CN102675023A - Preparation method of narrow-fraction high-purity isohexane - Google Patents
Preparation method of narrow-fraction high-purity isohexane Download PDFInfo
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- CN102675023A CN102675023A CN201210157047XA CN201210157047A CN102675023A CN 102675023 A CN102675023 A CN 102675023A CN 201210157047X A CN201210157047X A CN 201210157047XA CN 201210157047 A CN201210157047 A CN 201210157047A CN 102675023 A CN102675023 A CN 102675023A
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Abstract
The invention relates to a preparation method of narrow-fraction high-purity isohexane and belongs to the technical field of petrochemical engineering. According to the preparation method, raffinate oil containing isohexane is used as raw materials, firstly, the coarse fractionation is carried out to obtain narrow fractions, and then, Ni/gamma-Al2O3 hydrogenation catalysts are adopted; and the hydrorefining is carried out under the process conditions that the hydrogen oil ratio is (100-400):1, the liquid phase airspeed is 1.0 to 3 h<-1>, the temperature is 170 to 195 DEG C, and the pressure is 1.5 to 3.0 MPa, , finally, the rectification is carried out, 60-to-66 DEG C fractions are obtained, and target products of high-purity extraction solvent isohexane are obtained. The preparation method has the advantages that the narrow-fraction separation method is adopted before the hydrorefining, the subsequent treatment operation flow process is simplified, and the product purity is high.
Description
Technical field
The preparation method of the high-purity isohexane of a kind of narrow fraction belongs to the petrochemical technology field.
Background technology
The grease industry was done discussion to more than 60 kinds of organic solvents, and the azeotropic solvent that discovery isohexane, Virahol, ethanol, acetic acid second extremely reach them all has the feasibility that alternative normal hexane makes to leach solvent.Because the isohexane boiling point is low, is easy to remove, security is superior to normal hexane; And energy cost is low, leaches device and hexane and leaches no especially big change etc., in recent years; In U.S. You Chang commercially produced, isohexane leached from original 1/3 and increases to some extent, and becomes main flow gradually.Therefore, the technology of preparing of high-purity narrow fraction isohexane has become the key that the alternative hexane Vegetable oil fat of isohexane is kept the safety in production and prepared the environmental protection edible oil.
Chinese patent (200410027004.5) discloses a kind of method of manufacture of isohexane solvent.This method is a raw material with No. 6 solvent oils, is on the packing tower of 30 ~ 35:1 at aspect ratio, with working pressure 0.105MPa (cutting off); 50 ~ 55 ℃ of tower top temperatures under the cutting condition of reflux ratio 50 ~ 70, are collected 58 ~ 63 ℃ cut; This cut is at pressure 1.0MPa, 150 ℃ of temperature, air speed 2-3h
-1, hydrogenation under the processing condition of hydrogen-oil ratio 50:1 finally obtains containing the isohexane more than 95%.
Chinese patent (200910083134.3) discloses a kind of preparation method of narrow fraction nontoxic high-purity isohexane.It is the benzene series catalytic hydrogenation catalyst that this method is selected active metal nickel for use; The CR of boiling range≤140 ℃, aromaticity content≤1.3%, sulphur content≤1ppm is raffinated oil and industrial hydrogen together pumps into hydrogenator, is 5.5 ~ 7.5 at hydrogen oil quality ratio: 100, liquid benzene air speed 0.01 ~ 1.0h
-1, 160 ~ 175 ℃ of temperature, pressure 0.3 ~ 1.5MPa condition under, under the effect of catalyzer, carry out total composition shortening, de-aromatizing and desulfurizing; To introduce lightness-removing column through the product of de-aromatizing and desulfurizing, remove the light constituent of cut≤60 ℃; To introduce weight-removing column through taking off light residue cut, remove the heavy constituent of cut>=75 ℃; To carry out meticulous fractionation through taking off heavy residue cut (60 ~ 75 ℃) introducing isohexane tower, and cut 60 ~ 64.5 ℃ of cuts and be required product.
Chinese patent 95121454.3 discloses a kind of preparation method who contains the product of Trimethylmethane/isohexane.This method comprises sends the iso-pentane raw material into the disproportionation step, in the presence of alkene and/or senior branched paraffin through with acidity H
oThe temperature of acid catalyst greater than 8 between 0 ~ 150 ℃ contacts and with iso-pentane raw material disproportionation, takes out the product that contains Trimethylmethane/isohexane.
The method of mentioning in the above-mentioned patent of taking off aromatic hydrocarbons exists technical process complicacy, the single shortcoming of raw material sources.Can not extensively satisfy the actual production requirement of solvent oil deeply de-aromatizing.
Summary of the invention
The technical problem that the present invention will solve is: overcome the deficiency of prior art, provide a kind of technical process simple, the preparation method of the high-purity isohexane of a kind of narrow fraction that the product out-degree is high.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of the high-purity isohexane of this a kind of narrow fraction; It is characterized in that: the cut of raffinating oil to contain isohexane is a raw material; Carrying out roughing out earlier, to obtain boiling range be 60 ~ 70 ℃ narrow fraction; Carry out unifining again, obtain high-purity isohexane of 60 ~ 66 ℃ of cuts.
Concrete process step is:
1, will contain raffinating oil of isohexane carries out roughing out to obtain boiling range is 60 ~ 70 ℃, aromaticity content≤1.3%, sulphur content≤80 μ g/g cuts;
2, will carry out the well-mixed cut of slightly carrying with hydrogen and carry out hydrofining reaction, adopt Ni/ γ-A1 through process furnace
2O
3Hydrogenation catalyst; Processing condition are: at hydrogen-oil ratio is 100 ~ 400:1, liquid phase air speed 1.0 ~ 3.0h
-1, 170 ~ 195 ℃ of temperature, working pressure 1.5 ~ 3.0MPa.
3, the introducing of the product behind hydrogenation aromatics-removing theoretical plate number is 75 rectifying tower, and obtaining 60 ~ 66 ℃ of cuts is the high-purity extraction solvent isohexane of title product.
Concrete, the described cut of raffinating oil that contains isohexane is that pyrolysis gasoline is raffinated oil or aromatic hydrocarbons is raffinated oil or both arbitrary proportion mixtures.
Concrete, said Ni/ γ-A1
2O
3Catalyzer is 21wt%≤NiO≤60wt%, and surplus is A1
2O
3Catalyzer.
Preferably, the working pressure in the said process step 3 is 2.0MPa.
Among the present invention, different according to the raw material sources mode, can raffinate oil and pyrolysis gasoline is raffinated oil with arbitrary proportion blended aromatic hydrocarbons, also can be any one component wherein, two kinds of raw materials can replenish each other, enlarge raw material sources.Do not influence the actual production effect.Mouthful temperature that distillates of rectifying tower top is separated when accurately being controlled at 60 ~ 66 ℃ and is obtained cut among the present invention, and it is 95% high-purity isohexane component that this cut promptly gets purity.
Compared with prior art, the beneficial effect that the preparation method had of the high-purity isohexane of a kind of narrow fraction of the present invention is: the present invention is the raw material production isohexane with the blending ingredients of raffinating oil, and has improved the utilization ratio of sub product in the industrial production, has improved its income.Under situation about being becoming tight market supply day, the present invention utilizes the secondary processing cut to be the raw material production high value added product, open raw material sources newly.The present invention takes the close cut separation method before unifining, simplified the post-treatment operations flow process, and product purity is high.The present invention selects for use and contains the raffinating oil to raw material has improved the utilization ratio of sub product in the industrial production of isohexane, uses special catalyst to keep operational condition gentle relatively.Restriction with processing condition has improved production efficiency.
Embodiment
Below in conjunction with specific embodiment the present invention is described further, wherein embodiment.
Embodiment 1
1, is the raw material of raffinating oil with character such as table 1 raw material A;
2, in water distilling apparatus, mixing raffinated oil and distill, obtain 60 ~ 70 ℃ boiling range, aromaticity content≤1.3%, sulphur content≤80 μ g/g cuts;
3, will carry out the premixed cut of slightly carrying with hydrogen and on the 100ml fixed bed hydrogenation reactor, carry out the hydrogenation experiment.Carry out hydrofining reaction through heating, adopt Ni/ γ-A1
2O
3Hydrogenation catalyst, NiO content are 40wt%, and surplus is A1
2O
3, processing condition are: at hydrogen-oil ratio is 100:1, liquid phase air speed 2.0h
-1, 180 ℃ of temperature, pressure 1.5MPa.In the operating process,, come in contact reaction with catalyzer with getting into from hydrogenator top after raw oil cut and the hydrogen pre-mixing.The mode that test adopts one way to pass through is carried out hydrogenation.Reaction product derives from reactor lower part, is cooled to get into rectifier unit behind the normal temperature and carry out fractionation.
4, to introduce theoretical plate number be that 75 10L rectifying tower reacts back mixing prod fractionation to the product behind the hydrogenation aromatics-removing.Obtaining cut is the high-purity extraction solvent isohexane of title product.
Embodiment 2
Adopt embodiment 1 process mode in processing condition to be: Ni/ γ-A1 with the mixing oil of raw oil character such as table 1 raw material A
2O
3The NiO content of catalyzer is 21wt%, and surplus is A1
2O
3, 170 ℃ of temperature, working pressure 1.8MPa, hydrogen to oil volume ratio 200, air speed 2.3h
-1Carry out hydrofining reaction.Gained hydrogenated products target product character after fractionation is seen table 2 product A.
Embodiment 3
Adopt embodiment 1 process mode in processing condition to be: Ni/ γ-A1 with the mixing oil of raw oil character such as table 1 raw material C
2O
3The NiO content of catalyzer is 35wt%, and surplus is A1
2O
3, 180 ℃ of temperature, working pressure 2.5MPa, hydrogen to oil volume ratio 300, air speed 1.8h
-1Carry out hydrofining reaction.Gained hydrogenated products target product character after fractionation is seen table 2 product B.
Embodiment 4
Adopt embodiment 1 process mode in processing condition to be: Ni/ γ-A1 with the mixing oil of raw oil character such as table 1 raw material D
2O
3The NiO content of catalyzer is 60wt%, and surplus is A1
2O
3, 195 ℃ of temperature, working pressure 2.08MPa, hydrogen to oil volume ratio 400, air speed 3.0h
-1Carry out hydrofining reaction.Institute's gained hydrogenated products target product character after fractionation is seen table 2 products C.
Embodiment 5
Adopt embodiment 1 process mode in processing condition to be: Ni/ γ-A1 with the mixing oil of raw oil character such as table 1 raw material E
2O
3The NiO content of catalyzer is 45wt%, and surplus is A1
2O
3, 190 ℃ of temperature, working pressure 3.0MPa, hydrogen to oil volume ratio 300, air speed 1.5h
-1Carry out hydrofining reaction.Institute's gained hydrogenated products target product character after fractionation is seen table 2 products C.
Table 1 mixing raw material oiliness matter
| Project | Raw material A | Raw material B | Raw material C | Raw material D | Raw material E | Analytical procedure |
| Ratio of mixture | 0:1 | 1:0 | 1:1 | 1:100 | 100:1 | / |
| Sulphur/% | 0.0042 | 0.0088 | 0.0055 | 0.0045 | 0.0085 | SH/T?0253 |
| Aromatic hydrocarbons/% | 1.41 | 1.04 | 1.23 | 1.38 | 1.08 | SH/T?0166 |
| Bromine index, mgBr/100g | 6746 | 9883 | 7073 | 6824 | 9465 | GB/T?11136 |
The high-purity isohexane character of table 2
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any professional and technical personnel of being familiar with possibly utilize the technology contents of above-mentioned announcement to change or be modified as the equivalent embodiment of equivalent variations.But everyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and remodeling that above embodiment did, still belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.
Claims (5)
1. the preparation method of the high-purity isohexane of narrow fraction, it is characterized in that: the cut of raffinating oil to contain isohexane is a raw material, carrying out roughing out earlier, to obtain boiling range be 60 ~ 70 ℃ narrow fraction, carries out unifining again, obtains high-purity isohexane of 60 ~ 66 ℃ of cuts.
2. the preparation method of the high-purity isohexane of a kind of narrow fraction according to claim 1 is characterized in that, concrete process step is:
2.1, will contain raffinating oil of isohexane and carry out roughing out to obtain boiling range be 60 ~ 70 ℃, aromaticity content≤1.3%, sulphur content≤80 μ g/g cuts;
2.2, will carry out the well-mixed cut of slightly carrying with hydrogen and carry out hydrofining reaction through process furnace, adopt Ni/ γ-A1
2O
3Hydrogenation catalyst; Processing condition are: at hydrogen-oil ratio is 100 ~ 400:1, liquid phase air speed 1.0 ~ 3.0h
-1, 170 ~ 195 ℃ of temperature, working pressure 1.5 ~ 3.0MPa.
2.3, to introduce theoretical plate number be 75 rectifying tower to the product behind the hydrogenation aromatics-removing, obtaining 60 ~ 66 ℃ of cuts is the high-purity extraction solvent isohexane of title product.
3. the preparation method of the high-purity isohexane of a kind of narrow fraction according to claim 1 and 2 is characterized in that: the described cut of raffinating oil that contains isohexane is that pyrolysis gasoline is raffinated oil or aromatic hydrocarbons is raffinated oil or both arbitrary proportion mixtures.
4. the preparation method of the high-purity isohexane of a kind of narrow fraction according to claim 2 is characterized in that: said Ni/ γ-A1
2O
3Catalyzer is 21wt%≤NiO≤60wt%, and surplus is A1
2O
3Catalyzer.
5. the preparation method of the high-purity isohexane of a kind of narrow fraction according to claim 2 is characterized in that: working pressure is 2.0MPa in the said step 2.3.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833499A (en) * | 2012-11-27 | 2014-06-04 | 中国石油天然气股份有限公司 | Method for preparing high-purity isohexane solvent oil |
| CN113004112A (en) * | 2021-03-04 | 2021-06-22 | 滁州市润达溶剂有限公司 | Isohexane preparation process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569782A (en) * | 2004-04-27 | 2005-01-26 | 广州赫尔普化工有限公司 | Method for preparing isohexane solvent |
| CN101875594A (en) * | 2009-04-30 | 2010-11-03 | 中国海洋石油总公司 | Method for preparing narrow fraction nontoxic high-purity isohexane |
| CN102351627A (en) * | 2011-09-07 | 2012-02-15 | 洛阳金达石化有限责任公司 | Process method for extracting normal hexane and isohexane from crude hexane |
-
2012
- 2012-05-19 CN CN201210157047.XA patent/CN102675023B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1569782A (en) * | 2004-04-27 | 2005-01-26 | 广州赫尔普化工有限公司 | Method for preparing isohexane solvent |
| CN101875594A (en) * | 2009-04-30 | 2010-11-03 | 中国海洋石油总公司 | Method for preparing narrow fraction nontoxic high-purity isohexane |
| CN102351627A (en) * | 2011-09-07 | 2012-02-15 | 洛阳金达石化有限责任公司 | Process method for extracting normal hexane and isohexane from crude hexane |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833499A (en) * | 2012-11-27 | 2014-06-04 | 中国石油天然气股份有限公司 | Method for preparing high-purity isohexane solvent oil |
| CN103833499B (en) * | 2012-11-27 | 2016-03-09 | 中国石油天然气股份有限公司 | A kind of preparation method of high purity isohexane solvent oil |
| 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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