CN103833499B - A kind of preparation method of high purity isohexane solvent oil - Google Patents
A kind of preparation method of high purity isohexane solvent oil Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high purity isohexane solvent oil; By reforming raffinate oil hydrofining, adopt nickel catalyst, processing condition: pressure is 0.2 ~ 2.0Mpa, temperature is 80 ~ 220 DEG C, and air speed is 2.0 ~ 4.0h-1, and hydrogen-oil ratio is 40 ~ 200v/v; Hydrorefined reforming raffinate oil is excised on true boiling point distillation instrument > 65 DEG C of cuts, above-mentioned steps is repeated 3 times and collect≤65 DEG C of cuts, by collect≤65 DEG C of cuts cut on true boiling point distillation instrument again, tower top distillates product and adopts multiple bottle to collect differing temps section product, every 0.5 DEG C is a fraction section, obtains the isohexane product that purity is 95.323% between 59.5-62 DEG C; Present method take reforming raffinate oil as raw material, adopts high reactivity nickel catalyst hydrofining Arene removal and alkene, and true boiling point distillation instrument obtains by cutting twice fractionation the isohexane product that purity is not less than 95%.
Description
Technical field
The present invention relates to a kind of preparation method of high purity isohexane solvent oil, is a kind of by refining, that separation means obtains high purity product preparation method.
Background technology
Along with the rapid growth of national economy, the demand of various varsol product constantly increases, and people to health environment-friendly be familiar with day by day deep, the quality of every profession and trade to varsol is made to it is also proposed stricter requirement, therefore, from seed output and quality two aspects, varsol has the huge market space and development space in China, special solvent oil is developed into from usual vehicle oil to the demand of solvent oil in market, wherein low impurity, narrow boiling range, just highly purified/isoparaffin solvent oil has good solvability because of it, higher security, less toxicity, suitable volatility, and the feasibility that other solvent oil products alternative are used for every profession and trade is subject to market favor gradually.
Isohexane is a kind of non-polar solvent, water insoluble, is dissolved in ethanol, ether, can also dissolve other hydro carbons and halohydrocarbon, be mainly used in solvent for polymerization, agent released by precision instrumentation cleaning and oil, essential oil thinners etc., are mainly used in the product scopes such as non-toxic spray, solvent, clean-out system.At present, isohexane is domestic has part refinery to produce, such as, Lanzhou, Liaoyang, Dalian, the Yanshan Mountain, Yang Zi, output is many within 10,000 tons/year, all parts of the country are sold on the basis meeting our factory's consumption, sales situation is good, due to the few huge market demand of isohexane output, price was in ascendant trend always in recent years, the isohexane price of purity requirement in August 95% in 2012 is about 12000 yuan/ton, isohexane is in backorder status in China at present, major part depends on import, China now only has Herpu Chemical Co., Ltd., Guangzhou one to stablize provides isohexane in a large number, there is the isohexane production marketing of different purity on the flourishing ground such as city and Liaoyang, northeast of coastal economy, but mostly be only to sell and do not produce, and supply is all little.
CN95121454.3 discloses a kind of preparation method of the product containing Trimethylmethane/isohexane.The method comprises sends iso-pentane raw material into disproportionation step, under the existence of alkene and/or senior branched paraffin by with acidity H
othe temperature exposure of the acid catalyst being greater than 8 between 0 ~ 150 ° of C and by iso-pentane raw material disproportionation, take out the product containing Trimethylmethane/isohexane.
CN200410027004.5 discloses a kind of manufacture method of isohexane solvent.The method is with 6# solvent oil for raw material, and adopt packing tower fractionation cutting to collect the cut of 58 ~ 63 DEG C, this cut finally obtains the isohexane containing more than 95% through hydrogenation.The method list tower continuous seepage, less investment, floor space is little, operates, manages simply, efficiently.
CN200910083134.3 discloses a kind of preparation method of narrow fraction nontoxic high-purity isohexane.The method is raw material with reforming raffinate oil, selects active metal nickel to be benzene series catalytic hydrogenation catalyst, under the effect of catalyzer, carries out total composition shortening, de-aromatizing and desulfurizing; Product through de-aromatizing and desulfurizing is introduced lightness-removing column, removes the light constituent of cut≤60 DEG C; Introduce weight-removing column by through de-light residue cut, remove the heavy constituent of cut >=75 DEG C; Carrying out meticulous fractionation by introducing isohexane tower through de-heavy residue cut (60 ~ 75 DEG C), cutting 60 ~ 64.5 DEG C of cuts and being required product.The method catalyzer operational condition is relatively gentle, de-aromatizing and desulfurizing Be very effective, features simple and practical process, and stable and reliable product quality, economical efficiency are high.
CN201110263745.3 mono-kind is by the processing method of thick hexane extraction normal hexane, isohexane, CN201120334519.5 mono-kind is by the device of thick hexane extraction normal hexane, isohexane, CN201120334491.5 mono-kind is by the hydro-refining unit of thick hexane extraction normal hexane, isohexane, CN201120334470.3 mono-kind is by the fractionation plant of thick hexane extraction normal hexane, isohexane, and above-mentioned four patents have carried out comprehensive description from the hydrofining unit of processing method, industrial installation, device and product fractionation unit four aspects to production just/isohexane.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high purity isohexane solvent oil, take reforming raffinate oil as raw material, adopt high reactivity nickel catalyst hydrofining Arene removal and alkene, true boiling point distillation instrument obtains by cutting twice fractionation the isohexane product that purity is not less than 95%.
The preparation method of high purity isohexane solvent oil of the present invention adopts following technical scheme:
(1) preparation of high reactivity nickel catalyst, adds sesbania powder, after nitric acid, phosphoric acid, water mediates in aluminium hydroxide dry powder, extruded moulding, 120 DEG C of dry 2h, 550 DEG C of roasting 4h, obtained support of the catalyst; Prepare nickeliferous and solution that is promoter metal, equivalent impregnation on alumina supporter, 120 DEG C of dry 2h, 500 DEG C of roasting 4h, obtained catalyzer, the active metal of catalyzer is in its content of NiO for 25% ~ 50%, and preferred metal content is 30% ~ 35%;
(2) reforming raffinate oil hydrofining on 100mL small hydrogenation device, adopts nickel catalyst prepared by step 1, at pressure range 0.2 ~ 2.0Mpa, and temperature range 80 ~ 220 DEG C, space velocity range 2.0 ~ 4.0h
-1, under the processing condition of hydrogen-oil ratio scope 40 ~ 200v/v, product sulphur content < 0.5 μ g/g, bromine index < 0.2mgBr/100g, aromaticity content < 0.001m%.
(3), > 65 DEG C of cuts will be excised through the hydrorefined reforming raffinate oil of step 2 on true boiling point distillation instrument, this true boiling point distillation instrument meets ASTMD2892 standard, theoretical plate number 15 pieces, tower reactor volume 20L, trim the top of column is than 10 ~ 20:1, and tower reactor heats aperture 20% ~ 40%.
(4), step 3 is repeated 3 times and collect≤65 DEG C of cuts, ≤ 65 DEG C of fractions consistings are in table 1, by collect≤65 DEG C of cuts cut on true boiling point distillation instrument again, trim the top of column compares 20:1, tower reactor heating aperture 20%, tower top distillates product and adopts multiple bottle to collect differing temps section product, and every 0.5 DEG C is a fraction section, obtains the isohexane product that purity is 95.323% between 59.5-62 DEG C.
Invention effect
1, the present invention is that raw material carries out hydrogenation with reforming raffinate oil, and catalyst activity is high, and product property is excellent, can carry out comprehensive utilization of separation according to the finished product target to raffinating oil, and reduces the necessity of refining after target product needs.
2, the nickel catalyst that prepared by the present invention can make hydrogenated products take off to containing alkene and aromatic hydrocarbons hardly under the processing condition comparatively relaxed, and hydrofining effect is very remarkable.
3, the true boiling point distillation instrument of 15 pieces has carried out cutting twice fractionation to hydrorefined raffinating oil in the present invention, having used every 0.5 DEG C is cleverly that a fraction section collects product, investigate the purity of each fraction section isohexane, search out optimum cutting temperature section.
4, the present invention is in product separation process, and adopting every 0.5 DEG C of multiple bottle to be that a fraction section collects product, is the key obtaining high purity isohexane product on the true boiling point distillation instrument that theoretical plate number is lower.
Accompanying drawing explanation
Fig. 1 flowsheeting schema.
Embodiment
A preparation method for high purity isohexane solvent oil, is characterized in that:
(1), the preparation of nickel catalyst
In aluminium hydroxide dry powder, add sesbania powder, after nitric acid, phosphoric acid, water mediates, extruded moulding, 120 DEG C of dry 2h, 550 DEG C of roasting 4h, obtained support of the catalyst; Prepare nickeliferous and solution that is promoter metal, equivalent impregnation is on alumina supporter, and 120 DEG C of dry 2h, 500 DEG C of roasting 4h, obtain catalyzer.
The active metal of catalyzer is in its content of NiO for 25m% ~ 50m%, and preferred metal content is 30m% ~ 35m%, and profile is trifolium bar Ф 1.3 × 3 ~ 8mm, and bulk density is 0.9 ~ 1.1g/ml, and specific surface area is 120 ~ 160cm
2/ g, intensity>=220N/cm.
(2) reforming raffinate oil hydrofining removes sulphur, alkene and aromatic hydrocarbons
In reforming raffinate oil, isohexane content is 18% ~ 35%, and boiling range≤130 DEG C, sulphur content≤3.0 μ g/g, bromine index≤4000mgBr/100g, aromaticity content are 0.90% ~ 1.90%.
Reforming raffinate oil hydrofining on 100mL small hydrogenation device, adopts nickel catalyst prepared by step 1, at pressure range 0.2 ~ 2.0Mpa, and temperature range 80 ~ 220 DEG C, space velocity range 2.0 ~ 4.0h
-1, under the processing condition of hydrogen-oil ratio scope 40 ~ 200v/v, product sulphur content < 0.5 μ g/g, bromine index < 0.2mgBr/100g, aromaticity content < 0.001m%.
(3), true boiling point distillation instrument removes heavy constituent
> 65 DEG C will be excised on true boiling point distillation instrument through the hydrorefined reforming raffinate oil of step 2, this true boiling point distillation instrument meets ASTMD2892 standard, theoretical plate number 15 pieces, tower reactor volume 20L, trim the top of column is than 10 ~ 20:1, and tower reactor heats aperture 20% ~ 40%.
(4), light constituent segmentation cutting and product-collecting
Step 3 is repeated 3 times and collect≤65 DEG C of cuts, ≤ 65 DEG C of fractions consistings are in table 1, by collect≤65 DEG C of cuts cut on true boiling point distillation instrument again, trim the top of column compares 20:1, tower reactor heating aperture 20%, tower top distillates product and adopts multiple bottle to collect differing temps section product, and every 0.5 DEG C is a fraction section, and composition is in table 1.The isohexane product that purity is 95.323% is obtained between 59.5-62 DEG C.
Product composition (wt%) that table 1 is collected
| Cut title | Yield, % | Normal hexane | Isohexane | Carbon six naphthenic hydrocarbon |
| ≤ 65 DEG C of cuts | / | 14.121 | 76.593 | 4.514 |
| 58.5-59.5℃ | 4.70 | 1.55 | 91.880 | 0.242 |
| 59.5-60℃ | 5.15 | 1.994 | 93.652 | 0.449 |
| 60-60.5°C | 6.55 | 2.463 | 95.224 | 0.531 |
| 60.5-61℃ | 9.46 | 2.605 | 96.624 | 0.637 |
| 61-61.5℃ | 7.53 | 3.055 | 96.129 | 0.788 |
| 61.5-62℃ | 6.32 | 4.573 | 94.364 | 0.978 |
| 62-62.5℃ | 5.87 | 5.681 | 92.810 | 1.233 |
| 59.5-62℃ | 35.01 | 3.028 | 95.323 | 0.713 |
Adopt the catalyzer of above-mentioned preparation, hydrofining technology technology and isohexane product separation purification mode, the high purity isohexane solvent oil production character of gained is in table 2.
Table 2 isohexane product property
(5), the software simulation of double tower fractionation cutting calculates
True boiling point distillation instrument theoretical plate number is not enough, the isohexane product of purity requirement can not be obtained by single flash cutting, the hydrorefined reforming raffinate oil of step 2 calculates distillation cutting isohexane product on AspenHYSYS process simulation software, adopt cascade towers successively to remove heavy constituent and light constituent, the schema that simulation adopts is shown in Fig. 1.Reforming raffinate oil 7 enters tower 1, removes restructuring 4, and light constituent 3 enters tower 2, and tower top discharges undesirable components 5, obtains isohexane product 6 at the bottom of tower.
The operating parameters of simulation is in table 3, and isohexane product purity and yield are respectively 95.380% and 87.30%.
Table 3 operating parameters
| Project | Tower 1 | Tower 2 |
| Theoretical plate number, block | 40 | 20 |
| Reflux ratio, m/m | 8 | 20 |
| Tower top/bottom pressure, KPa | 5/50 | 5/50 |
| Tower top temperature, DEG C | 57.17 | 37.68 |
| Bottom temperature, DEG C | 97.51 | 72.72 |
Claims (1)
1. a preparation method for high purity isohexane solvent oil, is characterized in that:
(1) preparation of nickel catalyst, adds sesbania powder, after nitric acid, phosphoric acid, water mediates in aluminium hydroxide dry powder, extruded moulding, 120 DEG C of dry 2h, 550 DEG C of roasting 4h, obtained support of the catalyst; Prepare nickeliferous and solution that is promoter metal, equivalent impregnation on alumina supporter, 120 DEG C of dry 2h, 500 DEG C of roasting 4h, obtained catalyzer, the active metal of catalyzer in its content of NiO for 25m% ~ 50m%;
Catalyst appearance is trifolium bar Φ 1.3 × 3 ~ 8mm, and bulk density is 0.9 ~ 1.1g/ml, and specific surface area is 120 ~ 160cm
2/ g, intensity>=220N/cm;
(2) reforming raffinate oil hydrofining removes sulphur, alkene and aromatic hydrocarbons, in reforming raffinate oil, dissident's alkane content is 18% ~ 35%, and boiling range≤130 DEG C, sulphur content≤3.0 μ g/g, bromine index≤4000mgBr/100g, aromaticity content are 0.90% ~ 1.90%; Reforming raffinate oil hydrofining on 100mL small hydrogenation device, adopt nickel catalyst prepared by step 1, processing condition: pressure is 0.2 ~ 2.0Mpa, temperature is 80 ~ 220 DEG C, and air speed is 2.0 ~ 4.0h
-1, hydrogen-oil ratio is under the processing condition of 40 ~ 200v/v, and product sulphur content <0.5 μ g/g, bromine index <0.2mgBr/100g, aromaticity content are <0.001m%;
(3) > 65 DEG C of cuts will be excised through the hydrorefined reforming raffinate oil of step 2 on true boiling point distillation instrument, this true boiling point distillation instrument meets ASTMD2892 standard, theoretical plate number 15 pieces, tower reactor volume 20L, trim the top of column is than 10 ~ 20:1, and tower reactor heats aperture 20% ~ 40%;
(4) step 3 is repeated 3 times and collect≤65 DEG C of cuts, by collect≤65 DEG C of cuts cut on true boiling point distillation instrument again, trim the top of column compares 20:1, tower reactor heating aperture 20%, tower top distillates product and adopts multiple bottle to collect differing temps section product, every 0.5 DEG C is a fraction section, obtains the isohexane product that purity is 95.323% between 59.5-62 DEG C.
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| CN104673381A (en) * | 2015-01-21 | 2015-06-03 | 安徽海德石油化工有限公司 | Method for preparing 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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| 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 |
| CN202237321U (en) * | 2011-09-07 | 2012-05-30 | 洛阳金达石化有限责任公司 | Fractionation plant for extracting n-hexane and isohexane from crude hexane |
| CN202246472U (en) * | 2011-09-07 | 2012-05-30 | 洛阳金达石化有限责任公司 | Device for extracting normal hexane and isohexane from crude hexane |
| CN102675023A (en) * | 2012-05-19 | 2012-09-19 | 淄博汇佳橡胶新型材料有限公司 | Preparation method of narrow-fraction high-purity isohexane |
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Patent Citations (6)
| 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 |
| CN202237321U (en) * | 2011-09-07 | 2012-05-30 | 洛阳金达石化有限责任公司 | Fractionation plant for extracting n-hexane and isohexane from crude hexane |
| CN202246472U (en) * | 2011-09-07 | 2012-05-30 | 洛阳金达石化有限责任公司 | Device for extracting normal hexane and isohexane from crude hexane |
| CN102675023A (en) * | 2012-05-19 | 2012-09-19 | 淄博汇佳橡胶新型材料有限公司 | Preparation method of narrow-fraction high-purity isohexane |
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