CN105176558B - A kind of middle coalite tar heavy metal removal consisting of phase-transferring agent and application - Google Patents
A kind of middle coalite tar heavy metal removal consisting of phase-transferring agent and application Download PDFInfo
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- CN105176558B CN105176558B CN201510556051.7A CN201510556051A CN105176558B CN 105176558 B CN105176558 B CN 105176558B CN 201510556051 A CN201510556051 A CN 201510556051A CN 105176558 B CN105176558 B CN 105176558B
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Abstract
The invention provides a kind of middle coalite tar heavy metal removal consisting of phase-transferring agent and application, the consisting of phase-transferring agent is by the weight % of organic acid 20~50, the weight % of chelating agent 30~55, the weight % of surfactant 10~30, the weight % of corrosion inhibiter 1~4 and excess water composition, its Fe that will effectively can exist in medium temperature coal tar mink cell focus with oil-soluble, the transfer of Ca elements is water miscible, and be targetedly water-soluble iron by PORPHYRIN IRON transfer, so as to remove the Fe in coal tar well, Ca metallic elements, and the present invention is conducive to the operation of electric desalting equipment safety and stability for a long time in the application of middle coalite tar heavy metal removal, total deferrization rate and decalcification rate are up to more than 95%, the removal efficiency of PORPHYRIN IRON is more up to more than 95%, the handling process follow-up to catalytic hydrogenation etc. is prevented effectively to cause harm.
Description
Technical field
It is more particularly to a kind of for coalite tar heavy metal in removing the invention belongs to coal tar processing technology field
Consisting of phase-transferring agent and its application.
Background technology
At present, China or even the whole world all suffer from energy scarcity this problem.China is coal producer maximum in the world
One of, with the rapid development of economy, China, which already turns into world energy sources, consumes big country, while demand of the market to oil product
Increasingly increase, oil supply deficiency is outstanding day by day, seek new alternative energy source imperative.Energy resource structure based on coal is not
Come in quite long-term to be difficult to change.Therefore, efficient utilize of coal has obtained extensive concern and research.Seek New-type fuel
The energy is extremely urgent, and China Shaanxi North Shaanxi produces low temperature coal in a large amount of accessory substances from coking of coal and gasification industry every year
Tar, conventional liquid fuel, such as gasoline, diesel oil are prepared by being hydrogenated with to it, so as to alleviate energy scarcity this problem.
Coal tar is an important channel of solution energy scarcity by being hydrogenated with production by lightening for vapour, diesel oil, but in hydrogenation
During, metal especially Fe, Ca in oil product can produce serious harm to catalyst.Before coal tar hydrogenating, catalyst is all
Presulfurization can be shifted to an earlier date and just carried excessive hydrogen sulfide on its activity, catalyst to improve.Fe, Ca ion in oil product can absorb
Excessive hydrogen sulfide is converted into metal sulfide on catalyst, is eventually deposited on beds, cause catalyst surface area,
The reduction of specific surface area and pore volume, causes bed pressure drop to raise.Poisoning, caking or the inactivation of catalyst can also be caused in addition
Deng, reduce catalyst service life, shorten the cycle of operation, increase hydrogenation cost.The present inventor has found in research process, northern Shensi
The oily tenor of light fraction below middle 380 DEG C of coalite tar is below 2.0 μ g/g, and directly it subsequently can be located
Reason.Therefore, only the removing of row metal need to be entered to mink cell focus before to coal tar hydrogenating, so as to alleviate coal tar cleaning equipment
Treating capacity, be conducive to the operation that cleaning equipment long-term safety is stable.
In view of the above-mentioned problems, certain references disclosing coal tar preprocess method both at home and abroad.Document coalite tar is demulsified
In dehydration research, author is using breaking methods such as heating standing, addition demulsifier, stirring, ultrasound and centrifugal treatings to low temperature
Coal tar is dehydrated, but it is difficult heavy metal element in removing coal tar.In addition, document response phase method optimization coal tar electricity is de-
In salt technique, use the center combination design principle of Responds Surface Methodology to optimize coal tar electricity on the basis of experiment of single factor and take off
Salt, dewatering process so that the coal tar tenor after final electricity is de- is 24~25 μ g/g, but with the quality to being hydrogenated with oil product
It is required that more and more higher, we need to so be conducive to follow-up processing by the control of coal tar tenor in very low scope.
The A of CN 101067012 disclose acrylic acid (ester) and acid anhydrides and amide copolymer removed in crude oil or hydrocarbon ils calcium,
Application in the metals such as iron, sodium, specifically discloses demetallated application process.Metal remover is contacted with hydrocarbon ils, then used
Electric field-chemical demulsifying process or centrifugal method realize water-oil separating, obtain removing the hydrocarbon ils of metal.The object of the metal remover is
Crude oil and hydrocarbon ils, its decalcification rate is up to 69.1%；When the iron content of feedstock oil is higher than 5 μ g/g, its deferrization rate is only up to
61.9%.
The A of CN 103642519 disclose a kind of method of coal tar low pressure demetalization dechlorination, and this method includes following step
Suddenly：Guard catalyst is loaded in fixed bed hydrogenation reactor；Hydrogen is imported from fixed bed hydrogenation reactor bottom, by coal tar
Oil is imported at the top of fixed bed hydrogenation reactor；6th pipeline is set at the top of fixed bed hydrogenation reactor, and managed to the 6th
Injection hydrogen chloride absorption solvent in line.The technique of the coal tar low pressure demetalization dechlorination is different from present invention process, its technique
It is complex.
The A of CN 1982413 disclose a kind of metal remover, and the metal remover contains organic carboxyl acid and organic phospho acid, can be with
The ferro element in hydrocarbon feed is effectively removed, deferrization rate is up to more than 95%, and can effectively remove Determination of multiple metal elements.Institute
The object for stating metal remover is hydrocarbon feed, and the organic acidic substances contained by it can cause corrosion to equipment, influence cleaning equipment
Long-term safety stable operation.
The A of CN 103937529 disclose a kind of crude oil metal remover, and its component and content are：(A) sulfonic compound 5
~60 weight %, the weight % of (B) ammonium salt compound 1~30, the weight % of (C) isocyanate ester compound 0.1~10, (D) inhibition
Agent 0.05~5%, the weight % of (E) solvent 10~90.The object of the metal remover is crude oil, and its deferrization rate and decalcification rate
Do not reach more than 90% simultaneously.
It is more currently for the metal remover of crude oil, and it is seldom for the metal remover of coal tar, especially in coal tar
Metallic iron, the method for calcium constituent removing and consisting of phase-transferring agent are very few.
The content of the invention
An object of the present invention is to provide the consisting of phase-transferring agent that a kind of stability is good, demetallization per is high, especially to porphyrin
The removing of iron.
The second object of the present invention is to provide coalite tar heavy metal during a kind of above-mentioned consisting of phase-transferring agent of application is realized
Removal methods, so as to mitigate the treating capacity of equipment, improve production efficiency.
To achieve these goals, the technical solution adopted in the present invention is as follows：
Coalite tar heavy metal removal is made up of with consisting of phase-transferring agent the raw material of following quality proportioning in this：
The content of above each component is with consisting of phase-transferring agent gross weight meter；
The organic acid is malonic acid and maleic acid, the mixed acid of tartaric acid, and wherein malonic acid accounts for organic acid gross weight
35%~40%, maleic acid accounts for the 30%~35% of organic acid gross weight, and surplus is tartaric acid；
The chelating agent is any one in aminotriacetic acid, N- (2- ethoxys) ethylenediamine triacetic acid trisodium salt and amino
The mixed liquor of any one in three methylenephosphonic acids, ethylene diamine tetra methylene phosphonic acid, wherein aminotriacetic acid account for chelating agent gross weight
65%~70%, N- (2- ethoxys) ethylenediamine triacetic acid trisodium salt accounts for the 60%~65% of chelating agent gross weight, and surplus is ammonia
The methylenephosphonic acid of base three or ethylene diamine tetra methylene phosphonic acid；
The surfactant is polypropylene glycol and diglycolamine or the mixed liquor of dimethylethanolamine, wherein polypropylene glycol
The 70%~80% of surfactant gross weight is accounted for, surplus is diglycolamine or dimethylethanolamine；
The corrosion inhibiter is any one in KI, pyridine.
The raw material of above-mentioned middle coalite tar heavy metal removal consisting of phase-transferring agent preferably following quality proportioning：
The number-average molecular weight of above-mentioned polypropylene glycol is 1000~2500.
A kind of application of above-mentioned consisting of phase-transferring agent in middle coalite tar heavy metal removal, its removing process is by following step
Rapid composition：
(1) middle coalite tar is conventionally fractionated, will be above 380 DEG C of mink cell focus with being less than or equal to 380 DEG C
Light oil separation；
(2) in the mink cell focus that implantation step (1) is separated after consisting of phase-transferring agent is mixed with water, water injection rate is heavy oil quality
6%~9%, consisting of phase-transferring agent injection rate is every gram of μ g/g of mink cell focus 100~500, is mixed, removed under electric field action metal from
Son, the de- temperature of electricity is 110~140 DEG C, and electric-field intensity is 1600~2000v/cm, and the residence time is 20~50min, is removed
The mink cell focus of metal；
(3) mink cell focus that step (2) is removed into metal is mixed with the light oil of step (1), obtains low in removing metal
Warm coal tar.
The middle coalite tar heavy metal removal of the present invention is having containing amino with the chelating agent selected by consisting of phase-transferring agent
The mixture of machine phosphonic acid and organic carboxyl acid, can be formed containing amino, carboxyl and phosphonate group with the iron ion existed in porphyrin form
More stable complex compound, is effectively water-soluble by Fe, Ca element transfer existed in medium temperature coal tar mink cell focus with oil-soluble
Property, and be targetedly water-soluble iron by PORPHYRIN IRON transfer, so that Fe, Ca metal member in removing coal tar well
Element, and the consisting of phase-transferring agent also has demulsification and demetallated double effects, reduces process costs, uses it for low in removing
The technique of heavy metal in warm coal tar is that coalite tar in northern Shensi first is carried out into cutting distillation, for higher than 380 DEG C
Mink cell focus takes off the removing into row metal Fe, Ca using one-level electricity, then electric product-stripping mechanism is mixed with the oil product less than 380 DEG C, obtains
Final demetalization coal tar, so that the treating capacity of cleaning equipment is reduced, and also its total deferrization rate and decalcification rate are above 95%,
The removal efficiency of PORPHYRIN IRON is more up to 95%, and operating cost is relatively low, and corrosivity is low, and treating capacity is reduced, and is conducive to electro-desalting
Equipment safety stablizes long-term operation, will not the handling process follow-up to catalytic hydrogenation etc. cause harm.
Embodiment
With reference to specific embodiment, the present invention is further elaborated.
Now by taking coalite tar in northern Shensi as an example, processing removing is carried out with the consisting of phase-transferring agent centering coalite tar of the present invention
The technique of its heavy metal is as follows：
(1) middle coalite tar is conventionally fractionated, will be above 380 DEG C of mink cell focus with being less than or equal to 380 DEG C
Light oil separation；
(2) in the mink cell focus that implantation step (1) is separated after consisting of phase-transferring agent is mixed with water, mix, taken off under electric field action
Except metal ion, obtain removing the mink cell focus of metal；
(3) mink cell focus that step (2) is removed into metal is mixed with the light oil of step (1), obtains low in removing metal
Warm coal tar.
It is as shown in the table for the property of coalite tar and its mink cell focus in northern Shensi：
The property of the coal tar of table 1 and its mink cell focus
Note：Density is surveyed at 25 DEG C, and viscosity is surveyed at 80 DEG C.
Embodiment 1
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 33% weight and 29% weight of 38% weight
Into mixed liquor；The mixing that chelating agent is made up of the aminotriacetic acid of 65% weight and the ATMP of 35% weight
Liquid；The mixed liquor that surfactant is made up of the polypropylene glycol of 70% weight and the diglycolamine of 30% weight, polypropylene glycol
Number-average molecular weight be 1000~2500；Corrosion inhibiter is to select KI.
Electro-desalting condition is：The de- temperature of electricity is 120 DEG C, and electric-field intensity is 1800v/cm, and the residence time is 30min, and phase turns
It is 200 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 200 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
8%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.4%, 95.8%, the removing of PORPHYRIN IRON
Rate is 95.7%.
Embodiment 2
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 35% weight and 30% weight of 35% weight
Into mixed liquor；Chelating agent is by mixing that the aminotriacetic acid of 70% weight and the ethylene diamine tetra methylene phosphonic acid of 30% weight are constituted
Close liquid；The mixed liquor that surfactant is made up of the polypropylene glycol of 75% weight and the diglycolamine of 25% weight, poly- the third two
The number-average molecular weight of alcohol is 1000~2500；Corrosion inhibiter is to select KI.
Electro-desalting condition is：The de- temperature of electricity is 120 DEG C, and electric-field intensity is 1800v/cm, and the residence time is 30min, and phase turns
It is 200 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 200 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
8%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.0%, 95.2%, the removing of PORPHYRIN IRON
Rate is 96.3%.
Embodiment 3
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 35% weight and 29% weight of 36% weight
Into mixed liquor；Chelating agent is N- (2- ethoxys) the ethylenediamine triacetic acid trisodium salts and the amino of 40% weight by 60% weight
The mixed liquor of three methylenephosphonic acids composition；Surfactant is polypropylene glycol by 80% weight and the diglycolamine of 20% weight；
Corrosion inhibiter is to select KI.
Electro-desalting condition is：The de- temperature of electricity is 120 DEG C, and electric-field intensity is 1800v/cm, and the residence time is 30min, and phase turns
It is 300 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 300 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
8%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.5%, 94.9%, the removing of PORPHYRIN IRON
Rate is 95.8%.
Embodiment 4
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 30% weight and 30% weight of 40% weight
Into mixed liquor；Chelating agent is N- (2- ethoxys) the ethylenediamine triacetic acid trisodium salts and the second two of 35% weight by 65% weight
The mixed liquor of the methylenephosphonic acid of amine four composition；Surfactant is the dimethyl second of polypropylene glycol by 75% weight and 25% weight
Hydramine；Corrosion inhibiter is to select KI.
Electro-desalting condition is：The de- temperature of electricity is 130 DEG C, and electric-field intensity is 2000v/cm, and the residence time is 40min, and phase turns
It is 100 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 300 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
7%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.4%, 95.6%, the removing of PORPHYRIN IRON
Rate is 95.1%.
Embodiment 5
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid of the malonic acid, the maleic acid of 30% weight and 30% weight of 40% weight
Constitute mixed liquor；Chelating agent constitutes mixing by the aminotriacetic acid of 70% weight and the ATMP of 30% weight
Liquid；Surfactant is made up of the polypropylene glycol of 80% weight and the diglycolamine of 20% weight；Corrosion inhibiter is to select iodate
Potassium.
Electro-desalting condition is：The de- temperature of electricity is 120 DEG C, and electric-field intensity is 1800v/cm, and the residence time is 30min, and phase turns
It is 300 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 300 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
8%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.1%, 95.7%, the removing of PORPHYRIN IRON
Rate is 95.4%.
Embodiment 6
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the mixing of the malonic acid of 40% weight, the weight of maleic acid 30% and the weight of tartaric acid 30%
Liquid；Chelating agent constitutes mixed liquor by the aminotriacetic acid of 65% weight and the ethylene diamine tetra methylene phosphonic acid of 35% weight；Table
Face activating agent constitutes mixed liquor by the weight of polypropylene glycol 75% and the weight of diglycolamine 25%；Corrosion inhibiter is to select pyridine.
Electro-desalting condition is：The de- temperature of electricity is 110 DEG C, and electric-field intensity is 1600v/cm, and the residence time is 50min, and phase turns
It is 500 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 500 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
9%.
The total deferrization rate and decalcification rate of the final coal tar of the present embodiment are respectively 95.7%, 95.1%, the removing of PORPHYRIN IRON
Rate is 95.2%.
Embodiment 7
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 34% weight and 30% weight of 36% weight
Into mixed liquor；The mixing that chelating agent is made up of the ATMP of 68% weight aminotriacetic acid and 32% weight
Liquid；Surfactant is made up of the polypropylene glycol of 70% weight and the diglycolamine of 30% weight；Corrosion inhibiter is to select iodate
Potassium.
Electro-desalting condition is：The de- temperature of electricity is 140 DEG C, and electric-field intensity is 2000v/cm, and the residence time is 20min, and phase turns
It is 400 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 400 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
6%.
Embodiment 8
Consisting of phase-transferring agent used in the present embodiment is made up of the raw material of following quality proportioning：
Wherein：Organic acid is by the tartaric acid group of the malonic acid, the maleic acid of 35% weight and 30% weight of 35% weight
Into mixed liquor；Chelating agent is N- (2- ethoxys) the ethylenediamine triacetic acid trisodiums and the amino three of 38% weight by 62% weight
The mixed liquor of methylenephosphonic acid composition；Surfactant is the diglycolamine group of polypropylene glycol by 73% weight and 27% weight
Into；Corrosion inhibiter is to select KI.
Electro-desalting condition is：The de- temperature of electricity is 100 DEG C, and electric-field intensity is 1700v/cm, and the residence time is 40min, and phase turns
It is 100 μ g/g to move the injection rate of agent, and as every gram mink cell focus contains 100 μ g consisting of phase-transferring agent, and water injection rate is heavy oil quality
9%.
In order to verify beneficial effects of the present invention, by consisting of phase-transferring agent used in above-described embodiment 1~6 respectively with commercially available ZC-
18 metal removers, GT-D07 metal removers, CY-110 metal removers and contrast medium 1, contrast medium 2, contrast medium 3 are replaced, and are handled
Coalite tar in northern Shensi, wherein：
Organic acid in contrast medium 1 selects malonic acid, and other components are same as Example 4；
Chelating agent in contrast medium 2 selects aminotriacetic acid, and other components are same as Example 5；
Surfactant in contrast medium 3 is diglycolamine, and other components are same as Example 6；
Comparative example 7 is coalite tar, other conditions and embodiment 1 in the direct consisting of phase-transferring agent processing northern Shensi with the present invention
It is identical.
Its heavy metal removing result is as shown in small table 2：
Metal remover and its corresponding heavy metal removing result used in each comparative example of table 2
| Metal remover | Total deferrization rate | Total decalcification rate | PORPHYRIN IRON removal efficiency | |
| Contrast 1 | ZC-18 | 78.7% | 70.8% | 75.5% |
| Contrast 2 | GT-D07 | 79.4% | 80.4% | 69.2% |
| Contrast 3 | CY-110 | 69.3% | 72.8% | 64.9% |
| Contrast 4 | Contrast medium 1 | 82.4% | 81.2% | 74.1% |
| Contrast 5 | Contrast medium 2 | 80.3% | 87.9% | 76.4% |
| Contrast 6 | Contrast medium 3 | 69.5% | 61.1% | 53.4% |
| Contrast 7 | It is same as Example 1 | 80.4% | 69.8% | 67.5% |
The heavy metal removing result of above-mentioned table 2 and the heavy metal removing effect of embodiments of the invention 1~6 are contrasted
Understand, the effect of consisting of phase-transferring agent removing heavy metal of the invention is substantially better than the effect of common commercially available metal remover, in addition will
The technique of electricity removing and the electricity removing of the direct coal tar of comparative example 7 is contrasted after the first fractionation of the present invention, illustrates phase of the invention
Transfer agent be directed to mink cell focus in middle coalite tar metal Fe, Ca removal effect it is higher, and the place of equipment can be reduced
Reason amount.
Claims (3)
1. a kind of middle coalite tar heavy metal removal consisting of phase-transferring agent, it is characterised in that by the raw material group of following quality proportioning
Into：
The content of above each component is with consisting of phase-transferring agent gross weight meter；
The organic acid is malonic acid and maleic acid, the mixed acid of tartaric acid, and wherein malonic acid accounts for the 35% of organic acid gross weight
~40%, maleic acid accounts for the 30%~35% of organic acid gross weight, and surplus is tartaric acid；
The chelating agent is any one in aminotriacetic acid, N- (2- ethoxys) ethylenediamine triacetic acid trisodium salt and amino front three
The mixed liquor of any one in phosphonic acids, ethylene diamine tetra methylene phosphonic acid is pitched, wherein aminotriacetic acid accounts for the 65% of chelating agent gross weight
~70%, N- (2- ethoxys) ethylenediamine triacetic acid trisodium salt accounts for the 60%~65% of chelating agent gross weight, and surplus is amino three
Methylenephosphonic acid or ethylene diamine tetra methylene phosphonic acid；
The surfactant is polypropylene glycol and diglycolamine or the mixed liquor of dimethylethanolamine, and wherein polypropylene glycol accounts for table
The 70%~80% of face total surfactant weight, surplus is diglycolamine or dimethylethanolamine, the number-average molecular weight of polypropylene glycol
For 1000~2500；
The corrosion inhibiter is any one in KI, pyridine.
2. middle coalite tar heavy metal removal consisting of phase-transferring agent according to claim 1, it is characterised in that by following
The raw material composition of quality proportioning：
3. purposes of the consisting of phase-transferring agent in middle coalite tar heavy metal removal described in a kind of claim 1, its user
Method is comprised the steps of：
(1) middle coalite tar is conventionally fractionated, will be above 380 DEG C of mink cell focus with it is light less than or equal to 380 DEG C
Matter oil separation；
(2) in the mink cell focus that implantation step (1) is separated after consisting of phase-transferring agent is mixed with water, water injection rate is the 8% of heavy oil quality,
Consisting of phase-transferring agent injection rate is every gram of μ g/g of mink cell focus 200, is mixed, and metal ion is removed under electric field action, the de- temperature of electricity is 120
DEG C, electric-field intensity is 1800v/cm, and the residence time is 30min, obtains removing the mink cell focus of metal；
(3) mink cell focus that step (2) is removed into metal is mixed with the light oil of step (1), obtains removing the middle low temperature coal of metal
Tar.
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