CN1342630A - Process for preparing high-purity n-pentane - Google Patents
Process for preparing high-purity n-pentane Download PDFInfo
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- CN1342630A CN1342630A CN 00122981 CN00122981A CN1342630A CN 1342630 A CN1342630 A CN 1342630A CN 00122981 CN00122981 CN 00122981 CN 00122981 A CN00122981 A CN 00122981A CN 1342630 A CN1342630 A CN 1342630A
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Abstract
A process for preparing high-purity n-pentane includes double-tower rectification, refining and dewateirng by molecular sieve, and features that more plates per meter for efficient filler in rectifying tower, more layer of tower plates, high rectification effect, high refining effect by removing S. olefin, oxygen and nitrogen contained compounds, arylhydrocarbon and water, low investment, and high output rate.
Description
The present invention relates to the two-tower rectification of petroleum refining process, refining and molecular sieve dehydration United Technologies, especially relate to the method for purification of Skellysolve A.
Introduce UOP dewaxing by molecular sieve technology continuously since China in 1994, Skellysolve A occurs on market as a component of dewaxing by molecular sieve desorbing agent.Up to the present, the Skellysolve A of each factory's use all is an imported product.Learn that from document the Skellysolve A of import all is to adopt rectifying and hydrofining process integration to produce, rectifying and hydrofining process integration, investment is big, the production cost height, the operational condition harshness is limited by scale and benefit, does not meet China's national situation.Distillation technology research and industrialization that Skellysolve A is purified had introduction on the document at home, as 87 pages of 68 pages of 35 pages of 1993 " chemistry world " the 1st phases, the 1st phase of nineteen ninety " refining of petroleum " and " catalytic reforming communication " the 4th phases in 1999.In April, 1987 Qilu Petrochemical company triumph refinery is a raw material with the triumph tops of reforming, and adopts two rectifying tower, produces Skellysolve A purity greater than 40% pentane oil; In April, 1999, Dalian Petrochemical Industry Company was a raw material with reformation pentane oil and tops, adopted 75 float valve 48519mm towers, told the pentane oil of iso-pentane purity 18～20%.Because the filler plate number of rectifying tower is low, the column plate number of plies is few, above-mentioned two kinds of rectifying separation precision are not enough.Skellysolve A removal of impurity process is the continuous treating process of a series of unit operations, existing document is not seen and is addressed, but close technology has a lot of reports, as " chemical industry progress " the 3rd phase 11 pages, 2000 2000 " modern chemical industry " the 3rd phase 14 pages of US5396020, UOP.The method of impurity such as the desulfurization of gasoline fraction oil, nitrogen, oxygen compound, alkene and aromatic hydrocarbons: chemistry, physics and the chemicophysical refining means of adopting are arranged, by fractionated system is light hydrocarbon mixture, the purified degree of depth is not enough, can not make the Skellysolve A foreign matter content reach the imported product standard.
The purpose of this invention is to provide a kind of simple and easy rectifying, the refining and dewatering process inequality with rectifying-hydrofining process integration.
The inventive method adopts high efficiency packing to carry out two-tower rectification, adopts washing, extraction and absorption to unite refining means then and deviates from impurity in the Skellysolve A, and molecular sieve dehydration is produced qualified product.The present invention is a raw material with reformation tops, pentane oil, carbon five lighter hydrocarbons or oil field lightweight oil, is made up of two-tower rectification, refining and dehydration.Every meter plate number of rectifying tower employing of two-tower rectification process is 15～20 high efficiency packing filling, and the column plate number of plies of each rectifying tower is 120-180.Treating process is made up of 3 processes of following out-of-order restriction: 1. alkaline aqueous solution and Skellysolve A volume ratio slightly are 0.2～2 respectively by the pump input mixer, and alkaline aqueous solution is sodium hydroxide (NaOH) and methyl alcohol (CH
3OH) mixed solution, concentration are 60～80%, wherein NaOH5～14%, CH
3OH75～46%.Then mixed solution is entered settlement separate jar, 10～30 ℃ of temperature, pressure 0.2～0.5MPa, duration of contact 2～8min, Skellysolve A is drawn from separating tank top; 2. thick Skellysolve A mixes with dilute sulphuric acid, and dilute sulphuric acid is 0.5～4 with thick Skellysolve A ratio, the concentration 3～10% of dilute sulphuric acid, mixed solution enters settlement separate jar, 10～30 ℃ of temperature, pressure 0.2～0.5MPa, mixing duration of contact is 2～8min, and thick Skellysolve A is drawn from separating tank top; The volume ratio of 3. taking off aromatic solvent and thick Skellysolve A is 0.5～5, by after being pumped into mixing tank mixing contact, enters settlement separator and separates respectively, and extraction temperature is 50～150 ℃, and extracting pressure is 0.5～1MPa, and slightly Skellysolve A flows out from the tank top.
Because the plate number of every meter of the filler of the rectifying tower of two-tower rectification is many among the present invention, the number of plies of rectifying tower column plate is many, and rectification effect is good, treating process adopts desulfurization, deolefination, contains oxygen, nitrogen compound, takes off aromatic hydrocarbons process integration and dewatering process, refining effect is good, separablely goes out highly purified Skellysolve A.The inventive method less investment, equipment is simple, produces flexibly, and simple to operate, yield is higher.
Below in conjunction with embodiment the inventive method is further described.
Embodiment 1.
Concrete technology comprises among the present invention:
1. two-tower rectification adopts the regular shape filler of metal corrugated plate packed rectification tower, and every meter plate number is 15, the packing tower column plate number of plies is 120.By feedstock pump the reformation tops is sent in interchanger and heater heats to the 100～200 ℃ scope from the head tank extraction, entered rectifying tower, tower top temperature 50-90 ℃, cat head volatilizes＜nC
5 0The promptly light component of light constituent than Skellysolve A, reflux through condensation, cooling and compression rear section, part enters oil tank, oil is extracted out through oil pump at the bottom of the tower, sends into well heater, is heated in 100～200 ℃ of scopes, enter another rectifying tower, tower top temperature 50-90 ℃, cat head steams thick Skellysolve A, purity 〉=95%, reflux through condensation, cooling rear section, reflux ratio is that 4 parts enter oil tank, and oil is extracted out by pump at the bottom of the tower, through with raw material heat exchange and condensation, the laggard oil tank of cooling.
2. refining, 1. desulfurization, certain proportion NaOH-CH
3The aqueous solution of OH and thick Skellysolve A wash extraction respectively by the pump input mixer, and the sulphur compound in the thick Skellysolve A dissolves in the aqueous solution, and mixed solution enters settlement separate jar then.Thick Skellysolve A proportion is little, leads to the thick product after the desulfurization from separating tank top.The alkaline aqueous solution of sulfocompound is sunken to the separating tank bottom than great.Alkaline aqueous solution can be recycled, and regularly changes according to sweetening effectiveness, enters neutralization tank.
In the method for the present invention, the concentration of alkali and methyl alcohol is the key factor that influences desulfurization degree in the alkaline aqueous solution, in thick Skellysolve A oil product kind, temperature, ratio of mixture one regularly, increase the concentration of alkali and methyl alcohol, desulfurization degree increases, but after the concentration of alkali and methyl alcohol was increased to a certain degree, desulfurization degree descended.So in the method for the present invention, the suitable concentration of alkali and methyl alcohol is: NaOH5～14%, CH
3OH75～46%, the total concn of mixed solution are 60～80%.Present embodiment is selected NaOH5% for use, CH
3OH75%, alkaline aqueous solution is 0.2 with thick Skellysolve A volume ratio, 10 ℃ of temperature, duration of contact 2min, pressure 0.2MPa.
2. deolefination, contain oxygen, nitrogen compound, the deolefination in the inventive method, the operational path that contains oxygen, nitrogen compound is identical with sweetening process with equipment, processing condition are different.Cleaning solvent is 3% dilute sulphuric acid, and dilute sulphuric acid is 0.5 with thick Skellysolve A ratio, and mixing duration of contact is 8min, 10～30 ℃ of temperature, pressure 0.2MPa.
3. take off aromatic hydrocarbons, sulfolane solvent and thick Skellysolve A volume ratio are 0.5, by after being pumped into mixing tank mixing contact, advance settlement separator and separate respectively, the thick Skellysolve A that proportion is little flows out from the tank top, cool off laggard oil tank, heavy sulfolane solvent is gone out by the separator underflow, recycles, when the extracting degree of depth is not enough, need propose dense processing, replenish fresh tetramethylene sulfone.
In the inventive method, solvent is the key factor of taking off aromatic hydrocarbons, and the solvent that can deviate from aromatic hydrocarbons has tetramethylene sulfone, dimethyl sulfoxide (DMSO), triethylene glycol ether and diethylene glycol ether.Extraction temperature is 50 ℃, and extracting pressure is 0.2MPa.
3. molecular sieve dehydration purifies.
Skellysolve A after refining is after be pumped into the dehydration tower that the 4A-3A molecular sieve is housed, purifying dehydration, and cat head goes out Skellysolve A.These processing condition: adsorption temp is 10～30 ℃, and adsorptive pressure is 0.3MPa, and the absorption air speed is 2.0m
3H
-1
Embodiment 2.
With the reformation pentane oil is raw material.
The first step: two-tower rectification, adopt the regular shape filler of metal corrugated plate packed rectification tower, every meter plate number is 20, the column plate number of plies of every tower is 180.Its operational condition: 50～90 ℃ of tower top temperatures; Tower top pressure 0.5MPa, reflux ratio 6.Raw material is through heat exchange and be heated to 100～200 ℃, enters rectifying tower, and cat head steams＜nC
5 0Light constituent, after condensation, cooling and compression, partial reflux, part oil-feed jar, oil is extracted out by pump and is sent into heater heats to 100～200 ℃ at the bottom of the tower, advances another tower, and cat head steams 〉=95% (weight) Skellysolve A slightly, after condensation, cooling, partial reflux, part is removed thick Skellysolve A jar.
Second step: basic solution washing, abstraction desulfurization.NaOH-CH
3The aqueous solution of OH and thick Skellysolve A wash extraction respectively by the pump input mixer, and sulfide dissolves in the aqueous solution, mixed solution enters settlement separate jar then, flow out on the little top from jar of thick Skellysolve A proportion after the desulfurization, and corresponding sulphurous water solution is sunken to the separating tank bottom than great.The aqueous solution recycles, and when the sweetening effectiveness difference, enters neutralization tank, handles.Present method operational condition: NaOH 14%, CH
3OH 46%.Alkaline aqueous solution is 2 with thick Skellysolve A volume ratio.Be 2min duration of contact, pressure 0.5MPa, 30 ℃ of temperature.
The 3rd step: carry out acidic aqueous solution washing and reaction, deolefination, contain oxygen, nitrogen compound.Operational path in the inventive method is identical with sweetening process with equipment, and cleaning solvent is 10% dilute sulphuric acid.The operational condition of this process is: dilute sulphuric acid is 4 with thick Skellysolve A volume ratio, and mixing duration of contact is 8min, and temperature is 30 ℃, pressure 0.5MPa.
The 4th step: aromatic hydrocarbons is taken off in the sulfolane solvent extracting.Sulfolane solvent and thick Skellysolve A respectively by be pumped into mixing tank mix contact after, advancing settlement separator separates, the thick Skellysolve A that proportion is little flows out from the tank top, cool off laggard oil tank, heavy sulfolane solvent is gone out by the jar underflow, recycles, when the extracting degree of depth is not enough, need propose dense processing, replenish fresh tetramethylene sulfone.Operational condition: the volume ratio of sulfolane solvent and thick Skellysolve A is 4, and extraction temperature is 150 ℃, and extracting pressure is 0.2MPa.
The 5th step: molecular sieve dehydration.Thick Skellysolve A is after be pumped into the dehydration tower that the 4A-3A molecular sieve is housed, purifying dehydration, and cat head goes out to meet the Skellysolve A of import standard.These processing condition: adsorption temp is 10～30 ℃, adsorptive pressure 0.5MPa, and the absorption air speed is 2.0 cubic metres of (2.0m per hour
3H
-1).
Embodiment 3.
With carbon five lighter hydrocarbons is raw material.
The first step: two-tower rectification, adopt the regular shape filler of metal corrugated plate packed rectification tower, every meter plate number is 18, the stage number of every tower is 150.Its operational condition: 50～90 ℃ of tower top temperatures; Tower top pressure 0.4MPa, reflux ratio 5.Raw material is through heat exchange and be heated to 100～200 ℃, enters rectifying tower, and cat head steams＜nC
5 0Light constituent, after condensation, cooling and compression, partial reflux, part oil-feed jar, oil is extracted out by pump and is sent into heater heats to 100～200 ℃ at the bottom of the tower, advances another tower, and cat head steams 〉=95% (weight) Skellysolve A slightly, after condensation, cooling, partial reflux, part is removed thick Skellysolve A jar.
Second step: basic solution washing, abstraction desulfurization.NaOH-CH
3The aqueous solution of OH and thick Skellysolve A wash extraction respectively by the pump input mixer, and sulfide dissolves in the aqueous solution, mixed solution enters settlement separate jar then, flow out on the little top from jar of thick Skellysolve A proportion after the desulfurization, and corresponding sulphurous water solution is sunken to the separating tank bottom than great.The aqueous solution recycles, and when the sweetening effectiveness difference, enters neutralization tank, handles.Present method operational condition: NaOH 8%, CH
3OH55%.Alkaline aqueous solution with thick Skellysolve A volume ratio is: 0.8.Be 5min duration of contact, pressure 0.4MPa, 20 ℃ of temperature.
The 3rd step: carry out acidic aqueous solution washing and reaction, deolefination, contain oxygen, nitrogen compound.Operational path in the inventive method is identical with sweetening process with equipment, and cleaning solvent is 10% dilute sulphuric acid.The operational condition of this process is: dilute sulphuric acid is 1 with thick Skellysolve A volume ratio, and mixing duration of contact is 6min, and temperature is 20 ℃, pressure 0.3MPa.
The 4th step: aromatic hydrocarbons is taken off in the sulfolane solvent extracting.Sulfolane solvent and thick Skellysolve A respectively by be pumped into mixing tank mix contact after, advancing settlement separator separates, the thick Skellysolve A that proportion is little flows out from the tank top, cool off laggard oil tank, heavy sulfolane solvent is gone out by the jar underflow, recycles, when the extracting degree of depth is not enough, need propose dense processing, replenish fresh tetramethylene sulfone.Operational condition: the volume ratio of sulfolane solvent and thick Skellysolve A is 3, and extraction temperature is 100 ℃, and extracting pressure is 0.5～1MPa.
The 5th step: molecular sieve dehydration.Thick Skellysolve A is after be pumped into the dehydration tower that the 4A-3A molecular sieve is housed, purifying dehydration, and cat head goes out to meet the Skellysolve A of import standard.These processing condition: adsorption temp is 20～30 ℃, adsorptive pressure 390～590KPa, and the absorption air speed is 2.0 cubic metres of (2.0m per hour
3H
-1).
The inventive method, the tops that goes for reforming, pentane oil, carbon five lighter hydrocarbons, oil field lightweight wet goods light hydrocarbon feedstocks.The part processing parameter that only needs to change wherein gets final product.
Claims (3)
1. method of producing the high purity Skellysolve A, with reformation tops, pentane oil, carbon five lighter hydrocarbons or oil field lightweight oil is raw material, form by two-tower rectification, refining and molecular sieve dehydration process, it is characterized in that: described treating process, 3 processes by arbitrary combination are formed, 1. alkaline aqueous solution is 0.2～2 with thick Skellysolve A volume ratio, respectively by the pump input mixer, then mixed solution is entered settlement separate jar, 10～30 ℃ of temperature, pressure 0.2～0.5MPa, duration of contact 2～8min, Skellysolve A is drawn from separating tank top; 2. thick Skellysolve A mixes with dilute sulphuric acid, and 3～10% dilute sulphuric acid is 0.5～4 with thick Skellysolve A volume ratio, and mixed solution enters settlement separate jar, 10～30 ℃ of temperature, pressure 0.2～0.5MPa, mixing duration of contact is 2～8min, thick Skellysolve A is drawn from separating tank top; 3. taking off aromatic solvent is 0.5～5 with thick Skellysolve A volume ratio, by after being pumped into mixing tank mixing contact, enters settlement separator and separates respectively, and extraction temperature is 50～150 ℃, and extracting pressure is 0.2～0.5MPa, and thick Skellysolve A takes out from the tank top.
2. the method for production Skellysolve A according to claim 1 is characterized in that: every meter plate number of rectifying tower employing of described two-tower rectification process is 15～20 high efficiency packing filling, and the column plate number of plies of each rectifying tower is 120-180.
3. the method for production Skellysolve A according to claim 1 and 2 is characterized in that: described alkaline aqueous solution is sodium hydroxide (NaOH) and methyl alcohol (CH
3OH) mixed solution, concentration are 60～80%, wherein NaOH 5～14%, CH
3OH 75～46%.
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| CN 00122981 CN1342630A (en) | 2000-09-12 | 2000-09-12 | Process for preparing high-purity n-pentane |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591558A (en) * | 2008-05-29 | 2009-12-02 | 北京三聚环保新材料股份有限公司 | A kind of in the hydrocarbon material dearsenicating technology high precision, capacity dehydration method |
| CN101602641B (en) * | 2009-07-09 | 2012-12-26 | 天津大学 | Double-effect rectification method and system thereof for finely separating hybrid pentane isomer |
| CN104958919A (en) * | 2015-07-13 | 2015-10-07 | 中国石油化工集团公司 | Multi-component rectifying tower and waste heat recycling method for same |
| CN105363420A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Dehydrating agent used for producing pentane meeting quality requirements of heat-carrying agent for polyolefin |
| CN105461503A (en) * | 2014-08-27 | 2016-04-06 | 中国石油化工股份有限公司 | Refining and dehydrating method for pentane |
| CN111057581A (en) * | 2018-10-17 | 2020-04-24 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for removing aromatic hydrocarbon from industrial grade light hydrocarbon |
| CN113004112A (en) * | 2021-03-04 | 2021-06-22 | 滁州市润达溶剂有限公司 | Isohexane preparation process |
-
2000
- 2000-09-12 CN CN 00122981 patent/CN1342630A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591558A (en) * | 2008-05-29 | 2009-12-02 | 北京三聚环保新材料股份有限公司 | A kind of in the hydrocarbon material dearsenicating technology high precision, capacity dehydration method |
| CN101602641B (en) * | 2009-07-09 | 2012-12-26 | 天津大学 | Double-effect rectification method and system thereof for finely separating hybrid pentane isomer |
| CN105363420A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Dehydrating agent used for producing pentane meeting quality requirements of heat-carrying agent for polyolefin |
| CN105461503A (en) * | 2014-08-27 | 2016-04-06 | 中国石油化工股份有限公司 | Refining and dehydrating method for pentane |
| CN104958919A (en) * | 2015-07-13 | 2015-10-07 | 中国石油化工集团公司 | Multi-component rectifying tower and waste heat recycling method for same |
| CN104958919B (en) * | 2015-07-13 | 2016-10-05 | 中国石油化工集团公司 | A kind of Multicomponent and the method for heat recovery thereof |
| CN111057581A (en) * | 2018-10-17 | 2020-04-24 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for removing aromatic hydrocarbon from industrial grade light hydrocarbon |
| CN113004112A (en) * | 2021-03-04 | 2021-06-22 | 滁州市润达溶剂有限公司 | Isohexane preparation process |
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