CN1063741C - Method for recovery of petroleum acids from mixed extract of isopropyl alcohol-ammonia water - Google Patents
Method for recovery of petroleum acids from mixed extract of isopropyl alcohol-ammonia water Download PDFInfo
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- CN1063741C CN1063741C CN95108252A CN95108252A CN1063741C CN 1063741 C CN1063741 C CN 1063741C CN 95108252 A CN95108252 A CN 95108252A CN 95108252 A CN95108252 A CN 95108252A CN 1063741 C CN1063741 C CN 1063741C
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- petroleum acid
- water
- flocculation agent
- petroleum
- acid
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Abstract
The present invention relates to a method of recovering petroleum acid. The petroleum acid in petroleum distillates can be extracted by composite ammonia water-isopropyl alcohol solvent. When the petroleum acid and the solvent in the waste composite solvent are recovered through distillation, a flocculating agent with the weight of 0.3 to 1.0% is added to solve the problem of emulsification in the process of the distillation, and the yield and the quality of the petroleum acid are improved.
Description
The invention relates to the recovery method of petroleum acid, particularly about from Virahol-ammoniacal liquor mixing extract, reclaiming the method for petroleum acid.International Patent classificating number is B01J19/02.
As everyone knows, in order to obtain to satisfy the distillate that product performance require, must remove the petroleum acid that contains in the sour petroleum fractions.The double solvents that available ammoniacal liquor and low mass molecule alcohol class form removes petroleum acid in the petroleum fractions by chemical reaction and extracting.Compare with the aqueous sodium hydroxide solution acid stripping method, the advantage of the double solvents acid stripping method that ammoniacal liquor and low mass molecule alcohol class form is that solvent is renewable, recycling, and no spent acid, alkaline residue produce, simultaneously the fine chemical material petroleum acid of recyclable preciousness.As U.S. Pat 4634519, invented with methyl alcohol-ammoniacal liquor double solvents and removed the 180-600 ℃ of petroleum acid in the distillate, direct heating gives up double solvents (being extract) with regard to recyclable solvent and petroleum acid but with after Virahol-ammoniacal liquor double solvents depickling, when Virahol in the useless double solvents of heating recovery, ammonia and petroleum acid, liquidus temperature rises to more than 86 ℃, the liquid phase of otherwise transparent becomes white emulsion, the petroleum acid yield is less than 50% (weight) as a result, and this is that the petroleum acid ammonium salt decomposes due to the back petroleum acid emulsification that produces.
The purpose of this invention is to provide a kind of method that reclaims petroleum acid from Virahol-ammoniacal liquor mixing extract, this is the method for a kind of simple and easy to do, cost-effective solution liquid phase emulsification problem when reclaiming petroleum acid, has improved the yield and the quality of petroleum acid simultaneously.
The object of the present invention is achieved like this, and a certain amount of flocculation agent is joined in useless Virahol-ammoniacal liquor double solvents, adds thermal distillation, the solvent that condensation steams is heated to certain temperature and is incubated for some time, stops heating, separate petroleum acid and water, reclaim petroleum acid.The water and the recovered solvent that contain flocculation agent are made into double solvents again, when reclaiming solvent and petroleum acid after the depickling, do not need to add flocculation agent again.
The mode of separating petroleum acid and water can adopt natural sedimentation.The mixture that is about to boil off the remaining oil sour water behind the solvent leaves standstill in separating funnel or other separator, utilizes the density difference of petroleum acid and water and immiscible character thereof, natural subsidence layering, separately petroleum acid and water.
The mode of separating petroleum acid and water can adopt a kind of extraction of benzene,toluene,xylene, 60～90 ℃ of sherwood oils, 90～180 ℃ of liquid hydrocarbons to reclaim petroleum acid.Be about to boil off the mixture of remaining petroleum acid and water behind the solvent, in the impouring separatory funnel, add a certain amount of above-mentioned solvent, fully vibration, petroleum acid is dissolved in solvent, settlement separate back is divided and is anhydrated, the solvent phase heating boils off solvent, petroleum acid.
In the method for the present invention, flocculation agent is one or more the arbitrary proportion mixture in sodium-chlor, ammonium chloride, Repone K, sodium sulfate, ammonium sulfate, vitriolate of tartar, SODIUMNITRATE, ammonium nitrate, the saltpetre, is best with the ammonium salt.The weight ratio of flocculation agent and useless double solvents is 0.2-1.0% (weight), and the best is 0.5-0.7% (weight).Said useless double solvents is the mixture of Virahol-ammoniacal liquor double solvents and petroleum acid.
In the method for the present invention, heating can be coal, electric furnace, steam or other type of heating, but all distillment finally should be heated to 90-100 ℃, and is incubated 1-7 minute, and optimum temps is 95-100 ℃, best soaking time 3-5 minute.
In the method for the present invention, the temperature of separating petroleum acid and water is 20-80 ℃, and the best is 50-70 ℃, separates petroleum acid and water and can adopt the natural subsidence partition method, also can adopt benzene,toluene,xylene, 60-90 ℃ sherwood oil, petroleum acid is reclaimed in a kind of extraction in 90-180 ℃ of liquid hydrocarbon.
Method of the present invention is applicable to the recovery of the petroleum acid that removes from 180-500 ℃ of distillate.
More particularly, a kind of method that from ammoniacal liquor-Virahol mixing extract, reclaims petroleum acid, it is characterized in that: when solvent in distillation recovery extract and petroleum acid, the flocculation agent that in extract, adds 0.3～1.0% (weight), be heated to 90～100 ℃ and be incubated 1～7 minute, separate petroleum acid and water when being cooled to 20～80 ℃, reclaim petroleum acid, the water that contains flocculation agent and cooling recovered solvent be mixed into again bonding solvent, when reclaiming petroleum acid again after its depickling, do not need to add again flocculation agent.
Flocculation agent be in sodium-chlor, ammonium chloride, Repone K, sodium sulfate, ammonium sulfate, vitriolate of tartar, SODIUMNITRATE, ammonium nitrate, the saltpetre one or both with the arbitrary proportion mixture, the add-on of flocculation agent is 0.5～0.7% (weight).Flocculation agent is best with the ammonium salt
Said heating can be coal, electric furnace, steam or alternate manner, and temperature of reaction is 95～100 ℃; Soaking time is 3-5 minute.The temperature of separating petroleum acid and water is 50-70 ℃.The mode of separating petroleum acid and water can adopt natural sedimentation, and the mode of separating petroleum acid and water can adopt a kind of extraction in benzene,toluene,xylene, 60～90 ℃ of sherwood oils, 90～180 ℃ of liquid hydrocarbons to reclaim petroleum acid.
Method of the present invention is applicable to the recovery of the petroleum acid that removes from 180～500 ℃ of distillates.
Principal feature of the present invention is: add the flocculation agent of inorganic salts in useless double solvents, solved the emulsification problem of liquid phase in the removal process, the yield of petroleum acid is brought up to more than 90% by 49.2%.Recovered solvent is made into double solvents again with the water that contains flocculation agent, when reclaiming with reheat after its depickling, does not need to add flocculation agent again, also can not produce emulsification.No waste sludge discharge helps environment protection.The present invention is simple and easy to do, and favorable economic benefit and social benefit are arranged.
The following examples are to further specify of the present invention, but not limit the scope of the invention.
Embodiment 1
In being the still kettle of 2 liters, volume adds 1000g and is the useless double solvents that removes petroleum acid 180～355 ℃ the diesel oil distillate from boiling range, and add 5g ammonium sulfate, and heating up with steam heating, vapour phase reclaims solvent through cooling, liquidus temperature finally rises to 100 ℃, and is incubated 3 minutes.It is transparent faint yellow that water is, and the upper strata is floating to have brown oily liquids to be petroleum acid.With liquid phase cools to 60～70 ℃, impouring separating funnel and insulation were left standstill 60 minutes, were divided into two-layerly up and down, and the upper strata is a petroleum acid, and lower floor is a water.Divide sub-cloud water, get the upper strata petroleum acid, be weighed as 24.1g, acid content 85.4% (weight), yield 95.9% (weight).
Embodiment 2
In the there-necked flask that the thermometer volume is 2 liters is housed, add 1000g and from boiling range is 391～495 ℃ reduced pressure distillate, remove the useless double solvents of petroleum acid, add 7g sodium-chlor, use the electric mantle heat temperature raising.Vapour phase reclaims solvent through cooling, and the liquid phase outlet temperature is raised to 98～100 ℃, and is incubated 3 minutes.Water is transparent light yellow, and the upper strata is floating to have brownish black oily matter to be petroleum acid.With liquid phase cools to 40～50 ℃, and add 60～90 ℃ of sherwood oil 150ml, fully standing demix in the impouring separating funnel behind the shake.Lower aqueous layer in the branch, upper strata solvent phase are steamed in 500ml and are stayed a bottle internal heating to boil off solvent, and residuum is a petroleum acid in the bottle, is weighed as 24.6g, and purity is 87.1% (weight), and yield is 98.2% (weight).
Embodiment 3
Mix with distillation recovered solvent and the water that contains flocculation agent, be mixed with double solvents again.With this double solvents diesel oil is carried out depickling.Get the useless agent 1000g after the depickling, do not add flocculation agent, join matrass internal heating to 98 ℃, and be incubated 5 minutes.Reclaim about the surplus liquid cooling to 40 ℃ behind the solvent and extract petroleum acid with benzene, petroleum acid 24.0g, its purity is 84.9% (weight), yield 95.2% (weight).
Claims (8)
1. method that from ammoniacal liquor-Virahol mixing extract, reclaims petroleum acid, it is characterized in that: when distilling the petroleum acid that reclaims in the extract, the flocculation agent that in extract, adds 0.3-1.0% (weight), be heated to 90-100 ℃ and be incubated 1-7 minute, separate petroleum acid and water when being cooled to 20-80 ℃, reclaim petroleum acid, the water that contains flocculation agent is mixed into double solvents again with the cooling recovered solvent, when reclaiming petroleum acid again after its depickling, do not need to add again flocculation agent.
2. method according to claim 1, it is characterized in that flocculation agent is one or more arbitrary proportion mixtures in sodium-chlor, ammonium chloride, Repone K, sodium sulfate, ammonium sulfate, vitriolate of tartar, ammonium nitrate, the saltpetre, the add-on of flocculation agent is 0.5-0.7% (weight).
3. method according to claim 1 is characterized in that flocculation agent is ammonium chloride or ammonium sulfate or ammonium nitrate.
4. method according to claim 1 is characterized in that said heating can adopt coal, electric furnace, steam to heat, and temperature of reaction is 95-100 ℃; Soaking time is 3-5 minute.
5. method according to claim 1, the temperature that it is characterized in that separating petroleum acid and water is 50-70 ℃.
6. method according to claim 1 is characterized in that the mode of separating petroleum acid and water can adopt natural sedimentation.
7. method according to claim 1, the mode that it is characterized in that separating petroleum acid and water can adopt the sherwood oil of benzene,toluene,xylene, 60-90 ℃, a kind of extraction in the 90-180 ℃ liquid hydrocarbon to reclaim petroleum acid.
8. be applicable to the recovery of the petroleum acid that from 180-500 ℃ of distillate, removes according to the arbitrary method of claim 1-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95108252A CN1063741C (en) | 1995-07-21 | 1995-07-21 | Method for recovery of petroleum acids from mixed extract of isopropyl alcohol-ammonia water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95108252A CN1063741C (en) | 1995-07-21 | 1995-07-21 | Method for recovery of petroleum acids from mixed extract of isopropyl alcohol-ammonia water |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1141281A CN1141281A (en) | 1997-01-29 |
| CN1063741C true CN1063741C (en) | 2001-03-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95108252A Expired - Fee Related CN1063741C (en) | 1995-07-21 | 1995-07-21 | Method for recovery of petroleum acids from mixed extract of isopropyl alcohol-ammonia water |
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| Country | Link |
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| CN (1) | CN1063741C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100506949C (en) * | 2006-04-18 | 2009-07-01 | 中国海洋石油总公司 | Method of eliminating naphthenic acid from crude oil or fraction oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4634519A (en) * | 1985-06-11 | 1987-01-06 | Chevron Research Company | Process for removing naphthenic acids from petroleum distillates |
| CN1049373A (en) * | 1990-09-17 | 1991-02-20 | 中国石油化工总公司 | Phosphoric acid/active carbon catalyst and coincidence process |
| CN1070182A (en) * | 1992-09-25 | 1993-03-24 | 新疆石油管理局重油加工研究所 | A kind of from heavy lubricating-oil distillation the method for separating naphthenic acid |
-
1995
- 1995-07-21 CN CN95108252A patent/CN1063741C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4634519A (en) * | 1985-06-11 | 1987-01-06 | Chevron Research Company | Process for removing naphthenic acids from petroleum distillates |
| CN1049373A (en) * | 1990-09-17 | 1991-02-20 | 中国石油化工总公司 | Phosphoric acid/active carbon catalyst and coincidence process |
| CN1070182A (en) * | 1992-09-25 | 1993-03-24 | 新疆石油管理局重油加工研究所 | A kind of from heavy lubricating-oil distillation the method for separating naphthenic acid |
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| Publication number | Publication date |
|---|---|
| CN1141281A (en) | 1997-01-29 |
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