CN101724438A - Crude oil desalting agent and preparation method thereof - Google Patents
Crude oil desalting agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a crude oil desalting agent and a preparation method thereof, which are mainly used for solving the shortcomings of poor demulsification and desalination effects, over-standard salt content in crude oil after electric desalination, large using quantity of demulsifier and the like of the conventional demulsifier. The demulsifier comprises (a) 10% by weight-60% by weight of polyoxyethylene polyoxypropylene polyethylene polyamine, (b) 1% by weight-20% by weight of asphaltene dispersant, (c) 1% by weight-20% by weight of surfactant, (d) 1% by weight-20% by weight of inorganic salt additive and (e) 10% by weight-60% by weight of solvent. The use of the desalting agent can better solve the problems, and the desalting agent has good demulsification, desalination and dehydration performances, thereby being particularly applicable to demulsification, desalination and dehydration of heavy oil with high gluey content and high asphaltene content.
Description
Technical field
The present invention relates to a kind of crude oil desalting agent and preparation method thereof, more particularly relate to a kind of prescription that is applicable to the desalting agent in the refinery crude oil electric desalting process and preparation method thereof.
Background technology
Crude oil electric desalting is the first working procedure of Crude Oil Processing, its objective is to remove salt, water and other impurity from crude oil.Emulsion splitter plays a crucial role in electric desalting profit breakdown of emulsion process, and it destroys the emulsifying film that surrounds water droplet, and stops the generation of water droplet external emulsification film.All there is narrow spectrum problem in general conventional emulsion splitter to crude oil at present, when oil property changes, the viscous crude of especially high colloid, asphalt content, the breakdown of emulsion desalting effect of conventional emulsion splitter is relatively poor, cause crude oil desalting content overproof after the electric desalting, thereby cause the fouling of water distilling apparatus overhead condensation cooling system heavy corrosion, furnace tubing and heat-exchange system, and secondary processing device catalyst deactivation etc.
Patent CN 101353591A relates to a kind of composite desalter and using method thereof.Composite desalter comprises 1～30% polymkeric substance and 20～90% organic acid, and all the other are water.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 monocarboxylic acid, polycarboxylic acid, aminocarboxylic acid, organic phosphine carboxylic acid or organic phosphine sulfonic.The composite desalter that this invention provided is applicable to breakdown of emulsion, dehydration and the demetalization of hydrocarbon ils, be specially adapted to breakdown of emulsion, dehydration, the demetalization of viscous crude inferior, but such inhibiter exist dosage big (150～3000ppm), have corrosion (organic carboxyl acid) to wait deficiency to equipment.
Summary of the invention
It is relatively poor to the present invention is directed to the conventional emulsion splitter breakdown of emulsion desalting effect that exists in the prior art, crude oil desalting content overproof after the electric desalting, shortcomings such as the emulsion splitter consumption is big provide a kind of heavy crude that is applicable to, breakdown of emulsion desalting agent of especially high colloid, high asphalt content viscous crude and preparation method thereof.
The invention provides a kind of crude oil desalting agent, it is characterized in that this desalting agent is made up of following component:
(a) polyethylene polyamine polyoxyethylene polyoxypropylene ether 10%～60%
(b) asphaltene dispersants 1%～20%
(c) tensio-active agent 1%～20%
(d) inorganic additive 1%～20%
(e) solvent 10%～60%
Above-mentioned content is weight percentage, in the desalting agent gross weight.
Wherein, the polyethylene polyamine polyoxyethylene polyoxypropylene ether described in the present invention has following structural formula:
A is 20～150 in the formula, b is 20～200, c is 20～150, n is 2～8 integer.The content of polyethylene polyamine polyoxyethylene polyoxypropylene ether is preferably 25 weight %～45 weight %.
Asphaltene dispersants described in the present invention can be wrapped in the difficult inorganic salt that remove in colloid, the bituminous matter in the thorough washing crude oil.Described asphaltene dispersants is Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, dodecyl phenol, 1,5-naphthalene disulfonate, 2, in 7-naphthalene disulfonate, nonyl phenol urea formaldehyde or the nonyl phenolic aldehyde polyimide resin any one, preferred Sodium dodecylbenzene sulfonate or nonyl phenol polyimide resin.The content of asphaltene dispersants is preferably 2 weight %～10 weight %.
Tensio-active agent described in the present invention can make polyethylene polyamine polyoxyethylene polyoxypropylene ether disperse better in oil-water mixture, improves the demulsification of desalting agent.Described tensio-active agent is any one in quaternary ammonium salt or the pyridines tensio-active agent, in preferred bromohexadecane yl pyridines, the chloro-hexadecane yl pyridines any one.The content of tensio-active agent is preferably 2 weight %～10 weight %.
Inorganic additive described in the present invention can improve the desalting efficiency of desalting agent to crude oil, and reduces oil-contg in the de-salted water.Described inorganic additive be in ammonium chloride, ammonium nitrate or the ammonium sulfate any one.The content of inorganic additive is preferably 5 weight %～15 weight %.
Solvent described in the present invention is the mixture of any one and water in methyl alcohol, ethanol or the Virahol, preferred alcohol and water mixture, and ethanol is 1: 0.5～2 with the quality ratio.The content of solvent is preferably 25 weight %～45 weight %.
The present invention also provides a kind of preparation method of described crude oil desalting agent, it is characterized in that:
(1) preparation of polyethylene polyamine polyoxyethylene polyoxypropylene ether:
A certain amount of polyethylene polyamine and catalyzer are joined in the autoclave; logical nitrogen protection; under 100～160 ℃ of temperature, slowly be pressed into a certain amount of propylene oxide with nitrogen; need logical water quench in the reaction process; react and slowly be pressed into a certain amount of oxyethane with nitrogen after 2～5 hours; 120～200 ℃ of reactions 2～5 hours; slowly be pressed into a certain amount of propylene oxide with nitrogen at last; 100～160 ℃ of reactions 2～5 hours, promptly obtain polyethylene polyamine polyoxyethylene polyoxypropylene ether after the cooling.
(2) preparation of crude oil desalting agent:
Polyethylene polyamine polyoxyethylene polyoxypropylene ether, asphaltene dispersants, tensio-active agent and the solvent of step (1) preparation are joined in the reactor 40～80 ℃ of stirrings 20～60 minutes, add inorganic additive then and stirred 20～60 minutes, be crude oil desalting agent of the present invention after mixing.
Polyethylene polyamine described in the present invention be in diethylenetriamine, triethylene tetramine or the tetraethylene pentamine any one.
Catalyzer described in the present invention is the oxide compound of the oxide compound of alkali or oxyhydroxide, alkaline-earth metal or oxyhydroxide, BF
3And AlCl
3In any one, be preferably in sodium hydroxide or the potassium hydroxide any one.
Polyethylene polyamine described in the present invention: oxyethane: the propylene oxide ratio is 1: 20～500: 20～500 (weight ratios), is preferably 1: 40～200: 40～200 (weight ratios).
Catalyst consumption described in the present invention is 0.1～2% of a raw material gross weight, is preferably 0.2～1.5% of raw material gross weight.
Crude oil desalting agent provided by the invention is used in breakdown of emulsion, desalination, the dehydration of crude oil in the refinery electric desalting process.The desalting agent consumption is 10～200 μ g/g in the crude oil electric desalting process, the salts contg of crude oil after the electric desalting can be reduced to below the 3mgNaCl/L, and water-content is reduced to below 0.2%.Crude oil desalting agent provided by the invention has good breakdown of emulsion desalination, dewatering, is particularly suitable for high colloid, the breakdown of emulsion desalination of high asphalt content viscous crude, dehydration.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but these embodiment do not limit the scope of the invention.
The evaluation method of desalting agent: be 1% the aqueous solution with the desalting agent dilute with water, get crude oil 50g and inject the 100ml desalter, inject water 2～4ml (4～8%), with a certain amount of concentration be 1% desalting agent, preheating manual mixing 200 times after 15 minutes under 120 ℃ of conditions of temperature, be electric desalting 30 minutes under 800V/cm, 120 ℃ of conditions of desalination temperature in strength of electric field then, salts contg, the water-content of cooling back sampling analysis crude oil.Analysis of moisture content adopts GB GB260 method to measure, and the saltiness analysis adopts GB GB6532 method to measure.
Wherein embodiment 1～embodiment 4 is the synthetic and preparation of desalting agent, and embodiment 5～embodiment 7 estimates the breakdown of emulsion desalting and dewatering effect of desalting agent to crude oil.
Embodiment 1
10g tetraethylene pentamine and 5g potassium hydroxide are joined in the autoclave; logical nitrogen protection; under 120 ℃ of temperature, slowly be pressed into the 400g propylene oxide with nitrogen; need logical water quench in the reaction process, reacted 2.5 hours, slowly be pressed into the oxyethane of 500g then with nitrogen; 150 ℃ of reactions 3 hours; slowly be pressed into the 400g propylene oxide with nitrogen at last,, promptly obtain polyethylene polyamine polyoxyethylene polyoxypropylene ether I after the cooling 120 ℃ of reactions 3 hours.
Embodiment 2
10g triethylene tetramine and 5g potassium hydroxide are joined in the autoclave; logical nitrogen protection; under 120 ℃ of temperature, slowly be pressed into the 300g propylene oxide with nitrogen; need logical water quench in the reaction process, reacted 3 hours, slowly be pressed into the oxyethane of 400g then with nitrogen; 150 ℃ of reactions 3 hours; slowly be pressed into the 300g propylene oxide with nitrogen at last,, promptly obtain polyethylene polyamine polyoxyethylene polyoxypropylene ether II after the cooling 120 ℃ of reactions 3 hours.
Embodiment 3
10g diethylenetriamine and 5g sodium hydroxide are joined in the autoclave; logical nitrogen protection; under 120 ℃ of temperature, slowly be pressed into the 300g propylene oxide with nitrogen; need logical water quench in the reaction process, reacted 3 hours, slowly be pressed into the oxyethane of 500g then with nitrogen; 150 ℃ of reactions 4 hours; slowly be pressed into the 400g propylene oxide with nitrogen at last,, promptly obtain polyethylene polyamine polyoxyethylene polyoxypropylene ether III after the cooling 120 ℃ of reactions 5 hours.
Embodiment 4
Mix according to the certainweight ratio with asphaltene dispersants, tensio-active agent, solvent and inorganic additive respectively and make crude oil desalting agent according to making polyethylene polyamine polyoxyethylene polyoxypropylene ether I, II or III among the embodiment 1～3, as shown in table 1.
The composition of table 1 different crude oils desalting agent
Embodiment 5
Estimate the breakdown of emulsion desalting and dewatering effect of desalting agent to Tahe Crude Oil, desalting agent is TY01 and TY02, and experiment is a Tahe Crude Oil with oil, and Tahe Crude Oil belongs to heavy high-sulfur crude oil, and density is 936.7kg/m
3, sulphur content is 2.1%; Nitrogen content is 0.46%, salts contg 274.5mgNaCl/L.Experimental result sees Table 2.
Table 2 desalting agent is to the electric desalting effect of Tahe Crude Oil
* the water-content vestige is＜0.03%
As can be seen from Table 2, desalting agent TY01 and TY02 reduce to 2.68mgNaCl/L and 2.36mgNaCl/L with Tahe heavy crude salts contg from 274.5mgNaCl/L respectively after through three grades of electric desalting, water-content is not for having, and hence one can see that, and desalting agent has good desalination, dehydrating effect to high saliferous Tahe heavy crude.
Embodiment 6
Estimate the breakdown of emulsion desalting and dewatering effect of desalting agent to isolated island viscous crude and river mouth crude oil, desalting agent is TY03 and TY04, experiment is the commingled crude (isolated island: the river mouth mass ratio is 58: 42) of isolated island viscous crude and isolated island viscous crude and river mouth crude oil with oil, and the density of Gudao crude is 0.9580g/cm
3, sulphur content is 2.0%, salts contg 62.1mgNaCl/L; The density of commingled crude is 0.9379g/cm
3, sulphur content is 1.7%, salts contg 44.6mgNaCl/L.Experimental result sees Table 3.
Table 3 desalting agent is to the electric desalting effect of isolated island viscous crude
As shown in Table 3, respectively isolated island viscous crude salts contg is reduced to 2.35mgNaCl/L and 2.48mgNaCl/L from 62.1mgNaCl/L after desalting agent TY03 and the electric desalting of TY04 process secondary, water-content all is 0.12%; Respectively commingled crude is reduced to 1.84mgNaCl/L and 2.16mgNaCl/L from 44.6mgNaCl/L, water-content is respectively 0.06% and 0.12%.Hence one can see that, and desalting agent also has good desalination, dehydrating effect to the isolated island viscous crude.
Embodiment 7
Estimate the breakdown of emulsion desalting and dewatering effect of desalting agent to northwest, Xinjiang office crude oil, desalting agent is TY05 and TY06, and experiment is a northwest office crude oil with oil, and northwest office oil density is 0.8944g/cm
3, sulphur content is 1.36%, salts contg is 44.5mg/L.Experimental result sees Table 4.
Table 4 desalting agent is to the electric desalting effect of northwest office crude oil
As shown in Table 4, respectively northwest office crude oil desalting content is reduced to 2.45mgNaCl/L and 2.48mgNaCl/L from 44.5mgNaCl/L after desalting agent TY05 and the electric desalting of TY06 process secondary, water-content all is a vestige.Hence one can see that, and desalting agent also has good desalination, dehydrating effect to northwest office crude oil.
Although the present invention has been done detailed explanation and has quoted some specific exampless as proof, to those skilled in the art, only otherwise leaving the spirit and scope of the present invention can be obvious as various changes and modifications.
Claims (13)
1. crude oil desalting agent is characterized in that being made up of following component and content:
(a) polyethylene polyamine polyoxyethylene polyoxypropylene ether 10%～60%
(b) asphaltene dispersants 1%～20%
(c) tensio-active agent 1%～20%
(d) inorganic additive 1%～20%
(e) solvent 10%～60%
Above content is weight percentage, in the desalting agent gross weight;
Wherein said polyethylene polyamine polyoxyethylene polyoxypropylene ether has following structural formula:
A is 20～150 in the formula, b is 20～200, c is 20～150, n is 2～8 integer;
Described asphaltene dispersants is Witco 1298 Soft Acid, Sodium dodecylbenzene sulfonate, dodecyl phenol, 1,5-naphthalene disulfonate, 2, any one in 7-naphthalene disulfonate, nonyl phenol urea formaldehyde or the nonyl phenolic aldehyde polyimide resin;
Described tensio-active agent is any one in quaternary ammonium salt or the pyridines tensio-active agent;
Described inorganic additive be in ammonium chloride, ammonium nitrate or the ammonium sulfate any one;
Described solvent is the mixture of any one and water in methyl alcohol, ethanol or the Virahol.
2. desalting agent according to claim 1, the content that it is characterized in that described polyethylene polyamine polyoxyethylene polyoxypropylene ether are 25 weight %～45 weight %.
3. desalting agent according to claim 1, the content that it is characterized in that described asphaltene dispersants are 2 weight %～10 weight %.
4. desalting agent according to claim 1, the content that it is characterized in that described tensio-active agent are 2 weight %～10 weight %.
5. according to described any desalting agent of claim 1～4, the content that it is characterized in that described inorganic additive is 5 weight %～15 weight %.
6. desalting agent according to claim 1, the content that it is characterized in that described solvent are 25 weight %～45 weight %.
7. according to claim 1 or 3 described desalting agents, it is characterized in that described asphaltene dispersants is Sodium dodecylbenzene sulfonate or nonyl phenol polyimide resin.
8. according to claim 1 or 4 described desalting agents, it is characterized in that described tensio-active agent be in bromohexadecane yl pyridines, the chloro-hexadecane yl pyridines any one.
9. according to claim 1 or 6 described desalting agents, it is characterized in that described solvent is ethanol and water mixture, ethanol is 1: 0.5～2 with the quality ratio.
10. the preparation method of the described desalting agent of claim 1 is characterized in that:
(1) preparation of polyethylene polyamine polyoxyethylene polyoxypropylene ether:
A certain amount of polyethylene polyamine and catalyzer are joined in the autoclave, logical nitrogen protection, under 100～160 ℃ of temperature, slowly be pressed into a certain amount of propylene oxide with nitrogen, need logical water quench in the reaction process, react and slowly be pressed into a certain amount of oxyethane with nitrogen after 2～5 hours, 120～200 ℃ of reactions 2～5 hours, slowly be pressed into a certain amount of propylene oxide with nitrogen at last, 100～160 ℃ of reactions 2～5 hours, promptly obtain polyethylene polyamine polyoxyethylene polyoxypropylene ether after the cooling;
(2) preparation of crude oil desalting agent:
Polyethylene polyamine polyoxyethylene polyoxypropylene ether, asphaltene dispersants, tensio-active agent and the solvent of step (1) preparation are joined in the reactor 40～80 ℃ of stirrings 20～60 minutes, add inorganic additive then and stirred 20～60 minutes, be crude oil desalting agent of the present invention after mixing;
Described polyethylene polyamine be in diethylenetriamine, triethylene tetramine or the tetraethylene pentamine any one;
Described catalyzer is the oxide compound of the oxide compound of alkali or oxyhydroxide, alkaline-earth metal or oxyhydroxide, BF
3And AlCl
3In any one;
Described polyethylene polyamine: oxyethane: the propylene oxide ratio is 1: 20～500: 20～500, and described ratio is a weight ratio;
Described catalyst consumption is 0.1～2% of a raw material gross weight.
11. preparation method according to claim 10 is characterized in that: described catalyzer is sodium hydroxide or potassium hydroxide.
12. preparation method according to claim 10 is characterized in that: described polyethylene polyamine: oxyethane: the ratio of propylene oxide is 1: 40～200: 40～200, and described ratio is a weight ratio.
13. according to claim 10 or 11 described preparation methods, it is characterized in that: described catalyst consumption is 0.2～1.5% of a raw material gross weight.
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