CN109943382A - A kind of fine purification treatment process of lube base oil - Google Patents

A kind of fine purification treatment process of lube base oil Download PDF

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Publication number
CN109943382A
CN109943382A CN201910343664.0A CN201910343664A CN109943382A CN 109943382 A CN109943382 A CN 109943382A CN 201910343664 A CN201910343664 A CN 201910343664A CN 109943382 A CN109943382 A CN 109943382A
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China
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base oil
carrier
ester
loaded article
processing method
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CN201910343664.0A
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Chinese (zh)
Inventor
马楷
刘月皞
梅莉
李霞
魏智侠
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Priority to CN201910343664.0A priority Critical patent/CN109943382A/en
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Abstract

The present invention provides a kind of fine purification treatment process of lube base oil, comprising: after base oil is mixed and is heat-treated with solid processing agent, filters, obtains purification base oil;The base oil is esters base oil;The solid processing agent is support type inorganic agent, including carrier and loaded article;The carrier is selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite;The loaded article is compound containing metal alkaline;In the compound containing metal alkaline, metal is selected from one or more of Mg, K, Ca and Al.The present invention is using esters base oil as specific process object, it is handled using above-mentioned specific support type inorganic agent, the trace impurity substance in esters base oil can effectively be removed, hence it is evident that the antioxygenic property, electrical property and storage stability for promoting base oil extend its storage life.

Description

A kind of fine purification treatment process of lube base oil
Technical field
The present invention relates to technical field of lubricating oil, in particular to a kind of fine purification treatment process of lube base oil.
Background technique
In lubricating oil, base oil is main basis, the property of physicochemical property strong influence lubricating oil product oil Can, especially it is affected to the physicochemical property of the key such as the antioxygenic property of base oil, storage stability.And in base oil Micro substance, which often leads to base oil or even product oil, cannot better meet application demand, but be limited to current analytical technology, The type and difference of micro substance can not be analyzed and be distinguished well in base oil, also can not further find out micro substance pair The affecting laws of base oil performance and targetedly remove micro substance.
Currently, in view of the above-mentioned problems, being usually to carry out simple process or purification to base oil to mention to remove micro substance Rise base oil performance;For example, being handled using solid processing agent.But due to being limited to micro substance type in base oil And difference is difficult to analyze discrimination, targetedly solid processing agent can not be selected to be handled, it is usually irregular in the prior art Property using some inorganic agents with absorption property, but its treatment effect is not good enough.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of fine purification treatment process of lube base oil, according to this hair The processing method of bright offer can be obviously improved antioxygenic property, storage stability and the electrical property of base oil.
The present invention provides a kind of fine purification treatment process of lube base oil, comprising:
It after base oil is mixed and is heat-treated with solid processing agent, filters, obtains purification base oil;
The base oil is esters base oil;
The solid processing agent is support type inorganic agent, including carrier and loaded article;
The carrier is selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite;
The loaded article is compound containing metal alkaline;
In the compound containing metal alkaline, metal is selected from one or more of Mg, K, Ca and Al.
Preferably, the compound containing metal alkaline is selected from MgO, KOH, CaO and Al2O3One or more of.
Preferably, it is compound to be selected from atlapulgite base complex, silica gel base complex, active carbon base for the support type inorganic agent One or more of object and hydrotalcite compound;
In the atlapulgite base complex, carrier is atlapulgite, and loaded article is selected from one of MgO, KOH and CaO Or it is several;
In the silica gel base complex, carrier is silica gel, and loaded article is selected from one or more of MgO, KOH and CaO;
In the active carbon base complex, carrier is active carbon, and loaded article is selected from MgO, KOH, CaO and Al2O3One of Or it is several;
In the hydrotalcite compound, carrier is hydrotalcite, and loaded article is selected from MgO, KOH, CaO and Al2O3In one Kind is several.
Preferably, in the support type inorganic agent, the mass ratio of loaded article and carrier is 2%~5%.
Preferably, the esters base oil is selected from that trihydroxymethylpropanyl ester, that trihydroxymethylpropanyl ester answers ester, decanedioic acid two is different Monooctyl ester, decanedioic acid didecyl, decanedioic acid tridecanol ester, diisooctyl adipate, diisooctyl phthalate and pentaerythrite One or more of ester.
Preferably, the mass ratio of the solid processing agent and base oil is 0.1%~5%.
Preferably, the trihydroxymethylpropanyl ester is C7~C10 trihydroxymethylpropanyl ester.
Preferably, the mass ratio of the solid processing agent and base oil is 0.3%~0.6%.
Preferably, the temperature of the heat treatment is 60~100 DEG C.
Preferably, the temperature of the heat treatment is 70~90 DEG C.
The present invention provides a kind of fine purification treatment process of lube base oil, comprising: by base oil and solid processing agent It after mixing and heat treatment, filters, obtains purification base oil;The base oil is esters base oil;The solid processing agent is negative Load type inorganic agent, including carrier and loaded article;The carrier is selected from one of atlapulgite, silica gel, active carbon and hydrotalcite Or it is several;The loaded article is compound containing metal alkaline;In the compound containing metal alkaline, metal be selected from Mg, K, Ca and One or more of Al.The present invention is using esters base oil as specific process object, at above-mentioned specific support type Reason agent is handled, and can effectively remove the microscale harmful substance in esters base oil, hence it is evident that promote the inoxidizability of base oil Energy, electrical property and storage stability, extend its storage life.
Specific embodiment
The present invention provides a kind of fine purification treatment process of lube base oil, comprising:
It after base oil is mixed and is heat-treated with solid processing agent, filters, obtains purification base oil;
The base oil is esters base oil;
The solid processing agent is support type inorganic agent, including carrier and loaded article;
The carrier is selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite;
The loaded article is compound containing metal alkaline;
In the compound containing metal alkaline, metal is selected from one or more of Mg, K, Ca and Al.
In the present invention, the base oil is esters base oil.The esters base oil is preferably trihydroxymethylpropanyl ester, three Hydroxymethyl-propane ester answers ester, Plexol 201, decanedioic acid didecyl, decanedioic acid tridecanol ester, diisooctyl adipate, neighbour One or more of phthalic acid di-isooctyl and pentaerythritol ester.Wherein, the trihydroxymethylpropanyl ester be preferably C7~ One or more of C10 trihydroxymethylpropanyl ester.It is preferably C7~C10 trihydroxy methyl third that the trihydroxymethylpropanyl ester, which answers ester, One or more of alkane adipate ester.The pentaerythritol ester is monopentaerythritol ester and/or pentaerythritol fatty acid ester.The present invention Using above-mentioned synthetic ester lubricant as dealing with objects, it can preferably cooperate with above-mentioned solid processing agent, it is micro to effectively remove its Harmful substance promotes its performance.The present invention is not particularly limited the source of the esters base oil, for general commercially available product or presses It is made according to synthetic method well known to those skilled in the art.
In the present invention, the solid processing agent is support type inorganic agent, including carrier and loaded article.Wherein, the carrier Selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite;The loaded article is compound containing metal alkaline; In the compound containing metal alkaline, metal is selected from one or more of Mg, K, Ca and Al.In the present invention, the silica gel is Inorganic silica gel.It is limited to micro substance type and difference in base oil to be difficult to analyze discrimination, can not targetedly select at solid Reason agent and base oil are handled, can only irregularities exploration, and compared to other base oils, esters base oil is removed containing can not Outside the trace impurity of discrimination, usually also contain the remaining trace catalyst of synthesis process, due to common process agent polarity very Difficulty takes into account the trace impurity of multifrequency nature, and purification is relatively difficult, through applicants have found that, using above-mentioned specific load Type inorganic agent and above-mentioned specific ester base oil are arranged in pairs or groups, and the harmful components in esters base oil can be effectively removed, hence it is evident that are promoted Antioxygenic property, electrical property and storage stability of base oil etc..
In the present invention, preferably, the support type inorganic agent be selected from atlapulgite base complex, silica gel base complex, One or more of active carbon base complex and hydrotalcite compound.
In the atlapulgite base complex, carrier is atlapulgite, and loaded article is selected from MgO, KOH, CaO and Al2O3In One or more, more preferably one or more of MgO, KOH and CaO.
In the silica gel base complex, carrier is silica gel, and loaded article is selected from MgO, KOH, CaO and Al2O3One of or it is several Kind, more preferably one or more of MgO, KOH and CaO.
In the active carbon base complex, carrier is active carbon, and loaded article is selected from MgO, KOH, CaO and Al2O3One of Or it is several.
In the hydrotalcite compound, carrier is hydrotalcite, and loaded article is selected from MgO, KOH, CaO and Al2O3One of Or it is several.
Treatment effect can preferably be promoted using above-mentioned support type inorganic agent, make esters base oil antioxygenic property and Storage stability is further promoted.And it has been investigated that, in above-mentioned solid processing agent, for esters base oil performance (antioxidant, Storage stability and electrical property) promotion degree height, arrange it is as follows: active carbon base complex inorganic agent > atlapulgite base Compound inorganic agent > hydrotalcite compound inorganic agent > silica gel base complex inorganic agent.
In the present invention, the support type inorganic agent can be made in the following manner:
S1: using after metal salt solution impregnated carrier, compound precursor is obtained;
S2: the compound precursor is calcined, support type inorganic agent is obtained.
Wherein, in the step S1, the metal in the metal salt solution is selected from one of Mg, K, Ca and Al or several Kind.Specifically, the metal salt solution is one in magnesium nitrate solution, potassium nitrate solution, liquor alumini chloridi and calcium nitrate solution Kind is several.The carrier is selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite.The carrier comes Source is not particularly limited, and is general commercially available product.In the present invention, after mixing carrier with metal salt solution, preferably also add Enter KOH solution, carries out impregnation under the conditions of existing for the KOH solution;In the KOH solution dosage of KOH preferably with it is above-mentioned Metal salt equimolar amounts.It after carrier is mixed with metal salt solution and KOH solution, is preferably stirred, mixes all materials.It is mixed After even, filtering, and washed with clear water, until obtaining compound precursor without metal potassium element in solution.
In the step S2, the temperature of the calcining is preferably 300~550 DEG C, and the time of calcining is preferably 400~ 540min.After calcining, support type inorganic agent is obtained.
Specifically, by taking atlapulgite base complex inorganic agent as an example, in some embodiments of the invention, preparation method It is as follows: to use equi-volume impregnating, activity will be added in magnesium nitrate solution/potassium nitrate solution/liquor alumini chloridi/calcium nitrate solution Carclazyte (metal salt and atlapulgite mass ratio be preferably 2%~5%), then be slowly added dropwise KOH solution (mass concentration 10%, KOH dosage and above-mentioned metal salt equimolar amounts), stir 60min under 200rpm, filter, clear water washs 3 times, into solution without gold Belong to potassium element;Take filter cake to be placed in Muffle furnace, 9h calcined at 300~550 DEG C, respectively obtain MgO- atlapulgite inorganic agent, KOH- atlapulgite inorganic agent, CaO- atlapulgite inorganic agent, Al2O3Atlapulgite inorganic agent.When carrier is other materials, It is carried out also according to above-mentioned preparation method, atlapulgite is replaced with into other carriers.
In the present invention, in the support type inorganic agent, the mass ratio of loaded article and carrier is preferably 2%~5%.
In the present invention, the mass ratio of the solid processing agent and base oil is preferably 0.1%~5%, and more preferably 0.3% ~0.6%.
The present invention is not particularly limited the mode for mixing base oil with solid processing agent, according to those skilled in the art Well known mixing method mixes material, such as can carry out mixing by stirring.
In the present invention, the temperature of the heat treatment is preferably 60~100 DEG C, if temperature is lower than 60 DEG C, cannot effectively be removed Esters base oil harmful components cannot preferably promote base oil performance, if temperature is higher than 100 DEG C, in esters base of the invention Under the mixed system environment of plinth oil and solid processing agent, it is easy to cause metallic element in solid processing agent to fall off, remains on basis In oil, its performance is influenced.The heat treatment temperature is more preferably 70~90 DEG C, most preferably 75 DEG C.The time of the heat treatment Preferably 30min~2h.
In the present invention, the filter membrane used that filters is preferably specification for the filter membrane no more than 10 μm.After filtering, Obtain purification base oil.
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention Limitation.In following embodiment, solid processing agent is obtained according to preparation method as described in the above technical scheme.
Embodiment 1
The MgO- silica gel treatment (load capacity 3%) of addition 0.5% into diisooctyl phthalate, after mixing, It is heat-treated 1h at 75 DEG C, filters, obtains purification base oil.
Embodiment 2
The MgO- hydrotalcite inorganic agent (load capacity 3%) of addition 0.5% into diisooctyl phthalate, mixes Afterwards, it is heat-treated 1h at 75 DEG C, filters, obtains purification base oil.
Embodiment 3
The MgO- atlapulgite inorganic agent (load capacity 3%) of addition 0.5% into diisooctyl phthalate, mixes Afterwards, it is heat-treated 1h at 75 DEG C, filters, obtains purification base oil.
Embodiment 4
The MgO- active carbon inorganic agent (load capacity 3%) of addition 0.5% into diisooctyl phthalate, mixes Afterwards, it is heat-treated 1h at 75 DEG C, filters, obtains purification base oil.
Comparative example 1
It is carried out according to the preparation process of embodiment 1, unlike, it is added without solid processing agent.
Embodiment 5
Examples 1 to 4 and 1 gained base oil of comparative example are tested for the property, test antioxygenic property, storage respectively surely Qualitative and electrical property.Wherein, the test of antioxygenic property is referring to SH/T 0450,180 DEG C, for 24 hours, 50mL air/min condition After lower processing, the rate of change in viscosity (%) and acid value variation (mgKOH/g) of oil product are tested.The test of storage stability are as follows: 24 DEG C Half a year, 1 year and 2 years are stored respectively, test the acid value variation (mgKOH/g) of oil product.The test of electrical property is referring to GB/T5654- 2007.Test result is referring to table 1:
The performance test results of table 1 Examples 1 to 4 and comparative example 1
It can be seen from 1 test result of table compared with comparative example 1, the antioxygenic property of the embodiment of the present invention 1~4, storage Stability and electrical property are obviously improved, it was demonstrated that, compared with original basis oil, using processing method of the invention, can significantly it mention Rise antioxygenic property, storage stability and the electrical property of base oil.In Examples 1 to 4, according to the height of resultant performance enhancements degree Low arrangement, it is as follows: 4 > embodiment of embodiment, 3 > embodiment, 2 > embodiment 1, it was demonstrated that, the place of active carbon base complex inorganic agent Manage the treatment effect > silicon of the treatment effect > hydrotalcite compound inorganic agent of effect > atlapulgite base complex inorganic agent The treatment effect of matrix compound inorganic agent.
Embodiment 6
The KOH- active carbon inorganic agent (load capacity 3%) of addition 0.5% into decanedioic acid didecyl, after mixing, in 75 It is heat-treated 1h at DEG C, filters, obtains purification base oil.
Embodiment 7
The KOH- active carbon inorganic agent (load capacity 3%) of addition 0.5% into diisooctyl adipate, after mixing, in It is heat-treated 1h at 75 DEG C, filters, obtains purification base oil.
Embodiment 8
To the KOH- active carbon inorganic agent of addition 0.5% in trihydroxymethylpropanyl ester (trihydroxymethylpropanyl ester of C7~10) (load capacity 3%) after mixing, is heat-treated 1h at 75 DEG C, filtering, obtains purification base oil.
Embodiment 9
The KOH- active carbon inorganic agent (load capacity 3%) of addition 0.5% into dioctyl sebacate, after mixing, in 75 It is heat-treated 1h at DEG C, filters, obtains purification base oil.
Embodiment 10
(1) one is tested
According to the test method of embodiment 5 respectively to esters base oil decanedioic acid didecyl, diisooctyl adipate, three hydroxyls Methyl-prop alkyl ester, dioctyl sebacate are tested for the property, as a result referring to table 2:
The performance test results of 2 esters base oil of table
Decanedioic acid didecyl, diisooctyl adipate, trihydroxymethylpropanyl ester, the last of the ten Heavenly stems two it can be seen from 2 test result of table The antioxygenic property of dioctyl phthalate, storage stability and electrical property are poor.
(2) two are tested
6~9 gained base oil of embodiment is tested for the property according to the test method of embodiment 5, as a result referring to table 3:
The performance test results of 3 embodiment 6~9 of table
3 test result of table is compared with table 2 can be seen that each embodiment in table 3 compared with the original basis oil in table 2 Antioxygenic property, storage stability and electrical property are obviously improved;It proves, compared with original basis oil, using processing of the invention After method processing, antioxygenic property, storage stability and the electrical property of various base oils can be obviously improved.
Used herein a specific example illustrates the principle and implementation of the invention, and above embodiments are said It is bright to be merely used to help understand method and its core concept of the invention, including best mode, and but also this field is appointed What technical staff can practice the present invention, including any device or system of manufacture and use, and implement the method for any combination. It should be pointed out that for those skilled in the art, it without departing from the principle of the present invention, can also be right Some improvement and modification can also be carried out by the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.This hair The range of bright patent protection is defined by the claims, and may include those skilled in the art it is conceivable that other implementations Example.If these other embodiments, which have, is similar to the structural element of claim character express, or if they include with Equivalent structural elements of the character express of claim without essence difference, are wanted then these other embodiments should also be included in right In the range of asking.

Claims (10)

1. a kind of fine purification treatment process of lube base oil characterized by comprising
It after base oil is mixed and is heat-treated with solid processing agent, filters, obtains purification base oil;
The base oil is esters base oil;
The solid processing agent is support type inorganic agent, including carrier and loaded article;
The carrier is selected from one or more of atlapulgite, silica gel, active carbon and hydrotalcite;
The loaded article is compound containing metal alkaline;
In the compound containing metal alkaline, metal is selected from one or more of Mg, K, Ca and Al.
2. processing method according to claim 1, which is characterized in that the compound containing metal alkaline be selected from MgO, KOH, CaO and Al2O3One or more of.
3. processing method according to claim 1 or 2, which is characterized in that the support type inorganic agent is selected from atlapulgite One or more of base complex, silica gel base complex, active carbon base complex and hydrotalcite compound;
In the atlapulgite base complex, carrier is atlapulgite, and loaded article is selected from one of MgO, KOH and CaO or several Kind;
In the silica gel base complex, carrier is silica gel, and loaded article is selected from one or more of MgO, KOH and CaO;
In the active carbon base complex, carrier is active carbon, and loaded article is selected from MgO, KOH, CaO and Al2O3One of or it is several Kind;
In the hydrotalcite compound, carrier is hydrotalcite, and loaded article is selected from MgO, KOH, CaO and Al2O3One of or It is several.
4. processing method according to claim 1, which is characterized in that in the support type inorganic agent, loaded article and carrier Mass ratio be 2%~5%.
5. processing method according to claim 1, which is characterized in that the esters base oil is selected from trimethylolpropane It is different pungent that ester, trihydroxymethylpropanyl ester answer ester, Plexol 201, decanedioic acid didecyl, decanedioic acid tridecanol ester, adipic acid two One or more of ester, diisooctyl phthalate and pentaerythritol ester.
6. processing method according to claim 1, which is characterized in that the mass ratio of the solid processing agent and base oil is 0.1%~5%.
7. processing method according to claim 5, which is characterized in that the trihydroxymethylpropanyl ester is tri- hydroxyl of C7~C10 Methyl-prop alkyl ester.
8. processing method according to claim 1 or 6, which is characterized in that the quality of the solid processing agent and base oil Than being 0.3%~0.6%.
9. processing method according to claim 1, which is characterized in that the temperature of the heat treatment is 60~100 DEG C.
10. processing method according to claim 9, which is characterized in that the temperature of the heat treatment is 70~90 DEG C.
CN201910343664.0A 2019-04-26 2019-04-26 A kind of fine purification treatment process of lube base oil Pending CN109943382A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113073000A (en) * 2021-03-08 2021-07-06 安徽中天石化股份有限公司 Method for improving performance of phosphate flame-retardant hydraulic oil

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CN106631782A (en) * 2016-10-17 2017-05-10 中国石油化工股份有限公司 Preparation method of pentaerythritol tetrabasic acid ester

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Publication number Priority date Publication date Assignee Title
CN101899355A (en) * 2009-05-27 2010-12-01 中国石油化工股份有限公司 Lubricating oil composite with oxidation resistance and preparation method thereof
CN102887825A (en) * 2012-09-04 2013-01-23 陕西省石油化工研究设计院 Method for preparing polyol ester lubricating oil by using composite solid acid catalyst
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