CN103045303B - A kind of preparation method of refrigerator oil base oil - Google Patents
A kind of preparation method of refrigerator oil base oil Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of refrigerator oil base oil; Take density as 950Kg/m
3~ 1000Kg/m
3, 100 DEG C of kinematic viscosity 200 ~ 1500mm
2the crude oil of/s, or the cycloalkyl long residuum of > 360 DEG C is raw material, through thermally splitting, 360 ~ 420 DEG C of cuts and hydrogen is carried out hydrofining reaction, hydrogenated oil is entered shape furfural extraction and obtain chaff essential oil; Chaff essential oil and hydrogen are carried out hydrodewaxing reaction; Hydrodewaxing is generated oil mix with carclazyte, crossed to filter by carclazyte and obtain clay-filtered oil, this clay-filtered oil is refrigerator oil base oil; Hydrobon catalyst active metal component is one in W, Ni, Co, Mo or its combination; Hydrodewaxing catalyst active metal component is one in Ni, Zn or its combination; Present method has widened refrigerator oil base oil raw material sources, produces the product meeting GB/T16630-1996 standard.
Description
Technical field
The present invention relates to the preparation method of refrigerator oil base oil, particularly utilize heavy hydrocarbon oil thermocracking process to produce a kind of preparation method of refrigerator oil base oil.
Background technology
Refrigerator oil is refrigeration compressor special lube, is the vital integral part determining and affect refrigerating function and effect in refrigeration system.High-quality refrigerator oil not only must possess thermochemical stability excellent when coexisting with refrigeration agent and intermiscibility, also must have excellent low-temperature fluidity, oilness, anti-bubble concurrently, and must be easy to produce, and raw material sources are reliable, do not pollute environment.Refrigerator oil generally comprises base oil and the various additive for improving other performance of refrigerator oil.The salient features of refrigerator oil is as rheological, viscosity temperature characteristic, low-temperature fluidity, flash-point and all determined by basic oil properties with the mutual solubility etc. of refrigeration agent.Therefore, the selection of refrigerator oil mainly concentrates in the selection of base oil.
The base oil of refrigerator oil can be divided into mineral oil origin and the large class of synthesis oil type two.The production of mineral oil origin refrigerator oil generally obtains base oil through techniques such as solvent treatment, solvent dewaxing, hydrogenation or clay finishings, then add multiple additives blending form.The base oil of compressor oil generally will account for more than 95% of processed oil, and therefore the quality good or not of base oil is directly connected to the quality level of compressor oil processed oil, and the quality of base oil has direct relation with its refining depth.The base oil that refining depth is dark, its heavy aromatics, gum level are just few.Carbon residue is low, and the susceptibility of oxidation inhibitor is all right, and the quality of base oil is just high, and its carbon deposit tendency in compressor assembly is little, and oil-water separativeness is good, and work-ing life is relatively just longer.The base oil of synthesis oil type is that the organic liquid base oil obtained with the method for chemosynthesis passes through the lubricating oil allocated or add multiple additives and make again.Its base oil major part is polymkeric substance or macromolecular organic compound.The kind of synthetic oil is a lot, and the synthetic oil as compressor oil mainly contains synthesis hydrocarbon (poly-1-olefin), organic ester (dibasic acid esters), polyalkylene glycol, fluorosilicon oil and phosphoric acid ester etc. 5 kinds.Synthetic oil has oxidation stability, and carbon deposit tendency is little, and the temperature range that can exceed plain mineral oil is lubricated, long service life, can meet the service requirements that general mineral oil origin compressor oil can not bear.But the cost ratio mineral oil origin compressor oil of synthesis oil type compressor oil is more expensive.
By inquiring about domestic patent, the patent relevant to refrigerator oil has following several sections:
(1) application number: 200780008494.6, " refrigerated machine oil composition ".The present invention relates to refrigerated machine oil composition, it is characterized in that containing the kinematic viscosity at 40 DEG C be 0.11 ~ 8mm
2the mixing base oil of/s, this mixing base oil contains: (A) is 5mm the kinematic viscosity of 40 DEG C
2the low viscosity base oil of/below s and (B) are 20 ~ 400mm the kinematic viscosity of 40 DEG C
2the high viscosity base oil of/s, (A) and (B) is the base oil containing at least one be selected from mineral oil, synthetic hydrocarbon compounds, oxygenatedchemicals and sulfocompound.
(2) application number: 01814730.5, " refrigerated machine oil composition ".Refrigerated machine oil composition of the present invention is containing having ester ring type ring and following general formula-COOR
1(in formula, R
1representing the alkyl of carbonatoms 1-30) 2 ester groups representing and this 2 ester groups are bonded to the refrigerated machine oil composition of the ester ring type di-carboxylic acid ester cpds on carbon atom that ester ring type ring adjoins each other, to improve its oilness, refrigeration property consistency, thermal hydrolysis stability and electrical insulating property is excellent, can also improve the efficiency of refrigeration system simultaneously.
(3) application number: 01814731.3, " refrigerated machine oil composition ".Refrigerated machine oil composition of the present invention, wherein containing the ester ring type multi-carboxylate compound using following compound (a)-(c) to obtain, when using together with natural series coolant such as HFC refrigeration agent and carbonic acid gas or hydrocarbon etc., can balance and good meet the over-all propertiess such as oilness, refrigeration agent consistency, thermal hydrolysis stability and electrical insulating property.
(4) application number: 97122040.9, " a kind of refrigerated machine oil composition ", discloses a kind of refrigerated machine oil composition, containing viscosity 10-150mm
2the C of the soft wax cracking of/s
5-C
18mixedαolefin stand oil, the conveniently alpha-olefin polymerization technique synthesis of this stand oil, adds additive and can produce the refrigerator oil fabulous with refrigeration agent HCFCS consistency
(5) application number: 200480043857.6, " refrigerator oil composition for carbon dioxide coolant ".The invention discloses a kind of refrigerator oil composition for carbon dioxide coolant, it can be used for the refrigeration system adopted under the supercritical state of carbon dioxide coolant, particularly can improve supercritical co by rate of heat exchange during heat exchanger, meanwhile, there is good weather resistance and oilness.
(6) application number: 200580007040.8, " refrigerator oil ".The feature of refrigerator oil of the present invention is to contain: nitrogen divides and is less than or equal to 50 quality ppm and the aromatic series mineral oil that divides (%CA) to be 5-25.Use refrigerator oil of the present invention, can high level and balancedly have stability, oilness and the consistency with refrigeration agent concurrently, can operate refrigerating and air conditioning device steadily in the long term.
(7) application number: 200710175413.3, " a kind of refrigerated machine oil composition and preparation method thereof ".This patent discloses a kind of refrigerated machine oil composition, mixedαolefin stand oil oily based on said composition contains and additive.
(8) application number: 200810223449.9, " production method of base oil of air-conditioner refrigeration oil ".The present invention relates to a kind of production method of base oil of air-conditioner refrigeration oil, with the raw material of the cut being greater than 360 DEG C in patent ZL 02104842.8 hydrogenated oil as hydrodewaxing, the generation oil of hydrodewaxing after atmospheric flashing, then carries out clay finishing; This base oil is with the mutual solubility of refrigeration agent freonll-11 is good, pour point, flock point are low, and sulphur nitrogen content is low, and meeting with freonll-11 is that the totally-enclosed air conditioner refrigerating compressor of refrigeration agent is to the requirement of refrigerator oil base oil.
For foreign patent, dominant query United States Patent (USP), the United States Patent (USP) related to mainly contains:
(1) patent No.: 4248726, a kind of high viscosity refrigerated machine oil composition.This full-bodied refrigerated machine oil composition comprises polyethylene or alkyl ether compound (A) and (B) and weight and accounts for the epoxy compounds of the Racemic glycidol ethers of A, B gross weight 0.1-10wt%, epoxy aliphatic ester and or epoxidised vegetables oil.
(2) patent No.: 4497721,4800030,5342533,6074573, refrigerated machine oil composition.The invention discloses a kind of refrigerated machine oil composition, at least containing a kind of mineral oil and a kind of synthetic oil or mixing oil, at least containing a kind of glycidyl compound or phosphide or ester class etc., this refrigerated machine oil composition shows very high stability when contacting with refrigerant containing halogen, effectively inhibit the generation of reacting hydrogenchloride with refrigerant containing halogen and and refrigeration agent have good consistency.Therefore this refrigerated machine oil composition has good lubricant effect.
(3) patent No.: US3953319A, proposes hydrofining-vitriolization-urea dewaxing-clay finishing refrigerator oil production method.
From above-mentioned disclosed technical literature scheme, the base oil component of refrigerator oil has two kinds: mineral oil and synthetic oil.And the performance of basic oil properties to refrigerator oil plays conclusive effect, by domestic and international contrastive analyze on patent, the in the majority of refrigerator oil is synthesized in research, but synthesis refrigerator oil cost is high, applies and is subject to certain restrictions.The application requiring of refrigerator oil and the good consistency of refrigeration agent, and under the operating mode of harshness, there is good lubricity and oxidation stability, and not with refrigeration agent generation chemical reaction.
Summary of the invention
The object of this invention is to provide a kind of with cycloalkyl heavy oil inferior or time processing cycloalkyl heavy oil for the preparation method of refrigerator oil base oil prepared by raw material.The method, to the strong adaptability of raw material, expands refrigerator oil base oil raw material sources, and the refrigerator oil base oil product prepared meets the standard of GB/T16630-1996.
Technical scheme provided by the invention is:
With naphthenic base crude inferior or time processing cycloalkyl heavy oil for raw material, an in-built dispersion inner member is entered from the bottom to top or without in the adiabatic reactor of inner member after process furnace heating, reactor reactant flow out, after quenching oil cooling, enters normal, vacuum fractionation tower fractionation and obtains refrigerator oil base oil feedstock fraction; This cut removes the heteroatomss such as S, N, O through hydrofining, and carries out olefin saturated and aromatic hydrogenation; Hydrofined oil removes many rings short-side chain aromatic hydrocarbon, sulfur-bearing in oil, containing oxygen, nitrogenous chemical combination and gum asphalt, obtains solvent-refined oil through solvent treatment; Solvent-refined oil, through hydrodewaxing, removes high pour point component; Hydrodewaxing reaction oil is through clay-filtered, and the clay-filtered oil obtained is exactly refrigerator oil base oil.
Specifically, technical scheme provided by the invention is: take density as 950Kg/m
3~ 1000Kg/m
3crude oil and long residuum, > 360 DEG C cycloalkyl long residuum be raw material, in-built dispersion inner member is entered or without in the adiabatic reactor of inner member after process furnace is heated to 360 ~ 480 DEG C, inner member is bubble deck, valve tray, traverse baffle or non-activity packing layer, control raw material 10 ~ 180 minutes residence time in the reactor, pressure 0.1 ~ 2.0MPa; Reactor reactant flow out cools through quenching oil, and quenching oil is that after cooling, thermally splitting generates oil, is cooled to 300 ~ 380 DEG C; Thermally splitting generates oil and cuts out 360 ~ 420 DEG C of cuts through fractionation; 360 ~ 420 DEG C of cuts are entered hydrofining reaction bed with hydrogen mixing post-heating to 250 DEG C ~ 400 DEG C, and controlling reaction bed temperature is 250 DEG C ~ 400 DEG C, and hydrogen dividing potential drop is 2.0 ~ 20MPa, and volume space velocity is 0.2 ~ 2.0h
-1, hydrogen to oil volume ratio 300: 1 ~ 1500: 1; The hydrogenated oil obtained from reactor enters in tower from solvent tower bottom, with enter tower furfural counter current contact from top and carry out heat and mass, operational condition is: solvent ratio 1.5 ~ 3.5: 1 (volume ratio), tower top temperature 85 ~ 115 DEG C, column bottom temperature 55 ~ 85 DEG C; Chaff essential oil is obtained through removing furfural from raffinating oil of flowing out of extracting tower top; Chaff essential oil enters hydrodewaxing reaction bed with hydrogen mixing post-heating to 200 DEG C ~ 350 DEG C, and controlling reaction bed temperature is 250 DEG C ~ 380 DEG C, and hydrogen dividing potential drop is 3.0 ~ 20MPa, and volume space velocity is 0.2 ~ 2.0h
-1, hydrogen to oil volume ratio 300: 1 ~ 1000: 1; Generate oil from reactor hydrodewaxing out to mix with carclazyte, be heated to 80 ~ 170 DEG C, carclazyte consumption is that hydrodewaxing generates 2 ~ 10% of oil quality, when mixing stops after 10-80 minute, crossed to filter by carclazyte and obtain clay-filtered oil, this clay-filtered oil is refrigerator oil base oil.
Or rather, technical scheme of the present invention is: with density at 950Kg/m
3~ 1000Kg/m
3crude oil and long residuum, > 360 DEG C of cycloalkyl long residuums be raw material, in-built dispersion inner member is entered or without in the adiabatic reactor of inner member after process furnace is heated to 390 DEG C ~ 430 DEG C, inner member can be bubble deck, valve tray and non-activity packing layer, control raw material 20 ~ 90 minutes residence time in the reactor, pressure 0.1 ~ 0.6MPa; Reactor reactant flow out cools through quenching oil, and quenching oil is that after cooling, thermally splitting generates oil, is cooled to 300 ~ 330 DEG C; Thermally splitting generates oil and cuts out 360 ~ 420 DEG C of cuts through fractionation; 360 ~ 420 DEG C of cuts are entered hydrofining reaction bed with hydrogen mixing post-heating to 280 DEG C ~ 350 DEG C, and controlling reaction bed temperature is 290 DEG C ~ 360 DEG C, and hydrogen dividing potential drop is 5.0 ~ 16MPa, and volume space velocity is 0.5 ~ 1.0h
-1, hydrogen to oil volume ratio 300: 1 ~ 800: 1; From reactor hydrogenated oil out through furfural solvent process for refining, operational condition is: solvent ratio 2.0 ~ 3.0: 1 (volume ratio), tower top temperature 95 ~ 105 DEG C, column bottom temperature 65 ~ 75 DEG C, raffinates oil to obtain chaff essential oil through removing furfural; Chaff essential oil enters hydrodewaxing reaction bed with hydrogen mixing post-heating to 270 DEG C ~ 350 DEG C, and controlling reaction bed temperature is 280 DEG C ~ 360 DEG C, and hydrogen dividing potential drop is 3.0 ~ 10MPa, and volume space velocity is 0.8 ~ 1.5h
-1, hydrogen to oil volume ratio 300: 1 ~ 500: 1; Hydrodewaxing generates oil and mixes with carclazyte, be heated to 110 ~ 150 DEG C, carclazyte consumption is that hydrodewaxing generates 3 ~ 6% of oil quality, mixes after residence time 30-50 minute, cross and filter carclazyte and obtain clay-filtered oil, this clay-filtered oil is refrigerator oil base oil.
The present invention uses catalyst for refining at hydrofining reaction bed, and the active metal component of catalyzer is one or two or more kinds combination in W, Ni, Co, Mo, and account for 10 ~ 40% of catalyst weight with oxide basis active metal component content, carrier is Al
2o
3or Al
2o
3-SiO
2sulfidizing is carried out before using; Use pour point depression catalyzer at hydrodewaxing reaction bed, the active metal component of catalyzer is one in Ni, Zn or its combination, accounts for 1 ~ 10% of catalyst weight with oxide basis active metallic content, and carrier is mordenite or ZSM-5 molecular sieve and Al
2o
3mixture, weight ratio is 1: 1, and can carry out sulfidizing before using also can without sulfidizing.
The invention solves refrigerator oil base oil the raw material sources single and resource Current Situation such as less, refrigerator oil base oil raw material sources are widened, with naphthenic base crude inferior or time processing cycloalkyl heavy oil for raw material, utilize thermally splitting-hydrofining-solvent treatment-hydrodewaxing-clay-filtered combination process, produce the refrigerator oil base oil product meeting GB/T16630-1996 standard.
Embodiment
Technical solution of the present invention and effect is set forth further below in conjunction with embodiment.
Embodiment 1
With cycloalkyl long residuum A for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst character is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 2
With naphthenic base crude B inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 3
With naphthenic base crude C inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 4
With naphthenic base crude D inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 5
With naphthenic base crude E inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 6
With cycloalkyl long residuum F inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 7
With cycloalkyl long residuum G inferior for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
Embodiment 8
With cycloalkyl long residuum G for raw material, feedstock property, in table 1, carries out thermocracking process, and thermocracking process operational condition is in table 2.Obtain refrigerator oil base oil raw material through cut cutting, this raw material obtains refrigerator oil base oil through hydrogenation, furfural, pour point depression and carclazyte production technique.Each production technique operating parameters is in table 3, table 4, table 5, table 6, and hydrogenation catalyst property analysis is in table 7.This base oil meets GB/T16630-1996 standard.
The analysis of table 1 feedstock property
Table 2 heat soaking operation parameter and property analysis
Table 3 hydrofining operational condition and property analysis
Table 4 furfural operational condition and chaff essential oil property analysis
Table 5 hydrodewaxing operational condition and pour point depression oil nature are analyzed
Table 6 carclazyte operational condition and white essential oil property analysis
The analysis of table 7 catalyst property
Claims (1)
1. a preparation method for refrigerator oil base oil, is characterized in that:
(1) take density as 950Kg/m
3~ 1000Kg/m
3, 100 DEG C of kinematic viscosity 200 ~ 1500mm
2the crude oil of/s, or the cycloalkyl long residuum of >360 DEG C is raw material, after process furnace is heated to 360 ~ 480 DEG C, enters in-built dispersion inner member or without in the adiabatic reactor of inner member, controls raw material 10 ~ 180 minutes residence time in the reactor, pressure 0.1 ~ 2.0MPa; Reactor reactant flow out cools through quenching oil, and quenching oil is that after cooling, thermally splitting generates oil, is cooled to 300 ~ 380 DEG C; Thermally splitting generates oil and cuts out 360 ~ 420 DEG C of cuts through fractionation;
(2) 360 ~ 420 DEG C of cuts are entered hydrofining reaction bed with hydrogen mixing post-heating to 250 DEG C ~ 400 DEG C, controlling reaction bed temperature is 250 DEG C ~ 400 DEG C, and hydrogen dividing potential drop is 2.0 ~ 20MPa, and volume space velocity is 0.2 ~ 2.0h
-1, hydrogen to oil volume ratio 300:1 ~ 1500:1;
(3) hydrogenated oil obtained from reactor enters in tower from solvent tower bottom, with enter tower furfural counter current contact from top and carry out heat and mass, operational condition is: solvent volume than 1.5 ~ 3.5:1, tower top temperature 85 ~ 115 DEG C, column bottom temperature 55 ~ 85 DEG C; Chaff essential oil is obtained through removing furfural from raffinating oil of flowing out of extracting tower top;
(4) chaff essential oil enters hydrodewaxing reaction bed with hydrogen mixing post-heating to 200 DEG C ~ 350 DEG C, and controlling reaction bed temperature is 250 DEG C ~ 380 DEG C, and hydrogen dividing potential drop is 3.0 ~ 20MPa, and volume space velocity is 0.2 ~ 2.0h
-1, hydrogen to oil volume ratio 300:1 ~ 1000:1;
(5) generate oil from reactor hydrodewaxing out to mix with carclazyte, be heated to 80 ~ 170 DEG C, carclazyte consumption is that hydrodewaxing generates 2 ~ 10% of oil quality, mixing stops after 10-80 minute, crossed to filter by carclazyte and obtain clay-filtered oil, this clay-filtered oil is refrigerator oil base oil;
Hydrofining reaction bed uses Hydrobon catalyst, and the active metal component of catalyzer is one in W, Ni, Co, Mo or its combination, and account for 10 ~ 40% of catalyst weight with oxide basis active metallic content, carrier is Al
2o
3-SiO
2, before using, carry out sulfidizing;
Hydrodewaxing reaction bed uses Hydrodewaxing catalyst, and the active metal component of catalyzer is one in Ni, Zn or its combination, accounts for 1 ~ 10% of catalyst weight with oxide basis active metallic content, and carrier is mordenite or ZSM-5 molecular sieve and Al
2o
3mixture.
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| CN104342206A (en) * | 2013-07-29 | 2015-02-11 | 山东鹏奥石油科技有限公司 | Lubricating oil hydrodewaxing production technology |
| CN109852459B (en) * | 2019-03-22 | 2021-06-01 | 合肥学院 | Synthetic method of ester lubricating oil containing molybdenum disulfide/spent clay compound lubricant dispersion system |
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Effective date of registration: 20180719 Address after: 100007 Dongzhimen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: PetroChina Karamay Petrochemical Co., Ltd. Patentee after: PetroChina Co.,Ltd. Address before: 100007 Oil Mansion, Oil Mansion, 9 Dongzhimen North Street, Dongcheng District, Beijing. Patentee before: PetroChina Co.,Ltd. |