CN1982414A - Method for decreasing petroleum acid value - Google Patents
Method for decreasing petroleum acid value Download PDFInfo
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- CN1982414A CN1982414A CN 200510134488 CN200510134488A CN1982414A CN 1982414 A CN1982414 A CN 1982414A CN 200510134488 CN200510134488 CN 200510134488 CN 200510134488 A CN200510134488 A CN 200510134488A CN 1982414 A CN1982414 A CN 1982414A
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Abstract
A method for decreasing petroleum acid value is carried out by heating acid-containing petroleum between 405-500degree for 5 seconds <1min, and contacting reactant with acid remover to obtain the de-pickled petroleum. It can supplement thermal cracking reaction with esterification also it's efficient, simple and has shorter thermal treatment time.
Description
Technical field
The invention relates to a kind of method of depickling, especially about a kind of method that reduces acid value of petroleum.
Background technology
Acidic substance in the oil are based on naphthenic acid, also comprise some other organic acid.In the petrolize process, naphthenic acid can directly react with iron, causes boiler tube, interchanger and other refining equipment to corrode; Naphthenic acid can also react with the protective membrane FeS of oil equipment, makes hardware expose new surface, is subjected to new corrosion, is especially surpassing under 200 ℃ the hot environment, and naphthenic acid sharply increases the corrodibility of hardware.If can not in refining process, remove the acidic substance in the oil, will influence end product quality, cause equipment failure, problem such as environmental pollution.Studies show that when the acid number in the oil surpassed 1 milligram of KOH/ gram, the acid corrosion meeting was very serious; Will cause remarkable corrosion to production and refining equipment when acid number reaches 0.5 milligram of KOH/ gram in the crude oil; And have only when acid number restrains less than 0.3 milligram of KOH/, just can not cause tangible equipment corrosion problem.Because the corrodibility of acid-containing raw oil, the refinery is unwilling to process the crude oil of acid number greater than 1 milligram of KOH/ gram usually.So the acid number in the crude oil can have influence on the price of crude oil, acid number is high more, and the price of crude oil is low more.Along with the supply of acid-containing raw oil is more and more, therefore the etching problem that how to solve acid in the oil also just more and more comes into one's own.
The method that removes the oil middle acid substance at present mainly contains the method for hydrogenation, alkali lye or the washing of amine alcoholic solution, solvent extraction, fractionation by adsorption.Hydrogenation method is removed organic acid by hydrogen in the presence of catalyzer, and removal effect is best, but the facility investment expense is higher, and hydrogen gas consumption is bigger.Alkali wash need consume a large amount of sodium hydroxide, the sodium sulfate serious environment pollution that separating naphthenic acid produced, and the naphthenic soap that remains in the oil product can reduce oil property.Amine alcohol method acid removal rate is higher, but solvent recuperation energy consumption height, the colourity of depickling oil is subjected to certain influence.The highest 99.9% the naphthenic acid that removes of solvent extraction process, but the Separation and Recovery of various components needs complex apparatus and higher energy consumption in the solvent.Adsorption method of separation only is applied to the laboratory at present, and there are many defectives in industrialization, need set up the huge process system of absorption, desorption, desorbing agent regeneration and solvent recuperation, and is difficult to avoid sorbent material to enter to cause ash content to increase in the oil product.For this reason, need to continue the method for a kind of simple, reduction acid value for crude oil that process cost is lower of research.
US 5891325 has introduced a kind of method of the crude oil behind the flash-evaporation dehydration being carried out multistage hot depickling processing, this method comprises the high-temperature temperature that heating crude oil is decomposed to the part organic acid that is enough to make in the crude oil, simultaneously in reaction process with the inert gas purge system, contain the easy volatile organic acid of hydrocarbon fraction and be difficult for the volatile hydrocarbon cut with acquisition, easy volatile is partly used in oxide compound, oxyhydroxide, carbonate of calcium, magnesium etc. and organic acid, then be difficult for volatile fraction and mix the crude oil that obtains after the depickling.
CN 1212373C discloses a kind of method that reduces acid value of petroleum, this method is hot depickling method, comprise that will contain sour oil is heated to 280-520 ℃, the sour oil that contains that will heat then enters in the adiabatic reactor, under 280-520 ℃, normal pressure to 5.0 MPa condition, stopped 1-300 minute, preferably under 430-500 ℃, 0.2-1.0 MPa condition, stopped 10-120 minute, naphthenic acid generation thermo-cracking is transformed, inject quenching oil at reactor outlet then, oil temperature after the reduction thermal treatment, at last the oil behind the chilling is entered separation column, with the H of carboxylic acid cracking generation
2O, CO
2, CO and partial cracking petroleum gas removes, and obtains the oil after the depickling.Though adopt this method can remove most petroleum acid,, under the used condition of this method, side reactions such as serious cracking, polymerization can take place, cracking produces a large amount of H
2O, CO
2, the CO micro-molecular gas, polymerization then produces the bigger product of a large amount of molecular weight, as coke, makes oil property take place significantly to change, crude yield is very low.
US 5948238 has proposed a kind ofly to reduce the method for acid value of petroleum by esterification, and it is that room temperature to 450 ℃, metal carboxylate are catalyzer, C that this method is included in temperature of reaction
2-C
6Monohydroxy-alcohol or dibasic alcohol be that de-acidying agent, molar ratio of alcohol to acid are to carry out esterification deacidification under the condition of 0.5-20.
CN 1456638A discloses a kind of method that reduces crude oil and distillate acid number, this method is the esterification deacidification method, comprise stock oil and alcohols or alcamines de-acidying agent generation esterification under temperature is 90-500 ℃, reaction separated unreacted de-acidying agent by settlement separate or evaporation, distillatory method then for 1-600 minute with stock oil.
The main drawback of esterification process is that the consumption of alcohol is bigger, long reaction time, and the volume of esterifier is big, and investment is many, can increase more cost to some high-acid crude oils, and acid removal rate is high more, and the ratio of required alcohol is big more, and cost is also just high more.
Summary of the invention
The objective of the invention is can influence oil properties or the higher shortcoming of cost for the method that overcomes prior art reduction acid value of petroleum, and providing a kind of does not influence oil properties and the method for the reduction acid value of petroleum that cost is low, efficient is high, easy to implement.
The inventor is by discovering, be lower than under 400 ℃ the condition, the naphthenic acid acid removal rate is lower, need the very long reaction times, and temperature is when being higher than 400 ℃, even crude oil stopped 1 minute under this temperature, also have serious cracking, polyreaction generation, produce more micro-molecular gas and coke.And adopt the depickling of pure esterification method, when even the add-on of alcohol is 10 weight % of former weight of oil, the acid number that also can only only be the second line of distillation distillate of 3.9 milligrams of KOH/ grams with initial acid value content is reduced to 0.4 milligram of KOH/ gram, acid removal rate only reaches 89.74%, and the acid number of the product after the depickling still is higher than 0.3 milligram of KOH/ gram of safe bottom line that hardware requires acid number.And if hot depickling and esterification deacidification are combined, on the one hand the condition by reducing hot depickling, sacrifice the part acid removal rate of hot depickling, to prevent side reactions such as oil generation cracking and polymerization, thereby reduce influence to oil property, utilize the waste heat of hot depickling on the other hand, carry out esterification by adding a spot of alcohols, remove hot depickling and do not remove clean acid number.Can avoid both deficiencies like this, promptly under than short residence time(SRT) or relatively low temperature, carry out hot depickling, both can reach good deacidification effect, cracking can not take place again, utilize the waste heat of hot depickling to carry out esterification simultaneously, reduce the dosage of esterification deacidification agent on the one hand, avoid repeating to heat the power loss that causes on the other hand, and comprehensive acid removal rate substantially exceed the acid removal rate that these two kinds of methods are used separately, and comprehensive benefit is higher than sum of the two also up to more than 99%.
The invention provides a kind of method that reduces acid value of petroleum, this method comprises and heats 5 seconds to less than 1 minute between 405-500 ℃ with containing sour oil, then gained reaction product and de-acidying agent is carried out contact reacts, obtains the depickling oil.
Method provided by the invention organically combines hot depickling and esterification deacidification method, the problem that the oil property of having avoided crude oil at high temperature to cause because of overstand on the one hand changes, avoided the mass consumption of de-acidying agent on the other hand again, thereby reduced production cost, saved a large amount of Separation and Recovery steps.Specifically, method provided by the invention has following advantage:
(1) less to oil properties influence: with esterification supplemental heat cracking depickling, can the shortening heat treatment time, significantly reduce or avoid influence oil properties;
(2) the de-acidying agent consumption is less: because esterification is carried out after the thermo-cracking depickling, required de-acidying agent is wanted much less than omnidistance esterification deacidification, and the de-acidying agent that only need contain the 0.01-2 weight % of sour oil weight makes acid removal rate up to more than 99%;
(3) deacidification efficiency height: because esterification is carried out, can make the abundant esterification of uncracked acidic substance under comparatively high temps, make acid removal rate up to more than 99%;
(4) technology is simple, easy to implement: whole process only needs to increase hot deacidifying device before advancing separation column and the esterification device gets final product, and needn't significantly adjust original device.
Description of drawings
Fig. 1 is the process flow sheet of reduction acid value of petroleum method provided by the invention.
Specific implementation method
The method of reduction acid value of petroleum provided by the invention comprises and heats 5 seconds to less than 1 minute between 405-500 ℃ with containing sour oil, then gained reaction product and de-acidying agent is carried out contact reacts, obtains the depickling oil.
Among the present invention, described mainly is that acid and pure esterification take place with contact reacts de-acidying agent, and therefore there is no particular limitation to described catalytic temperature, and the temperature of conventional esterification gets final product.But one skilled in the art will appreciate that temperature of reaction is favourable to esterification, temperature of reaction is high more, helps the carrying out of esterification more.But the too high meeting of temperature of reaction causes cracking, polymerization and other side reaction of oil, and therefore according to method provided by the invention, described and catalytic temperature de-acidying agent is preferably 200-400 ℃, more preferably 200-350 ℃.
Owing to be not higher than 400 ℃ with the catalytic temperature of de-acidying agent, under this temperature, have only a spot of oil generation cracking, polyreaction, therefore the described catalytic time decides on the progress of esterification.Because esterification is reversible reaction, when the reaction beginning, when especially reaction raw materials was excessive greatly, reaction was carried out towards the esterification deacidification direction; After reaction proceeded to a certain degree, when especially the concentration of reaction raw materials was less than the concentration of esterification products, reaction was carried out towards the direction that contrary direction promptly generates carboxylic acid, and this is very unfavorable to depickling.Therefore, after reaction proceeds to a certain degree, prolong the reaction times depickling be there is no benefit, thereby the present invention is 1-300 minute with catalytic time of de-acidying agent preferably more preferably 30-100 minute.
There is no particular restriction to the pressure of reaction system in the present invention, is generally reaction system self vapour pressure under this temperature, also can additionally pressurize or reduce pressure.Be preferably the vapour pressure of reaction system self.Under temperature of the present invention and other condition, the pressure of described reaction system can be normal pressure to 5 MPa.
Because the present invention earlier carries out hot depickling reaction to containing sour oil between 405-500 ℃, therefore the amount of described de-acidying agent can reduce greatly, the purpose that production cost reduces greatly when realizing abundant depickling.Among the present invention, the add-on of described de-acidying agent is not less than the 0.01 weight % that contains sour oil total amount can realize that acid removal rate reaches more than 95%, the add-on of preferred de-acidying agent is the 0.01-2 weight % that contains sour oil total amount, and more preferably 0.05 weight % is extremely less than 0.3 weight %.
Described de-acidying agent can be various can with the reaction of acids impurity in the oil and reaction product can be removed from oil effectively or the material that equipment and oil do not had a negative impact, can be organism, also can be inorganics.For example, described de-acidying agent can be in organic alcohols, the alcamine compound one or more.Because the ammonium salt that alcamine compound and naphthenic acid reaction generate can have a negative impact to following process, therefore de-acidying agent of the present invention is not for containing amino alcohols.Described organic alcohols can be selected from C
1-C
10In monobasic alkyl alcohol or the polynary alkyl alcohol one or more are as in methyl alcohol, ethanol, propyl alcohol, butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, ethylene glycol, propylene glycol, butyleneglycol, Diethylene Glycol, triethylene glycol, glycerol, the tetramethylolmethane one or more.Because lower boiling alcohol volatilizees, reduces reaction effect easily, so one or more in the higher ethylene glycol of preferred use boiling point, Diethylene Glycol, the tetramethylolmethane in the specific embodiment of the invention.
Among the present invention, it is described that to contain sour oil can be crude oil or various petroleum fractions, wherein crude oil can be one or more in crude oil behind the various desalting and dewaterings or the topped crude that removes moisture and part lighter hydrocarbons by flash distillation, and petroleum fractions comprises one or more in gasoline, diesel oil, kerosene, wax oil, long residuum, the vacuum residuum.Be preferably the crude oil behind the desalting and dewatering.
Of the present inventionly contain the heating of sour oil between 405-500 ℃ and can in preheater, carry out, also can in adiabatic reactor, carry out.Lack very much (less than 1 minute) heat-up time between 405-500 ℃ owing to contain sour oil among the present invention, so preferably directly in preheater, carry out in the specific embodiment of the invention.Reduce requirement thus to equipment.
Describedly contain sour oil and heat 5 seconds to less than 1 minute mainly being to carry out thermo-cracking and change in order to contain organic acid in the sour oil between 405-500 ℃, therefore, the present invention is called hot depickling reaction with the reaction under this temperature.Described hot depickling reaction can remove the organic acid that contains 50-80 weight % in the sour oil on the one hand, on the other hand in this time range, have only side reactions such as the oil generation cracking of minute quantity and polymerization, and when temperature surpasses 1 minute greater than 500 ℃ or time, have bulk petroleum generation cracking, polymerization, form micro-molecular gas and/or the bigger product of molecular weight, so more preferably 405-450 ℃ of the temperature of hot depickling reaction described in the present invention, the reaction times is 10-50 second more preferably.
Because the temperature of reaction of preferred described esterification deacidification reaction is a little less than the temperature of hot depickling reaction, therefore, method provided by the invention comprises also that preferably the product with hot depickling reaction carries out the refrigerative step.Described cooling can realize in various manners, for side reactions such as the cracking after the hot depickling of effective inhibition, polymerizations, the present invention preferably adopts the mode that feeds quenching oil to realize, the add-on of quenching oil is so that the oil temperature after the hot depickling is reduced to 200-400 ℃ is as the criterion.Described quenching oil can be that temperature is lower than 120 ℃ diesel oil, in the long residuum one or more.
Under the preferable case, method provided by the present invention also comprises the step of the depickling oil after the depickling being carried out separation and purification.Fractionated method is preferably adopted in described separation and purification.Fractionation mainly is to remove the H that produces in the depickling reaction of reducing phlegm and internal heat
2O, CO
2, CO, product and de-acidying agent that molecular weight is bigger.Described fractionated concrete operations have been conventionally known to one of skill in the art, do not repeat them here.
Particularly, the method for reduction acid value of petroleum of the present invention can realize by technical process shown in Figure 1.As shown in Figure 1, containing sour oil enters the preheater 2 405-500 ℃ of heating 5 seconds to less than 1 minute from pipeline 1, carry out hot depickling reaction, send into de-acidying agent after then the hot depickling reaction product of gained being cooled to 200-400 ℃ by quenching oil in pipeline 3 and carry out esterification deacidification reaction in the esterifier 4, the esterification deacidification product that obtains enters from pipeline 5 and carries out fractionation the separation column 6, removes the H that the carboxylic acid cracking produces
2O, CO
2, CO, product and de-acidying agent that molecular weight is bigger, obtain the depickling petroleum products.
The yield of employing micro-molecular gas and coke is weighed the change degree of oil property among the present invention, and the yield of micro-molecular gas yield and coke is high more, and the degree that oil property changes is high more, and vice versa.The concrete measuring method of the yield of micro-molecular gas and coke has been those skilled in the art, does not repeat them here.
The following examples will the present invention is further illustrated.
Embodiment 1
Present embodiment is used to illustrate the method for reduction acid value of petroleum provided by the invention.
As shown in Figure 1, be that the desalted and dewatered crude oil of 18.21 milligrams of KOH/ gram enters from pipeline 1 and is preheating to 440 ℃ the preheater 2 and carries out hot depickling reaction with acid number, the time of hot depickling reaction was 30 seconds, the hot depickling reaction product that obtains is cooled to 250 ℃ by carrying out heat exchange with 50 ℃ diesel oil in pipeline 3, send into together with the tetramethylolmethane of the glycerol of relative desalted and dewatered crude oil weight 0.5 weight % and 0.8 weight % then and carry out the esterification deacidification reaction in the esterifier 4, the time of reaction is 200 minutes, the esterification deacidification product that obtains enters from pipeline 5 and carries out fractionation the separation column 6, and obtaining acid number content is the depickling crude oil products of 0.18 milligram of KOH/ gram, micro-molecular gas and coke.The acid removal rate of whole process flow is 99.01%, the yield of micro-molecular gas and coke is 20%.
Embodiment 2
Present embodiment is used to illustrate the method for reduction acid value of petroleum provided by the invention.
As shown in Figure 1, be that the desalted and dewatered crude oil of 10.36 milligrams of KOH/ gram enters from pipeline 1 and is preheating to 420 ℃ the preheater 2 and carries out hot depickling reaction with acid number, the time of hot depickling reaction was 50 seconds, the hot depickling reaction product that obtains is cooled to 300 ℃ by carrying out heat exchange with 30 ℃ diesel oil in pipeline 3, send into together with the Diethylene Glycol of relative desalted and dewatered crude oil weight 0.5 weight % then and carry out the esterification deacidification reaction in the esterifier 4, the time of reaction is 30 minutes, the esterification deacidification product that obtains enters from pipeline 5 and carries out fractionation the separation column 6, and obtaining acid number content is the depickling crude oil products of 0.08 milligram of KOH/ gram, micro-molecular gas and coke.The acid removal rate of whole process flow is 99.23%, the yield of micro-molecular gas and coke is 10%.
Embodiment 3
Present embodiment is used to illustrate the method for reduction acid value of petroleum provided by the invention.
As shown in Figure 1, be that the desalted and dewatered crude oil of 13.10 milligrams of KOH/ gram enters from pipeline 1 and is preheating to 405 ℃ the preheater 2 and carries out hot depickling reaction with acid number, the time of hot depickling reaction was 50 seconds, the hot depickling reaction product that obtains is cooled to 200 ℃ by carrying out heat exchange with 30 ℃ long residuum in pipeline 3, send into together with the triethylene glycol of relative desalted and dewatered crude oil weight 1.0 weight % then and carry out the esterification deacidification reaction in the esterifier 4, the time of reaction is 280 minutes, the esterification deacidification product that obtains enters from pipeline 5 and carries out fractionation the separation column 6, and obtaining acid number content is the depickling crude oil products of 0.02 milligram of KOH/ gram, micro-molecular gas and coke.The acid removal rate of whole process flow is 99.87%, the yield of micro-molecular gas and coke is 15%.
Embodiment 4
Present embodiment is used to illustrate the method for reduction acid value of petroleum provided by the invention.
Be that the desalted and dewatered crude oil of 10.36 milligrams of KOH/ gram enters from pipeline 1 and is preheated to 480 ℃ the preheater 2 and carries out hot depickling reaction with acid number, the time of hot depickling reaction was 15 seconds, the hot depickling reaction product that obtains is cooled to 350 ℃ by carrying out heat exchange with 30 ℃ long residuum in pipeline 3, send into together with the tetramethylolmethane of relative desalted and dewatered crude oil weight 0.8 weight % then and carry out the esterification deacidification reaction in the esterifier 4, the time of reaction is 50 minutes, the esterification deacidification product that obtains enters from pipeline 5 and carries out fractionation the separation column 6, and obtaining acid number content is the depickling crude oil products of 0.05 milligram of KOH/ gram, micro-molecular gas and coke.The acid removal rate of whole process flow is 99.52%, the yield of micro-molecular gas and coke is 18%.
Comparative Examples 1
This Comparative Examples is used for illustrating that prior art reduces the method for acid value of petroleum.
Adopt the method described in the CN 121373C, will the acid number identical be that the crude oil of the desalting and dewatering of 10.36 milligrams of KOH/ grams is heated to 480 ℃ and carries out hot depickling reaction in thermal reactor with embodiment 4, the time of hot depickling reaction is 10 minutes, and obtaining acid number content after the fractionation is depickling crude oil products, micro-molecular gas and the coke of 0.02 milligram of KOH/ gram.The acid removal rate of whole process flow is 99.80%, the yield of micro-molecular gas and coke is 60%.
Claims (8)
1, a kind of method that reduces acid value of petroleum, this method comprise and heat 5 seconds to less than 1 minute between 405-500 ℃ with containing sour oil, then gained reaction product and de-acidying agent are carried out contact reacts, obtain the depickling oil.
2, method according to claim 1, wherein, it is 200-400 ℃ that described and de-acidying agent carries out catalytic temperature, the time is 1-300 minute.
3, method according to claim 2, wherein, it is 200-350 ℃ that described and de-acidying agent carries out catalytic temperature, the time is 30-100 minute.
4, method according to claim 1, wherein, the add-on of described de-acidying agent is the 0.01-2 weight % that contains sour oil add-on.
5, method according to claim 1, wherein, described de-acidying agent is C
1-C
10Organic alcohol.
6, method according to claim 5, wherein, described organic alcohol is selected from one or more in ethylene glycol, Diethylene Glycol, triethylene glycol, propylene glycol, butyleneglycol, glycerol, the tetramethylolmethane.
7, method according to claim 1, wherein, this method comprises that also the depickling oil that will obtain carries out the step that fractionation purifies.
8, step according to claim 1, wherein, the described crude oil that contains sour oil for the process desalting and dewatering.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368107B (en) * | 2007-08-15 | 2012-05-30 | 中国石油化工股份有限公司 | Method for removing petroleum acid from hydrocarbon oil |
| CN101368108B (en) * | 2007-08-15 | 2012-11-14 | 中国石油化工股份有限公司 | Utilization method of crude glycerine |
| CN104122321A (en) * | 2013-04-28 | 2014-10-29 | 威尔资源有限公司 | Method for measuring acid compounds in petroleum |
| CN104806222A (en) * | 2015-05-13 | 2015-07-29 | 赵松柏 | Treatment process of acid-containing crude oil after acidification of oil well |
-
2005
- 2005-12-15 CN CNB2005101344888A patent/CN100523136C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368107B (en) * | 2007-08-15 | 2012-05-30 | 中国石油化工股份有限公司 | Method for removing petroleum acid from hydrocarbon oil |
| CN101368108B (en) * | 2007-08-15 | 2012-11-14 | 中国石油化工股份有限公司 | Utilization method of crude glycerine |
| CN104122321A (en) * | 2013-04-28 | 2014-10-29 | 威尔资源有限公司 | Method for measuring acid compounds in petroleum |
| CN104806222A (en) * | 2015-05-13 | 2015-07-29 | 赵松柏 | Treatment process of acid-containing crude oil after acidification of oil well |
| CN104806222B (en) * | 2015-05-13 | 2017-05-31 | 唐山市曹妃甸区浦圣石油技术服务有限公司 | The handling process of acid-containing raw oil after oil well acidation |
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| CN100523136C (en) | 2009-08-05 |
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