CN101265419B - One-stage medium-pressure hydrogenation method for producing food-level white oil - Google Patents
One-stage medium-pressure hydrogenation method for producing food-level white oil Download PDFInfo
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Abstract
The invention relates to a method for producing food-grade white oil through a medium pressure hydrogenation. After raw oil and hydrogen gas are mixed, the hydrogenation reaction is performed, under the reaction conditions as follows: the temperature is 180 to 320 DEG C, the hydrogen partial pressure is 4.0 to 1.0 Mpa, the volume space velocity is 0.1 to 1.0h<-1>, and the hydrogen and oil volume ratio is (200-1000):1; the catalyst pore volume is 0.4 to 1.0ml.g<-1>, and the specific surface area is 150 to 280m<2>.g<-1>; the content of active component metal Ni is 1 to 55 percent of the total weight of the catalyst, the carrier adopts the mixture of macropore aluminium oxide and microbore aluminium oxide, the weight ratio of the both is (2-4):1, silicon or/and phosphor is (are) added in thecarrier as the additive, the content of the silicon in aluminium oxide is 1 to 20 percent, the content of the phosphor is 1 to 10 percent, or the content of the silicon and the phosphor is 1 to 10 percent. The method has the advantages that the process is simple, the operation is convenient, the investment and the operation costs are low, the raw material source is wide, and the method is appliedto the production of the food-grade white oil.
Description
Technical field
The present invention relates to a kind of is raw material with lubricant base or industrial white oil after refining, adopts one section medium-pressure hydrocracking to produce the method for food-level white oil.
Background technology
Characteristics such as white oil is meant the mineral oil through deep refining, has the color water-white, and is transparent, and impurity such as the heterogeneous ring compound of sulfur-bearing, nitrogen, oxygen, aromatic hydrocarbons are low all have in industrial circle and household chemicals manufacturing very and use widely.White oil also can be divided into technical grade, the level/pharmaceutical grade of making up and food grade according to features such as its foreign matter content, colors.Wherein the refining degree of food-level white oil is the darkest, specification of quality is the strictest.
The hydrofining method is produced white oil, and its cardinal principle is by hydrogenation, makes non-hydrocarbon compound hydrogenolysis such as sulphur in the stock oil, nitrogen, oxygen, makes alkene, arenes selectivity hydrogenation saturated, and can remove impurity such as metal, asphalt colloid.Principal reaction in hydrogenation process is desulfurization, denitrogenation, deoxidation, alkene and aromatic hydrocarbons saturated, and hydrodemetallation (HDM).Because product is extremely strict to the restriction of aromaticity content, and the hydrogenation of aromatic hydrocarbons is subjected to thermodynamics equilibrium limit to be difficult at high temperature carry out, all adopt high pressure, low temperature hydrogenation so write articles the preceding production white oil technology of introducing to this patent, and, adopt one-stage hydrogenation or multistage hydrogenation technique according to different with to product requirement of raw material.With quality raw material preferably, as hydrocracking tail oil, or through the lubricant base of peracid pre-refining, general aromaticity content is lower than 5%, can obtain industrial grade white oil through one-stage hydrogenation.With fair raw material, as lubricant base or solvent treatment dewaxing wet goods, aromaticity content is 10%～20%, and through two-stage hydrogenation, one-stage hydrogenation can obtain industrial grade white oil, and secondary hydrogenation can obtain food cosmetic grade white oil.If raw material is poorer,, then need hydrogenation more than three sections as vacuum distillate.
The one-stage hydrogenation process that CN1510110A introduces, its processing condition hydrogen dividing potential drop 8.0～20.0MPa, 180～270 ℃ of temperature, volume space velocity 0.15～1.2h
-1, hydrogen to oil volume ratio 150～800:1.
CN1362486A has introduced a kind of one-stage serial explained hereafter method.The hydrogenation technique condition is: pressure 8.0～20.0MPa; 150～300 ℃ of temperature of reaction; Volume space velocity 0.1～1.5h
-1Hydrogen to oil volume ratio 100～1500:1.
US4072603 has also introduced a kind of method of one-stage hydrogenation manufacture white oil.This method is a raw material with the hydrocracking tail oil after dewaxing, and adopting tungsten one nickel that is carried on silicon one alumina supporter is hydrogenation catalyst.But this method also can only the manufacture grade white oil.
US4055481 has introduced a kind of method that adopts two-stage hydrogenation to produce white oil.This method is raw material with the lubricant base, obtains the intermediates of low-sulfur, low arene content through the hydrogenation of first section sulfur resistant catalyst, and the lights removal that produces in hydrogenation process through distillation enters second section hydrogenation then again.Second section hydrogenation adopts the nickel catalyzator that is carried on the alumina supporter, and product can reach the food-level white oil specification of quality behind hydrogenation.
Take a broad view of above-mentioned prior art, one-stage process can only the manufacture grade white oil; Though and two-stage method can be produced food-level white oil, need with two kinds of different hydrogenation catalysts, and be difficult to produce food-level white oil in the industrial practice.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with lubricant base or industrial white oil after refining, adopts one section medium-pressure hydrocracking to produce the method for food-level white oil.
Technical process of the present invention is as described below: stock oil and hydrogen enter reactor after mixing, and contact with catalyzer, take off S, take off N and aromatic hydrocarbons saturated reaction, and reaction product obtains the food-level white oil product after stripping or distillation; Hydrogenation conditions is: 180～320 ℃ of temperature, hydrogen dividing potential drop 4.0～10.0MPa, volume space velocity 0.1～1.0h
-1, hydrogen to oil volume ratio 200～1000:1; The preferred reaction conditions of hydrogenation reaction of the present invention is 210～300 ℃ of temperature, hydrogen dividing potential drop 6.0～8.0MPa, volume space velocity 0.3～0.6h
-1, hydrogen to oil volume ratio 400～800:1.
Present method catalyst system therefor pore volume is 0.4～1.0ml.g
-1, specific surface area 150～280m
2.g
-1This catalyzer contains a kind of metal Ni, take on the activity of such catalysts component, active ingredient is supported on the alumina supporter, the content that reactive metal is fit to is counted 1～55% of total catalyst weight by oxide weight, preferred content is 30～50%, and active metal component can be to go back ortho states, oxidation state, and is wherein better to go back ortho states.The carrier of catalyst system therefor is the mixture of macroporous aluminium oxide and little porous aluminum oxide, little porous aluminum oxide is a pseudo-boehmite, require it to contain the gibbsite amount and be no more than 3w%, the weight ratio of macroporous aluminium oxide and little porous aluminum oxide is 2～4: 1, silicon is or/and phosphorus is auxiliary agent adds in the carrier, be that silicone content is 1～20w% in the benchmark aluminum oxide with the catalyzer wherein by oxide weight, more preferably silicone content is 1～10w%, phosphorus content is 1～10W%, preferred phosphorus content is 2～5W%, silicon and phosphorus content are 1～10w%, and its surplus is a vehicle weight.
Preparation of catalysts method used herein is as follows: will add mineral acid behind the macroporous aluminium oxide of siliceous and phosphorus, the aperture alumina powder thorough mixing, make the plasticity-mashed prod, be extruded into leafy careless type by orifice plate, become the carrier of this catalyzer after drying, the activation.Active ingredient Ni adopts a step to be total to steeping fluid and is dipped on the carrier.Promptly get catalyzer of the present invention after catalyzer drying behind the dipping, roasting, the activation.Above-mentioned macroporous aluminium oxide can obtain suitable micropore like this and distribute and enough big pore volume by repeatedly becoming the preparation of glue method, can make silicon or phosphoric be well-dispersed in alumina surface, helps improving activity of such catalysts.
The raw material of technical solution of the present invention can be hydrocracking tail oil dewaxing treated oil, lubricant base or an industrial white oil, requires viscosity 10～40mm
2.s
-1(40 ℃), sulphur content ≯ 15mg.kg
-1, nitrogen content ≯ 10mg.kg
-1, aromaticity content＜10w%.Because of the hydrogenation of condensed-nuclei aromatics and heterogeneous ring compound is undertaken by ring stage by stage, removing of impurity such as ring filling and sulphur, nitrogen is relevant with the hydrogenation performance, and open loop is relevant with the catalyst acid sexual function, so it is difunctional to require catalyst system therefor to have.Catalyst metal content height of the present invention, and add auxiliary agent Si or the P with acid function makes this catalyzer have certain acid function, thereby has the higher activity and the hydrogenation degree of depth, impurity such as its sulphur, nitrogen remove and the aromatic hydrocarbons saturability stronger.Qing gas Chun Du ≧ 85v%, Liuization Qing Han Liang ≦ 15mlm in the hydrogen
-3
Under processing condition of the present invention and catalyzer, can in one-stage hydrogenation, promptly obtain the food-level white oil of top grade product under the press strip spare.Technology of the present invention is simple, and is easy to operate, and investment and process cost are low, and raw material sources are extensive, have obvious improvement.
Embodiment
1, the preparation of hydrogenation catalyst
Embodiment 1
The preparation of support of the catalyst: a kind of siliceous and phosphorus macropore and aperture aluminum hydroxide solid elastomer are made into 1000g by mass ratio 4:1, add acetic acid 25g, citric acid 25g, sesbania powder 25g and deionized water 800ml, mix and pinch extruded moulding, 110 ℃ of dry 3h, 550 ℃ of roasting 3h make carrier.The pore volume of this carrier is 0.82ml.g
-1, specific surface is 316m
2.g
-1, tap density is 540kg.m
-3, be shaped as cylindric, granularity Φ 1.6 * (4-6) mm, 120 ℃ of oven dry 3h.
The preparation of steeping fluid: under 20 ℃ of temperature, add the 810g nickelous nitrate in the 500ml deionized water, stirring and dissolving, filter nickel nitrate aqueous solution 1000ml, containing NiO in this solution is 264kg.m
-3
Get the carrier 100g of preparation, the steeping fluid 150ml of preparation, 20 ℃ of following excessive dippings, 110 ℃ of oven dry 3h, 480 ℃ of roasting 3h are cooled to room temperature and make catalyzer and be designated as C1.Main physico-chemical property sees Table 1
Embodiment 2
Embodiment 1 is made the 3rd step operation that catalyzer repeats embodiment 1, make catalyzer and be designated as C2, main physico-chemical property sees Table 1.
Embodiment 3
Embodiment 2 is made catalyzer repeat embodiment 2 operations, make catalyzer and be designated as C3, main physico-chemical property sees Table 1.
The main physico-chemical property of table 1 white oil Hydrobon catalyst
| Catalyzer | ω(NiO)/m％ | Profile | Side pressure strength //Ncm -1 | Bulk density/gml -1 | Pore volume/mlg -1 | Specific surface/m 2·g -1 |
| C1 | 22.3 | Trifolium | 127 | 0.77 | 0.64 | 264 |
| C2 | 41.2 | Trifolium | 159 | 0.94 | 0.34 | 186 |
| C3 | 51.4 | Trifolium | 170 | 1.07 | 0.28 | 178 |
2, the activation of catalyzer
Embodiment 4
The catalyzer of embodiment 1,2,3 preparations is put into fixed-bed reactor before use, carries out hydrogen reduction, and the reductive condition sees Table 2.
The processing condition of table 2 catalyzer hydrogen reduction
| Catalyzer | Hydrogen pressure/MPa | Gas agent volume ratio | First constant temperature zone/℃ | Constant temperature time/h | Second constant temperature zone/℃ | Constant temperature time/h | The 3rd constant temperature zone/℃ | Constant temperature time/h | The 4th constant temperature zone/℃ | Constant temperature time/h |
| C1 | 6.5 | 700 | 120 | 4 | 240 | 4 | 300 | 8 | 340 | 4 |
| C2 | 7.0 | 600 | 120 | 6 | 240 | 6 | 300 | 8 | 340 | 6 |
| C3 | 7.5 | 700 | 120 | 6 | 240 | 6 | 300 | 8 | 340 | 6 |
3, produce the method for food-level white oil
The embodiment of the invention is all carried out on continous way small fixed hydrogenation unit, and the catalyst system therefor carrier is identical.
Embodiment 5
Present embodiment is the preparation method of 15# food-level white oil.Used stock oil is the lubricant base of Dushanzi petro-chemical corporation of CNPC in the present embodiment, and its character sees Table 3.The Hydrobon catalyst of present embodiment is by the C3 catalyzer that embodiment 3 obtains, and puts it in the fixed-bed reactor and forms beds, carries out cooling to 190 ℃ of side line oil-feed material after hydrogen reduction constant temperature finishes according to the reductive condition of table 2.
When carrying out hydrofining, the processing condition of fixed-bed reactor are: reaction pressure is that 7.0MPa, 210 ℃ of temperature, hydrogen to oil volume ratio are 500, volume space velocity is 0.4h
-1Present embodiment only need pass through one stage hydrofining, can produce qualified 15# food-level white oil.Product analysis the results are shown in Table 4.
Embodiment 6
Present embodiment is the preparation of 26# food-level white oil.Used stock oil is grand hundred million 26# of the chemical company industrial grade white oils in Fushun in the present embodiment.Main character sees Table 3.Catalyzer is catalyzer C2, and reductive condition sees Table 2.Processing condition are: reaction pressure is that 8.0MPa, temperature are that 220 ℃, hydrogen to oil volume ratio are 600, volume space velocity is 0.4h
-1The analytical results of 26# food-level white oil sees Table 4.
Table 3 raw material physico-chemical property
| Project | Lubricant base | The 26# industrial white oil |
| Flash-point (opening)/℃ | 221 | 218 |
| Outward appearance (range estimation) | Slightly yellow has fluorescence | Water white transparency |
| Condensation point/℃ | -19 | -16 |
| Kinematic viscosity (40 ℃)/mm 2.s | 16.5 | 27.4 |
| Condensed-nuclei aromatics, ultraviolet absorptivity/cm -1(260-420nm) | 1.786 | 0.164 |
| S/mg.kg -1 | 6.0 | 2.8 |
| N/mg.kg -1 | 4.2 | 2.2 |
| Acid number mgKOH/g | 0.005 | - |
| Carbon residue % | 0.002 | - |
| Colloid % | 0.14 | - |
Table 4 white oil product analysis result
| Project | The 15# quality index | The 15# analytical results | The 26# quality index | The 26# analytical results | Test method |
| Kinematic viscosity (40 ℃)/mm2.s-1 | 12.5～17.5 | 16.8 | 24～28 | 26.4 | GB/T265 |
| Flash-point (opening)/℃ | Be not less than 165 | 218 | Be not less than 165 | 221 | GB/T3536 |
| Color is not less than for Sai Shi number | +30 | +30 | +30 | +30 | GB/T3555 |
| Water soluble acid or alkali | Do not have | Do not have | Do not have | Do not have | GB/T259 |
| Mechanical impurity/%m | Do not have | Do not have | Do not have | Do not have | GB/T511 |
| Moisture/%m | Do not have | Do not have | Do not have | Do not have | GB/T260 |
| Arsenic/mg.kg-1 is not more than | 1 | 0.01 | 1 | 0.01 | GB/T8450 |
| Heavy metal/mg.kg-1 is not more than | 10 | 1 | 10 | 1 | GB/T8451 |
| Lead/mg.kg-1 is not more than | 1 | 0.01 | 1 | 0.01 | GB/T8449 |
| Readily carbonizable substance | By | By | By | By | GB/T11079 |
| Solid paraffin | By | By | By | By | SH/T0134 |
| Condensed-nuclei aromatics, ultraviolet absorptivity/cm -1(260-420nm) | Be not more than 0.1 | 0.03 | Be not more than 0.1 | 0.026 | GB/T11081 |
Claims (7)
1. the method for food-level white oil is produced in one section medium-pressure hydrocracking, it is characterized in that: stock oil and hydrogen enter reactor after mixing, contact with catalyzer, take off S, take off N and aromatic hydrocarbons saturated reaction, reaction product obtains the food-level white oil product after stripping or distillation;
Hydrogenation conditions is: 180～320 ℃ of temperature, hydrogen dividing potential drop 4.0～10.0MPa, volume space velocity 0.1～1.0h
-1, hydrogen to oil volume ratio 200～1000: 1;
Catalyzer is that the mixture with macroporous aluminium oxide and little porous aluminum oxide is that carrier immerses nickeliferous metallic salt, and pore volume is 0.4～1.0ml.g
-1, specific surface area 150～280m
2.g
-1
The content of catalyst activity component metals Ni is counted 1～55% of total catalyst weight by oxide weight, carrier is the mixture of macroporous aluminium oxide and little porous aluminum oxide, the weight ratio of macroporous aluminium oxide and little porous aluminum oxide is 2～4: 1, little porous aluminum oxide is a pseudo-boehmite, contain gibbsite weight less than 3% of its weight, be added with silicon in the carrier or/and phosphorus is auxiliary agent, it is as the criterion with total catalyst weight by oxide weight, in the aluminum oxide silicone content be 1～20% or phosphorus content be 1～10% or silicon and phosphorus content be 1～10%, its surplus is a vehicle weight;
Described stock oil is hydrocracking tail oil dewaxing treated oil, lubricant base or industrial white oil, requires viscosity 10～40mm
2.s
-1(40 ℃), sulphur content ≯ 15mg.kg
-1, nitrogen content ≯ 10mg.kg
-1, aromaticity content＜10w%.
2. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, and it is characterized in that: the condition of hydrogenation reaction is 210～300 ℃ of temperature, hydrogen dividing potential drop 6.0～8.0MPa, volume space velocity 0.3～0.6h
-1, hydrogen to oil volume ratio 400～800: 1.
3. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, and it is characterized in that: the content of metal Ni is counted 30～50% of total catalyst weight by oxide weight.
4. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, and it is characterized in that: active metal component can be to go back ortho states or oxidation state.
5. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, and it is characterized in that: be as the criterion with total catalyst weight by oxide weight, silicone content is 1～10%.
6. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, and it is characterized in that: be as the criterion with total catalyst weight by oxide weight, phosphorus content is 2～5%.
7. the method for food-level white oil is produced in one section medium-pressure hydrocracking according to claim 1, it is characterized in that: hydrogen purity 〉=85v%, hydrogen sulfide content≤15mlm in the hydrogen
-3
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013644B (en) * | 2011-09-22 | 2014-12-03 | 中国石油化工股份有限公司 | Method for producing base oil from waste lubricating oil |
| CN104212490B (en) * | 2014-08-26 | 2016-01-20 | 天津凯威永利联合化学有限责任公司 | A kind of preparation method of low viscosity white oil |
| CN107629817B (en) * | 2017-10-20 | 2020-01-31 | 神华集团有限责任公司 | Preparation method of white oil |
| CN109722300B (en) * | 2017-10-31 | 2021-05-14 | 中国石油化工股份有限公司 | Hydrogenation method for producing crude white oil |
| CN109735365A (en) * | 2019-02-26 | 2019-05-10 | 宁波科元精化有限公司 | A kind of technique that heavy raw oil produces No. 7 white oils |
| CN112226210A (en) * | 2020-11-08 | 2021-01-15 | 盘锦北方沥青股份有限公司 | Heat conduction oil with low oil sludge tendency and preparation method thereof |
| CN115322805B (en) * | 2022-09-01 | 2023-05-02 | 道尔顿(广东)新材料科技有限公司 | Preparation method of food-grade white oil |
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|---|---|---|---|---|
| US4072603A (en) * | 1976-10-29 | 1978-02-07 | Suntech, Inc. | Process to make technical white oils |
| CN1049800A (en) * | 1989-08-28 | 1991-03-13 | 中国石油化工总公司石油化工科学研究院 | The preparation of nickel/aluminium oxide catalyst |
| CN1362486A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Hydrogenation process of producing food-level white oil |
| CN1510110A (en) * | 2002-12-24 | 2004-07-07 | 中国石油化工股份有限公司 | Production of high viscosity food grade white oil |
| CN1769380A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | One-step hydrogenation method for producing super white oil |
-
2007
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4072603A (en) * | 1976-10-29 | 1978-02-07 | Suntech, Inc. | Process to make technical white oils |
| CN1049800A (en) * | 1989-08-28 | 1991-03-13 | 中国石油化工总公司石油化工科学研究院 | The preparation of nickel/aluminium oxide catalyst |
| CN1362486A (en) * | 2001-01-05 | 2002-08-07 | 中国石油化工股份有限公司 | Hydrogenation process of producing food-level white oil |
| CN1510110A (en) * | 2002-12-24 | 2004-07-07 | 中国石油化工股份有限公司 | Production of high viscosity food grade white oil |
| CN1769380A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | One-step hydrogenation method for producing super white oil |
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