN107570152A - A kind of catalyst and hydrotreating method for high calcium content heavy crude oil hydrocracking - Google Patents
A kind of catalyst and hydrotreating method for high calcium content heavy crude oil hydrocracking Download PDFInfo
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Abstract
The present invention relates to a kind of catalyst and hydrotreating method for high calcium content heavy crude oil hydrocracking, belong to technical field of petrochemical industry.The catalyst of the hydrocracking process has preferable catalytic efficiency, selectivity and the tolerance to calcium content, the global shape of the catalyst is sheet, rather than traditional graininess, so that crude oil easily forms surface erosion when having its surface flow, product calcium is taken away, alleviates the surface calcium contamination inactivation of catalyst.
Description
Technical field
The present invention relates to a kind of catalyst and hydrotreating method for high calcium content heavy crude oil hydrocracking, belong to
Technical field of petrochemical industry.
Background technology
With the application of tertiary oil recovery technology, fracture acidizing technology and calcic Oilfield Chemicals.Crude oil calcium content has substantially
The trend of rising.The influence increased to petroleum refining process of Calcium in Crude Oil content is extremely serious, not only aggravates the corrosion of equipment,
Influence safety in production.Cause catalyst loss of activity, unplanned shutdown is caused when serious.Decalcification problem oneself to turn into limitation crude oil deep
Spend one of bottleneck of processing and utilization Crude Oil.
The source of Calcium in Crude Oil may have following several respects：1st, into during oil, the calcium in ancient organisms remains in biology
In oil, this part calcium is mainly organocalcium compound, and sub-fraction is inorganic calcium compound；2nd, it is layer by layer limestone, selenolite
Or the calcic such as dolomite rock stratum, inorganic calcium salt particle therein are wrapped up by oil, this part calcium is mainly inorganic calcium compound, typically
For discrete particles and abrasion thing, or calcic particulate；3rd, in oil recovery process, because pressure declines.Temperature change.Two kinds of not phases
The water of compatibility mutually mixes.Or more than reasons such as solubility, incrustation scale is generated in oil extraction system, is carried secretly by crude oil；4th, the displacement of reservoir oil
The Oilfield Chemicals of some calcics, corrosion inhibiter, drilling well, well workover, completion fluid, scale preventative and plugging agent etc. are injected in journey.
Generally.Calcium in crude oil is divided into inorganic calcium and the major class of organic calcium two.Inorganic calcium with calcium chloride, calcium carbonate,
The forms such as calcium sulfate are present, and organic calcium exists in the form of calcium naphthenate, fatty acid calcium, phenol calcium etc., and wherein calcium is largely with oil
Organic calcium form such as the calcium naphthenate of dissolubility, phenol calcium, fatty acid calcium is present.
Calcium naphthenate and phenol in crude oil can produce obvious influence to the process being hydrocracked.Oil hydrogen addition technology is stone
Oil product is refined, the important means of modification and heavy oil lighting.Hydrogenation catalyst must carry out presulfurization before use, can just make
Catalyst has higher activity, by usually absorbing excessive hydrogen sulfide in the catalyst of presulfurization.In addition.In hydrogenating materials
Also a certain amount of sulfide is all contained.After hydrogenation reaction, these sulfide transform into hydrogen sulfide and entered in recycle hydrogen.Add
Metal calcium impurities in hydrogen feedstock, generation deposition of sulfides are reacted on beds with hydrogen sulfide, these deposits are not only
The activated centre of closed catalyst, makes hydrogenation catalyst fast deactivation or fouling, and surface area, hole area, specific surface area are reduced.More
The serious is these deposits to be easily deposited on catalyst particles intergranular, especially at the top of fixed bed bed, blocks the bed of reactor
Layer, causes reactor pressure decrease significantly to rise, serious to hinder feedstock oil and recycle hydrogen to be led by the proper flow of beds
Cause device can not normal operation.
Therefore, develop and a kind of can be resistant to the catalyst that High calcium containing crudes are hydrocracked and have great importance.
The content of the invention
The purpose of the present invention is：A kind of catalyst of the hydrocracking process applied to High calcium containing crudes is provided, it is necessary to
With preferable catalytic efficiency, selectivity and the tolerance to calcium content, the global shape of the catalyst is sheet, rather than
Traditional graininess so that crude oil easily forms surface erosion when having its surface flow, and product calcium is taken away, alleviates catalyst
Surface calcium contamination inactivation；On the other hand, a kind of hydrogenation catalyst method is additionally provided.
Technical scheme is：
The first aspect of the invention：
A kind of catalyst for high calcium content heavy crude oil hydrocracking, its preparation method comprise the following steps：
1st step, the preparation of sheet catalyst carrier：By weight, by 10~15 parts of silicon source, 15~22 parts of silicon source, nitre
Sour 0.5~2 part of bismuth, 130~150 parts of ethanol, 0.05~0.2 part of template are well mixed；Nitre acid for adjusting pH is added to 2~4
Afterwards, reacted in autoclave；After reaction terminates, solids is filtered out, is dried；Again after calcining, grinding, sheet is obtained
Catalyst carrier；
2nd step, the amination of sheet catalyst carrier surface：By weight, 2~4 parts of sheet catalyst carriers, 12 are taken
~16 parts of 3- aminopropyl triethoxysilanes (APTES), are added into 80~115 parts of dimethylbenzene, carry out back flow reaction, reaction
After end, solid is centrifugally filtered out, then after ethanol is washed, is dried in vacuo, obtains amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by 3~5 parts of amination sheet catalyst carrier plus
Enter into 100~110 parts of water, then 2~8 parts of tetrabutyl titanate, 3~5 parts of ruthenium trichloride, bismuth nitrate 2~5 are added into water
Part, after being well mixed, nitric acid is slowly added dropwise, after adjusting pH to 3~4.5, reaction is hydrolyzed, reaction filters out solid after terminating
Thing, drying, then be sintered in hydrogen atmosphere, obtain catalyst.
In the 1st described step, silicon source is one or more of in aluminium hydroxide, aluminium chloride, aluminum nitrate or aluminum sulfate
Mixing；Silicon source is selected from tetraethyl orthosilicate；Described template is selected from cetyl trimethylammonium bromide (CTAB), tetrapropyl hydrogen
The mixing of one or both of amine-oxides (TPAOH).
In the 1st described step, the concentration of nitric acid is 30~50wt%, and autoclave reaction condition is reacted at 120~150 DEG C
4~8h；Calcining heat is 500~550 DEG C, in combustion process under air or oxygen atmosphere, calcining heating rate is 2~5 DEG C/
min。
In the 2nd described step, the temperature of back flow reaction is 80~85 DEG C, and the reaction time is 3~5h.
In the 3rd described step, the concentration of nitric acid is 40~55wt%, and the temperature of hydrolysis is 45~50 DEG C, and hydrolysis is anti-
8~12h between seasonable.
In the 3rd described step, the programming rate of sintering process is 3~6 DEG C/min, and at 450~550 DEG C keep 2~
4h, natural cooling.
A kind of method of hydrotreating of the heavy crude of high calcium content, comprises the following steps：
Heavy crude is in the presence of hydrogen gas successively by hydrogenation protecting agent, HDM agent, hydrogen desulfurization agent, above-mentioned
Be hydrocracked agent reactor carry out hydrogenation reaction.
Described hydrogenation protecting agent is alumina support and the molybdenum and tungsten that are supported on the alumina support.
Described HDM being of agent alumina supporter and the nickel and cobalt being supported on the alumina support.
Described being of hydrogen desulfurization agent alumina supporter and the nickel and cobalt being supported on the alumina support.
Described hydrogenation reaction 12.0~14.0MPa of hydrogen dividing potential drop, 370~420 DEG C of reaction temperature, hydrogen to oil volume ratio 330~
1100Nm3/m3, 0.1~2.0h of volume space velocity-1。
The heavy crude API degree 18~22 of described high calcium content, viscosity (80 DEG C) 55~62mm2/ s, sulfur content 1.5
~2.0wt%, 15~25ppm of heavy metal Ni, heavy metal V1.0~3.5ppm, Ca are 300~450ppm, carbon residue is 3~
6wt%.
Beneficial effect
Hydrogenation catalyst provided by the invention has special laminated structure, has resistance to doped calcium in hydrogenation process
Effect, there is the advantages of hydro-conversion efficiency high.
In preparation process, to carrier surface carry out amination after, can with formed during sequential hydrolysis it is negatively charged
Colloidal sol formed electrostatic self-assembled, the active component in colloidal sol is carried on carrier, improve catalytic effect.
Brief description of the drawings
Fig. 1 is the electron microscope picture of sheet catalyst prepared by embodiment 3.
Embodiment
Embodiment 1
For the catalyst of high calcium content heavy crude oil hydrocracking, its preparation method comprises the following steps：
1st step, the preparation of sheet catalyst carrier：By weight, by 10 parts of aluminum nitrate, 15 parts of tetraethyl orthosilicate,
0.5 part of bismuth nitrate, 130 parts of ethanol, 0.05 part of cetyl trimethylammonium bromide are well mixed；Nitre acid for adjusting pH is added to 2
Afterwards, reacted in autoclave, the concentration of nitric acid is 30wt%, and autoclave reaction condition is to react 4h at 120 DEG C；Reaction knot
Shu Hou, solids is filtered out, dried；Again after calcining, grinding, sheet catalyst carrier is obtained, calcining heat is 500 DEG C,
In combustion process under air or oxygen atmosphere, calcining heating rate is 2 DEG C/min；
2nd step, the amination of sheet catalyst carrier surface：By weight, take 2 parts of sheet catalyst carriers, 12 parts
3- aminopropyl triethoxysilanes (APTES), add into 80 parts of dimethylbenzene, carry out back flow reaction, the temperature of back flow reaction
It it is 80 DEG C, the reaction time is 3h, after reaction terminates, centrifugally filters out solid, then after ethanol is washed, is dried in vacuo, obtain
Amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by the 3 parts of additions of amination sheet catalyst carrier extremely
In 100 parts of water, then 2 parts of tetrabutyl titanate, 3 parts of ruthenium trichloride, 2 parts of bismuth nitrate are added into water, after being well mixed, slowly dripped
Add nitric acid, the concentration of nitric acid is 40wt%, and after adjusting pH to 3, reaction is hydrolyzed, and the temperature of hydrolysis is 45 DEG C, hydrolysis
Reaction time 8h, reaction filter out solids after terminating, and dry, then are sintered in hydrogen atmosphere, obtain catalyst, sintered
The programming rate of journey is 3 DEG C/min, and 2h, natural cooling are kept at 450 DEG C.
Embodiment 2
For the catalyst of high calcium content heavy crude oil hydrocracking, its preparation method comprises the following steps：
1st step, the preparation of sheet catalyst carrier：By weight, by 15 parts of aluminum nitrate, 22 parts of tetraethyl orthosilicate,
2 parts of bismuth nitrate, 150 parts of ethanol, 0.2 part of cetyl trimethylammonium bromide are well mixed；Nitre acid for adjusting pH is added to after 4,
Reacted in autoclave, the concentration of nitric acid is 50wt%, and autoclave reaction condition is to react 8h at 150 DEG C；Reaction terminates
Afterwards, solids is filtered out, is dried；Again after calcining, grinding, sheet catalyst carrier is obtained, calcining heat is 550 DEG C, combustion
During burning under air or oxygen atmosphere, calcining heating rate is 5 DEG C/min；
2nd step, the amination of sheet catalyst carrier surface：By weight, take 4 parts of sheet catalyst carriers, 16 parts
3- aminopropyl triethoxysilanes (APTES), add into 115 parts of dimethylbenzene, carry out back flow reaction, the temperature of back flow reaction
It it is 85 DEG C, the reaction time is 5h, after reaction terminates, centrifugally filters out solid, then after ethanol is washed, is dried in vacuo, obtain
Amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by the 5 parts of additions of amination sheet catalyst carrier extremely
In 110 parts of water, then 8 parts of tetrabutyl titanate, 5 parts of ruthenium trichloride, 5 parts of bismuth nitrate are added into water, after being well mixed, slowly dripped
Add nitric acid, the concentration of nitric acid is 55wt%, after adjusting pH to 4.5, reaction is hydrolyzed, the temperature of hydrolysis is 50 DEG C, water
Reaction time 12h is solved, reaction filters out solids after terminating, and dries, then is sintered in hydrogen atmosphere, obtains catalyst, burns
The programming rate of knot process is 6 DEG C/min, and 4h, natural cooling are kept at 550 DEG C.
Embodiment 3
For the catalyst of high calcium content heavy crude oil hydrocracking, its preparation method comprises the following steps：
1st step, the preparation of sheet catalyst carrier：By weight, by 12 parts of aluminum nitrate, 18 parts of tetraethyl orthosilicate,
1 part of bismuth nitrate, 140 parts of ethanol, 0.1 part of cetyl trimethylammonium bromide are well mixed；Nitre acid for adjusting pH is added to after 3,
Reacted in autoclave, the concentration of nitric acid is 40wt%, and autoclave reaction condition is to react 5h at 140 DEG C；Reaction terminates
Afterwards, solids is filtered out, is dried；Again after calcining, grinding, sheet catalyst carrier is obtained, calcining heat is 520 DEG C, combustion
During burning under air or oxygen atmosphere, calcining heating rate is 4 DEG C/min；
2nd step, the amination of sheet catalyst carrier surface：By weight, take 3 parts of sheet catalyst carriers, 15 parts
3- aminopropyl triethoxysilanes (APTES), add into 90 parts of dimethylbenzene, carry out back flow reaction, the temperature of back flow reaction
It it is 82 DEG C, the reaction time is 4h, after reaction terminates, centrifugally filters out solid, then after ethanol is washed, is dried in vacuo, obtain
Amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by the 4 parts of additions of amination sheet catalyst carrier extremely
In 105 parts of water, then 5 parts of tetrabutyl titanate, 4 parts of ruthenium trichloride, 4 parts of bismuth nitrate are added into water, after being well mixed, slowly dripped
Add nitric acid, the concentration of nitric acid is 45wt%, and after adjusting pH to 4, reaction is hydrolyzed, and the temperature of hydrolysis is 47 DEG C, hydrolysis
Reaction time 10h, reaction filter out solids after terminating, and dry, then are sintered in hydrogen atmosphere, obtain catalyst, sinter
The programming rate of process is 5 DEG C/min, and 3h, natural cooling are kept at 480 DEG C.
Reference examples 1
Difference with embodiment 3 is：The amination processing of the 2nd step is not carried out.
1st step, the preparation of sheet catalyst carrier：By weight, by 12 parts of aluminum nitrate, 18 parts of tetraethyl orthosilicate,
1 part of bismuth nitrate, 140 parts of ethanol, 0.1 part of cetyl trimethylammonium bromide are well mixed；Nitre acid for adjusting pH is added to after 3,
Reacted in autoclave, the concentration of nitric acid is 40wt%, and autoclave reaction condition is to react 5h at 140 DEG C；Reaction terminates
Afterwards, solids is filtered out, is dried；Again after calcining, grinding, sheet catalyst carrier is obtained, calcining heat is 520 DEG C, combustion
During burning under air or oxygen atmosphere, calcining heating rate is 4 DEG C/min；
2nd step, the area load of sheet catalyst：By weight, by the 4 parts of additions of sheet catalyst carrier to 105 parts
Water in, then into water add 5 parts of tetrabutyl titanate, 4 parts of ruthenium trichloride, 4 parts of bismuth nitrate, be well mixed after, nitre is slowly added dropwise
Acid, the concentration of nitric acid is 45wt%, after adjusting pH to 4, reaction is hydrolyzed, the temperature of hydrolysis is 47 DEG C, hydrolysis
Time 10h, reaction filter out solids after terminating, and dry, then are sintered in hydrogen atmosphere, obtain catalyst, sintering process
Programming rate be 5 DEG C/min, and 3h, natural cooling are kept at 480 DEG C.
Reference examples 2
Difference with embodiment 3 is：Ruthenium trichloride is not added in 3rd step.
1st step, the preparation of sheet catalyst carrier：By weight, by 12 parts of aluminum nitrate, 18 parts of tetraethyl orthosilicate,
1 part of bismuth nitrate, 140 parts of ethanol, 0.1 part of cetyl trimethylammonium bromide are well mixed；Nitre acid for adjusting pH is added to after 3,
Reacted in autoclave, the concentration of nitric acid is 40wt%, and autoclave reaction condition is to react 5h at 140 DEG C；Reaction terminates
Afterwards, solids is filtered out, is dried；Again after calcining, grinding, sheet catalyst carrier is obtained, calcining heat is 520 DEG C, combustion
During burning under air or oxygen atmosphere, calcining heating rate is 4 DEG C/min；
2nd step, the amination of sheet catalyst carrier surface：By weight, take 3 parts of sheet catalyst carriers, 15 parts
3- aminopropyl triethoxysilanes (APTES), add into 90 parts of dimethylbenzene, carry out back flow reaction, the temperature of back flow reaction
It it is 82 DEG C, the reaction time is 4h, after reaction terminates, centrifugally filters out solid, then after ethanol is washed, is dried in vacuo, obtain
Amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by the 4 parts of additions of amination sheet catalyst carrier extremely
In 105 parts of water, then 5 parts of tetrabutyl titanate, 4 parts of bismuth nitrate are added into water, after being well mixed, nitric acid, nitric acid is slowly added dropwise
Concentration be 45wt%, adjust pH to 4 after, reaction is hydrolyzed, the temperature of hydrolysis is 47 DEG C, hydrolysis time 10h,
Reaction filters out solids after terminating, and dries, then is sintered in hydrogen atmosphere, obtains catalyst, the heating speed of sintering process
Degree is 5 DEG C/min, and 3h, natural cooling are kept at 480 DEG C.
Reference examples 3
Difference with embodiment 3 is：Using the alumina support of routine, then carry out the load of Active sites.
By weight, by particle size range in 200~350nm 4 parts of water added to 105 parts of alumina support, then
Xiang Shuizhong adds 5 parts of tetrabutyl titanate, 4 parts of ruthenium trichloride, 4 parts of bismuth nitrate, and after being well mixed, nitric acid is slowly added dropwise, nitric acid
Concentration is 45wt%, after adjusting pH to 4, reaction is hydrolyzed, the temperature of hydrolysis is 47 DEG C, hydrolysis time 10h, instead
Solids is filtered out after should terminating, is dried, then is sintered in hydrogen atmosphere, obtains catalyst, the programming rate of sintering process
It is 5 DEG C/min, and 3h, natural cooling is kept at 480 DEG C.
The heavy crude API degree 18.5 of the high calcium content of use, viscosity (80 DEG C) 57.2mm2/ s, sulfur content are
1.65wt%, heavy metal Ni 18.2ppm, heavy metal V1.27ppm, Ca 359ppm, carbon residue 4.5wt%.
The catalyst that the above embodiments and reference examples are prepared carries out hydrogenation reaction in hydrogenation reactor, hydrogenation
React hydrogen dividing potential drop 12.40MPa, 390 DEG C of reaction temperature, hydrogen to oil volume ratio 800Nm3/m3, volume space velocity 0.8h-1。
The product of after hydrogenation reaction 600h and centre sampling is detected, index is as follows：
As can be seen from the above table, catalyst provided by the invention is applied in hydrocracking process, has stable
It is not easily susceptible to the effect that calcium content deposition influences.Embodiment 3 is for reference examples 1, after 600h is run, still have compared with
The effect of good reduction oil-producing density, illustrates in continuous motion process, the catalyst can keep preferable lytic effect, pass through
Activated centre is carried on surface with can forging a good relationship by ammoxidation；Embodiment 3 is lived for reference examples 2 by introducing
Property composition ruthenium, it is possible to increase cracking effect；Embodiment 3 is for reference examples 3, due to the laminated structure that carrier has, energy
Enough it is effectively prevented from calcium to deposit on the surface of catalyst, improves operation stability.
Claims (10)
1. a kind of catalyst for high calcium content heavy crude oil hydrocracking, it is characterised in that its preparation method includes as follows
Step：
1st step, the preparation of sheet catalyst carrier：By weight, by 10~15 parts of silicon source, 15~22 parts of silicon source, bismuth nitrate
0.5~2 part, 130~150 parts of ethanol, 0.05~0.2 part of template it is well mixed；Nitre acid for adjusting pH is added to after 2~4,
Reacted in autoclave；After reaction terminates, solids is filtered out, is dried；Again after calcining, grinding, sheet catalysis is obtained
Agent carrier；
2nd step, the amination of sheet catalyst carrier surface：By weight, 2~4 parts of sheet catalyst carriers, 12~16 are taken
The 3- aminopropyl triethoxysilanes (APTES) of part, are added into 80~115 parts of dimethylbenzene, carry out back flow reaction, and reaction terminates
Afterwards, solid is centrifugally filtered out, then after ethanol is washed, is dried in vacuo, obtains amination sheet catalyst carrier；
3rd step, the area load of sheet catalyst：By weight, by 3~5 parts of additions of amination sheet catalyst carrier extremely
In 100~110 parts of water, then 2~8 parts of tetrabutyl titanate, 3~5 parts of ruthenium trichloride, 2~5 parts of bismuth nitrate are added into water, mixed
After closing uniformly, nitric acid is slowly added dropwise, after adjusting pH to 3~4.5, reaction is hydrolyzed, reaction filters out solids after terminating, and dries
It is dry, then be sintered in hydrogen atmosphere, obtain catalyst.
2. the catalyst according to claim 1 for high calcium content heavy crude oil hydrocracking, it is characterised in that described
The 1st step in, silicon source is selected from aluminium hydroxide, aluminium chloride, one or more of mixing in aluminum nitrate or aluminum sulfate；Silicon source is selected from
Tetraethyl orthosilicate；Described template is selected from cetyl trimethylammonium bromide (CTAB), TPAOH (TPAOH)
One or both of mixing.
3. the catalyst according to claim 1 for high calcium content heavy crude oil hydrocracking, it is characterised in that described
The 1st step in, the concentration of nitric acid is 30~50wt%, and autoclave reaction condition is 4~8h of reaction at 120~150 DEG C；Calcining temperature
Degree is 500~550 DEG C, and in combustion process under air or oxygen atmosphere, calcining heating rate is 2~5 DEG C/min.
4. the catalyst according to claim 1 for high calcium content heavy crude oil hydrocracking, it is characterised in that described
The 2nd step in, the temperature of back flow reaction is 80~85 DEG C, and the reaction time is 3~5h.
5. the catalyst according to claim 1 for high calcium content heavy crude oil hydrocracking, it is characterised in that described
The 3rd step in, the concentration of nitric acid is 40~55wt%, and the temperature of hydrolysis is 45~50 DEG C, 8~12h of hydrolysis time.
6. the catalyst according to claim 1 for high calcium content heavy crude oil hydrocracking, it is characterised in that described
The 3rd step in, the programming rate of sintering process is 3~6 DEG C/min, and at 450~550 DEG C keep 2~4h, natural cooling.
7. application of the catalyst described in any one of claim 1~6 in hydrocracking heavy oil.
8. a kind of method of hydrotreating of the heavy crude of high calcium content, it is characterised in that comprise the following steps：Heavy crude is in hydrogen
In the presence of enter successively by hydrogenation protecting agent, HDM agent, hydrogen desulfurization agent, the above-mentioned reactor for being hydrocracked agent
Row hydrogenation reaction.
9. method of hydrotreating according to claim 8, it is characterised in that described hydrogenation protecting agent is alumina support and born
The molybdenum and tungsten being loaded on the alumina support；Described HDM being of agent alumina supporter and it is supported on the alumina support
Nickel and cobalt；Described being of hydrogen desulfurization agent alumina supporter and the nickel and cobalt being supported on the alumina support.
10. method of hydrotreating according to claim 8, it is characterised in that described hydrogenation reaction hydrogen dividing potential drop 12.0~
14.0MPa, 370~420 DEG C of reaction temperature, 330~1100Nm of hydrogen to oil volume ratio3/m3, 0.1~2.0h of volume space velocity-1；It is described
High calcium content heavy crude API degree 18~22, viscosity (80 DEG C) 55~62mm2/ s, sulfur content are 1.5~2.0wt%, weight
15~25ppm of W metal, heavy metal V 1.0~3.5ppm, Ca are 300~450ppm, and carbon residue is 3~6wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192666A (en) * | 2018-02-14 | 2018-06-22 | 彭杰 | A kind of method that petroleum naphtha hydrogenation cracking prepares high-knock rating gasoline |
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