CN101353591A - Composite desalter and use method thereof - Google Patents
Composite desalter and use method thereof Download PDFInfo
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- CN101353591A CN101353591A CNA2007101195562A CN200710119556A CN101353591A CN 101353591 A CN101353591 A CN 101353591A CN A2007101195562 A CNA2007101195562 A CN A2007101195562A CN 200710119556 A CN200710119556 A CN 200710119556A CN 101353591 A CN101353591 A CN 101353591A
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Abstract
The invention relates to a compound desalter and an application method thereof. The compound desalter comprises 1-30 percent of polymer, 20-90 percent of organic acid and the rest of water. The molecular chain of the polymer is composed of a chain segment copolymerized by styrene and unsaturated acid and a chain segment of polyether, and the two chain segments are connected by ester bonds; the organic acid is mono carboxylic acid, polybasic carboxylic acid, amino carboxylic acid, organic phosphine carboxylic acid or organic phosphine sulphonic acid. The compound desalter provided by the invention is applicable to the emulsion breaking, dehydration and demetalization of spraytex, especially the emulsion breaking, dehydration and demetalization of inferior thick oil.
Description
Technical field
The present invention relates to a kind of composite desalter and using method thereof that is used for deviating from the crude oil metallic element.
Background technology
Metallic element in the crude oil exists with forms such as water-soluble inorganic salt, mineral particle and organic compound or complex compounds, it is very big to Crude Oil Processing harm, as cause distillation cat head and condensation cooling system burn into furnace tubing and heat-exchange system fouling and cracking catalyst inactivation etc., therefore must it be removed in the electric desalting stage.The refinery technology of electric de-salting is to mix by water filling and crude oil, and inorganic salt in the crude oil and metal ion are extracted in the water, reaches the purpose of desalination at last through oily water separation.Yet, the electric desalting technology of crude oil can only be deviate from water-soluble salt and mineral particle by dehydrating of crude oil, metallic compound in the crude oil is except that sodium exists with muriate, most of metals such as calcium, magnesium, iron exist with forms such as naphthenate, phenates, exist with porphyrins or bituminous matter form and nickel, vanadium are many, therefore, only can't deviate from most of calcium, magnesium, iron in the crude oil by electric desalting technology.Reach demetallated purpose, must can be water-soluble or be scattered in the material of water by adding that metal remover changes into the organometallic compound in the crude oil.In addition, bituminous matter in the crude oil and colloid are natural water-in-oil emulsifiers, can form skin shape film in the water droplet surface adsorption, hinder the coalescent of water droplet, fully separate in order to guarantee profit, need adopt electricity, heat, chemical combined breakdown of emulsion in the electric desalting stage.In sum, in order to remove the metallic element in the crude oil to greatest extent, need to adopt metal remover on the one hand; Need to use emulsion splitter to improve oily water separation efficient as much as possible on the other hand.
At present, emulsion splitter has developed into the third generation, i.e. polymer nonionic surface active agent, and its advantage is that consumption is few, shortcoming is that specificity is strong.Along with the increase of heavy crude output, the crude oil demulsification problem is more and more outstanding, impels people constantly to seek better effects if, the emulsion splitter that universality is stronger.People find in practice, molecular weight height, the emulsion splitter better effects if of racemosus wooden fork.In the prior art, the method that improves the emulsion splitter molecular weight mainly contains 3 kinds: (1) adopts new catalyst, use tolylene diisocyanate chainextenders such as (TDI) (3) on pfpe molecule, to introduce polymerisable monomers such as vinylformic acid as triisobutyl aluminium-methyl ethyl diketone-water or triisobutyl aluminium-methyl ethyl diketone-water-oil of mirbane system (2), the pfpe molecule amount is increased by polymerization.Wherein the third method has overcome preceding two kinds of method catalyzer or chainextender costliness, and is poisonous, and the shortcoming of product dissolving difficulty is a kind of promising method.
Metal remover be can with precipitation agent, chelating or the complexing agent of metal ion effect in the crude oil.Domestic and foreign literature discloses a large amount of metal removers, as the Sodium hexametaphosphate 99 or the tripoly phosphate sodium STPP of CN1076473A report; CN8,610,728A, CN1,036,981A, US4,788,590, CN87,105,863, CN1,120,575A, CN1,120, aminocarboxylic acid or its esters, carboxylic acid or its esters etc. of report such as 575A.
CN1454967A, CN1521239A have reported the compound use of emulsion splitter and metal remover, but the emulsion splitter of the two employing is conventional emulsion splitter, and conventional emulsion splitter is not good enough to the demulsification of high bituminous matter viscous crude.Therefore, its described composite desalter is unsatisfactory for dehydration, desalination, the metal removal effect of viscous crude inferior.
Summary of the invention
The problem to be solved in the present invention provides a kind of composite desalter and using method thereof that is applicable to high bituminous matter viscous crude.
The invention provides a kind of composite desalter, comprise a kind of polymkeric substance and at least a organic acid.With the composite desalter total mass is benchmark, and polymer content is 1～30%, and organic acid content is 20～90%, and all the other are water.
Wherein, the molecular chain of polymkeric substance is made of segment and the polyether segment that vinylbenzene and unsaturated acid copolymerization form, and two kinds of segments link by ester bond.
Unsaturated acid is to contain-functional monomer of COO-group and unsaturated double-bond, is preferably in vinylformic acid, methacrylic acid, maleic anhydride, toxilic acid and the fumaric acid one or more.
Described polyethers is two blocks or the segmented copolymer of oxyethane and propylene oxide, and molecular weight is 500～30000, is preferably 800～25000, in the polyethers-and CH
2CH
2O-and-CH
2CH
2(CH
3) mass ratio of O-is 0.1～10: 1, is preferably 0.25～2.5: 1.
Described polyethers is for being one or more of initiator gained polyethers with alcohol, amine, phenol, carboxylic acid, acid amides, resol, phenol-amine resin or polyethylene polyamine, and being preferably is the mixture of initiator gained polyethers with monohydroxy-alcohol, alkyl phenolic resin, polyethylene polyamine respectively.The mass ratio of three kinds of polyethers is 1: 0.05～20: 0.05～40, be preferably 1: 0.2～5: 0.2～and 10.
Used polyethers, unsaturated acid, the cinnamic mass ratio of preparation polymkeric substance is 1～200: 1～10: 1, be preferably 10～120: 1～5: 1.
Above-mentioned polymkeric substance can adopt the preparation of two kinds of methods, and a kind of method is vinylbenzene-unsaturated acid multipolymer and polyethers to be carried out esterification prepare; Another kind method is to carry out esterification with unsaturated acid and polyethers earlier, introduces unsaturated group in polyethers, then with polyethers, unsaturated acid and styrene copolymerized.
The invention provides a kind of preparation method of above-mentioned polymkeric substance, may further comprise the steps.
(1) in the presence of initiator and alkali, two-stage polymerization propylene oxide, oxyethane obtain the polyethers of two blocks, or multistep polymerization obtain the polyethers of many blocks;
(2) step (1) gained polyethers and unsaturated acid, solvent, esterifying catalyst and stopper are added in the reactor, elevated temperature to 120～140 ℃, back flow reaction obtains esterification products;
(3) add unsaturated acid, vinylbenzene and initiator,, promptly get product after steaming solvent 65～95 ℃ of polyreactions.
Diverse initiator can obtain the polyethers of different structure, and its consumption also plays the effect of regulating the pfpe molecule amount.Initiator in the step (1) is alcohol, amine, phenol, carboxylic acid, acid amides, alkyl phenolic resin, alkylphenol polyimide resin or polyethylene polyamine.
The mol ratio of initiator in the step (1) and oxyethane, propylene oxide total amount is 1: 10～700.
Oxyethane, the general available following catalyst system of propylene oxide carry out polymerization.The anionoid polymerization of base catalysis, this class catalyzer has Na, K, Li, KOH, NaOH, and with the most use in the production is KOH and NaOH; The catalytic cationoid polymerisation of lewis acid, this type catalyst has BF
3, AlCl
3Deng; Coordinated cationic polymerization, catalyzer are metal oxygen key compound and alkaline earth metal compound etc.
Step (1) can adopt above-mentioned three class catalyzer, is preferably alkali catalyst, alkali metal hydroxide more preferably, and its consumption is 0.1～2% of oxyethane and a propylene oxide total mass.
In step (1) the gained polyethers one or more step (2) be can be used for, monohydroxy-alcohol, dibasic alcohol, alkyl phenolic resin, alkylphenol polyimide resin or polyethylene polyamine be preferably and be one or more of polyethers of initiator gained.Be the mixture of initiator gained polyethers with monohydroxy-alcohol, alkyl phenolic resin, polyethylene polyamine respectively more preferably, the mass ratio of three kinds of polyethers is 1: 0.05～20: 0.05～40, be preferably 1: 0.2～5: 0.2～and 10.
Esterification in the step (2) has water byproduct to produce, and is unfavorable for reaction thoroughly, need adopt conventional means to dewater in reaction process.Solvent in the step of the present invention (2) is conventional band aqua, as benzene,toluene,xylene, hexane or hexanaphthene, is preferably toluene; Solvent load is 50%～200% of a reactant total mass, preferred 80%～150%.
Esterifying catalyst in the step (2) is an acid catalyst, is preferably sulfuric acid, phosphoric acid or tosic acid, more preferably tosic acid.The consumption of acid catalyst is 0.1%～8% of a reactant total mass, is preferably 0.4%～1.5%.
Stopper in the step (2) is the radical polymerization stopper, preferred Resorcinol or MEHQ; The stopper consumption is 0.1%～1% of a unsaturated acid quality, preferred 0.2～0.6%.
The reaction times of step (2) is 2～24h, preferred 4～10h.
The polyethers of step (2) and (3), unsaturated acid total amount, vinylbenzene three's mass ratio is 1～200: 1～10: 1, be preferably 10～120: 1～5: 1.
The unsaturated acid amount ratio of step (2) and (3) is 1: 1～40.
Initiator in the step (3) is peroxide initiator or azo-initiator, preferred benzoyl peroxide or azo-bis-isobutyl cyanide; Initiator amount is 2%～45%, preferred 20%～35% of unsaturated acid, a vinylbenzene total mass.
Temperature of reaction in the step (3) is 65～95 ℃, preferred 80～90 ℃.
Reaction times 4～24h in the step (3), preferred 6～10h.
Organic acid among the present invention is one or more in monocarboxylic acid, di-carboxylic acid, tribasic carboxylic acid, aminocarboxylic acid, organic phosphine carboxylic acid and the organic phosphine sulfonic.
Above-mentioned monocarboxylic acid is one or more in formic acid, acetate, propionic acid and the butyric acid.
Above-mentioned di-carboxylic acid is one or more in propanedioic acid, Succinic Acid, pentanedioic acid, toxilic acid and the fumaric acid.
Above-mentioned tribasic carboxylic acid is the good and/or tartrate of citric acid.
Above-mentioned aminocarboxylic acid is nitrilotriacetic acid (NTA) and/or disodium ethylene diamine tetraacetate (EDTA).
Above-mentioned organic phosphine carboxylic acid is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (HEDP), Amino Trimethylene Phosphonic Acid (ATMP), ethylene diamine tetra methylene phosphonic acid (EDTMP), diethylene triamine pentamethylene phosphonic (DTPMP), 2-phosphonate group-1,2, one or more in 4-butane tricarboxylate (PBTC) and the 2-hydroxyl phosphino-acetate (HPAA).
Above-mentioned organic phosphine sulfonic is N, N, N '-trimethylene tri methylene phosphonic acid-quadrol-N '-hydroxypropyl sulfonic acid.
Composite desalter provided by the present invention can be used for breakdown of emulsion, dehydration and the demetalization of hydrocarbon ils.Composite desalter of the present invention can use in the demineralising process of routine, (consumption is 100～5000ppm with desalting agent in the actually operating, preferred 150～3000ppm), water filling (hydrocarbon ils quality 2～50%) and hydrocarbon ils (60～120 ℃) thorough mixing, breakdown of emulsion under heat and/or electric field action.
Composite desalter provided by the present invention comprises a kind of polymkeric substance and at least a organic acid.The molecular chain of polymkeric substance is made of segment and the polyether segment that vinylbenzene and unsaturated acid copolymerization form, and two kinds of segments link by ester bond; Organic acid is one or more in monocarboxylic acid, polycarboxylic acid, aminocarboxylic acid, organic phosphine carboxylic acid and the organic phosphine sulfonic.Composite desalter of the present invention has good breaking emulsion and dewatering, desalination and demetalization performance, is specially adapted to breakdown of emulsion, dehydration, the demetalization of viscous crude inferior.
Embodiment
Embodiment 1
Add 10g methyl alcohol and 1g potassium hydroxide in autoclave, logical nitrogen deoxygenation is warming up to 130 ℃, drip the 100g propylene oxide, when reaction pressure no longer reduces, be cooled to 110 ℃, drip 200 gram oxyethane, insulation no longer reduces until pressure, obtains two block polyether D1A.
Add 15g nonyl phenol urea formaldehyde (molecular weight is 1090) and 0.9g potassium hydroxide in autoclave, logical nitrogen deoxygenation drips the 36.2g propylene oxide, when reaction pressure no longer reduces, drips 65.8g oxyethane again, 130 ℃ of control reaction temperature, 2.3 kilograms/cm of pressure
2, treat that reacting ethylene oxide is complete, under this temperature, add the 72.5g propylene oxide, get block polyether D1B.
In autoclave, add the 5g tetraethylene pentamine, 2.4g potassium hydroxide and 400g propylene oxide, nitrogen replacement 2～3 times is warming up to 115 ℃, keeping temperature is 0 until pressure, after continuing to react half an hour, is warming up to 130 ℃, drip 200g oxyethane, no longer reduce, get block polyether D1C up to pressure.
Embodiment 2
In there-necked flask, once add vinylformic acid 4.2g, D1A polyethers 50g, tosic acid 0.62g, Resorcinol 0.012g, toluene 60ml loads onto water trap, stirs and is warmed up to 125～130 ℃, and back flow reaction 8h gets esterification products D2A solution.
Get above-mentioned D2A solution, add vinylformic acid 9.3g, vinylbenzene 3.3g, benzoyl peroxide 3.1g, toluene 50ml is at N
2Under environment and 85 ℃, reaction 8h steams solvent and gets polymerisate D2.
Embodiment 3
In there-necked flask, once add vinylformic acid 1.45g, D1A polyethers 15g, D1B polyethers 15g, D1C polyethers 15g, tosic acid 0.62g, Resorcinol 0.004g, toluene 60ml loads onto water trap, stirring is warmed up to 125～130 ℃, and back flow reaction 8h gets esterification products D3A solution.
Get above-mentioned D3A solution, add vinylformic acid 9.3g, vinylbenzene 3.3g, benzoyl peroxide 3.1g, toluene 50ml is at N
2Under environment and 85 ℃, reaction 8h steams solvent and gets polymerisate D3.
Embodiment 4
Estimate the breakdown of emulsion and the metal removal effect of desalting agent, the desalting agent prescription sees Table 1, and experiment is Kelamayi Jiu Qu viscous crude and the kerosene mixing oil with 7: 3 mixed with oil, calcium contents 154ppm, iron level 17.1ppm.
With desalting agent, water filling and be preheating to 90～100 ℃ stock oil thorough mixing 20 seconds in commercially available fruit juice agitator, pour in the cone-shaped glass desalter, adopt DPY-2 emulsion splitter competition instrument to carry out oily water separation, electric-force gradient 2000v/cm, 80 ℃ of temperature.Get after the oily water separation and take off back oil analysis water-content, measure metal content, and extract lower floor's water sample analysis oil-contg with plasma emission spectroscopy (ICP/AES).Experimental result sees Table 2.From experimental result as can be seen, desalting agent dosage 420ppm, the salts contg that takes off back crude oil is from 4.4ppmNaCl, drop to 1.1ppmNaCl, water-content 0.06% satisfies the requirement of Desalting and Dewatering from Crude Oil, desalting agent dosage 500ppm, the decalcification rate reaches 90.5%, deferrization rate 39.2%, and visible desalting agent has good desalination, dehydration is good and the demetalization performance.
Table 1
Table 2
Annotate: vestige is＜0.03%,
Embodiment 5
Estimate the breakdown of emulsion and the metal removal effect of desalting agent, the desalting agent prescription sees Table 3, and experiment is a Kelamayi Jiu Qu viscous crude with oil, calcium contents 266ppm, iron level 24.6ppm.Experimental technique is with example 4, and experimental result sees Table 4.As can be seen from Table 4, for iron calcium contents, Kelamayi Jiu Qu viscous crude that salts contg is high, desalting agent dosage 1714ppm, take off back crude oil desalting content and drop to 2.0ppm from 31.0ppm, water-content 0.2%, desalting agent dosage 2000ppm, the decalcification rate brings up to 89.4%, as seen desalting agent is to calcium iron level height, and the Kelamayi Jiu Qu viscous crude that salts contg is high has good desalination, dehydration and metal removal effect.
Table 3
Table 4
Embodiment 6
Estimate the breakdown of emulsion and the metal removal effect of desalting agent, the desalting agent prescription sees Table 5, and experiment is a huge port crude oil with oil, calcium contents 15ppm, salts contg 23.1ppmNaCl.Experimental technique is with example 4, and experimental result sees Table 6.As can be seen from Table 6, desalting agent dosage 220ppm takes off the oily salts contg 1.1ppm in back, water-content is a vestige, decalcification rate 85.4% is taken off the oily calcium contents 2.2ppm in back, and visible desalting agent also has good desalination, dehydration and metal removal effect to the relatively low huge port oil of calcium contents.
Table 5
Table 6
Claims (20)
1. a composite desalter comprises a kind of polymkeric substance and at least a organic acid and water, and polymer molecular chain is made of segment and the polyether segment that vinylbenzene and unsaturated acid copolymerization form, and two kinds of segments link by ester bond.
2. according to the described composite desalter of claim 1, it is characterized in that described unsaturated acid is one or more in vinylformic acid, methacrylic acid, maleic anhydride, toxilic acid and the fumaric acid.
3. according to the described composite desalter of claim 1, it is characterized in that described polyethers is two blocks or the segmented copolymer of oxyethane and propylene oxide.
4. according to the described composite desalter of claim 3, the molecular weight that it is characterized in that described polyethers is 500～30000.
5. according to the described composite desalter of claim 3, it is characterized in that in the described polyethers-CH
2CH
2O-and-CH
2CH
2(CH
3) mass ratio of O-is 0.1～10: 1.
6. according to the described composite desalter of claim 5, it is characterized in that in the described polyethers-CH
2CH
2O-and-CH
2CH
2(CH
3) mass ratio of O-is 0.25～2.5: 1.
7. according to the described composite desalter of claim 3, it is characterized in that described polyethers is for alcohol, amine, phenol, carboxylic acid, acid amides, resol, phenol-amine resin or polyethylene polyamine being in the initiator gained polyethers one or more.
8. according to the described composite desalter of claim 7, it is characterized in that described polyethers for being the mixture of initiator gained polyethers with monohydroxy-alcohol, alkyl phenolic resin, polyethylene polyamine respectively, the mass ratio of three kinds of polyethers is 1: 0.05～20: 0.05～40.
9. according to the described composite desalter of claim 8, the mass ratio that it is characterized in that three kinds of polyethers is 1: 0.2～5: 0.2～10.
10. according to the described composite desalter of claim 1, the mass ratio that it is characterized in that polyethers, unsaturated acid, vinylbenzene three is 1～200: 1～10: 1.
11. according to the described composite desalter of claim 10, the mass ratio that it is characterized in that polyethers, unsaturated acid, vinylbenzene three is 10～120: 1～5: 1.
12., it is characterized in that organic acid is one or more in monocarboxylic acid, di-carboxylic acid, tribasic carboxylic acid, aminocarboxylic acid, organic phosphine carboxylic acid and the organic phosphine sulfonic according to the described composite desalter of claim 1.
13., it is characterized in that monocarboxylic acid is one or more in formic acid, acetate, propionic acid and the butyric acid according to the described composite desalter of claim 12.
14., it is characterized in that di-carboxylic acid is one or more in propanedioic acid, Succinic Acid, pentanedioic acid, toxilic acid and the fumaric acid according to the described composite desalter of claim 12.
15., it is characterized in that tribasic carboxylic acid is citric acid and/or tartrate according to the described composite desalter of claim 12.
16., it is characterized in that aminocarboxylic acid is nitrilotriacetic acid and/or disodium ethylene diamine tetraacetate according to the described composite desalter of claim 12.
17. according to the described composite desalter of claim 12, it is characterized in that organic phosphine carboxylic acid is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, Amino Trimethylene Phosphonic Acid, ethylene diamine tetra methylene phosphonic acid, diethylene triamine pentamethylene phosphonic, 2-phosphonate group-1,2, one or more in 4-butane tricarboxylate and the 2-hydroxyl phosphino-acetate.
18., it is characterized in that organic phosphine sulfonic is N, N, N '-trimethylene tri methylene phosphonic acid-quadrol-N '-hydroxypropyl sulfonic acid according to the described composite desalter of claim 12.
19. according to the described composite desalter of claim 1, it is characterized in that with the composite desalter total mass be benchmark, the content of polymkeric substance is 1～30%, organic acid content is 20～90%.
20. the using method of the described composite desalter of claim 1 comprises with behind desalting agent, water filling and the hydrocarbon ils thorough mixing breakdown of emulsion under heat and/or electric field action.
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| CN102432112A (en) * | 2011-11-01 | 2012-05-02 | 中冶建筑研究总院有限公司 | Complexing agent |
| CN102453497A (en) * | 2010-10-25 | 2012-05-16 | 中国石油化工股份有限公司 | Demulsification method for hydrocarbon oil |
| CN102453496A (en) * | 2010-10-25 | 2012-05-16 | 中国石油化工股份有限公司 | Demulsifying agent and hydrocarbon oil demulsification method |
| CN101987965B (en) * | 2009-08-06 | 2013-10-16 | 中国科学院兰州化学物理研究所 | Compound desalter for crude oil |
| CN103571525A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工股份有限公司 | Composite desalting agent, and applications thereof |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4968449A (en) * | 1989-03-17 | 1990-11-06 | Nalco Chemical Company | Alkoxylated vinyl polymer demulsifiers |
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