CN1683479A - Process for preparing lubricating oil extreme pressure wear resistant additive - Google Patents

Process for preparing lubricating oil extreme pressure wear resistant additive Download PDF

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Publication number
CN1683479A
CN1683479A CN 200410031185 CN200410031185A CN1683479A CN 1683479 A CN1683479 A CN 1683479A CN 200410031185 CN200410031185 CN 200410031185 CN 200410031185 A CN200410031185 A CN 200410031185A CN 1683479 A CN1683479 A CN 1683479A
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oil
described preparation
reaction
lubricating oil
intermediate product
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CN 200410031185
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CN100338199C (en
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徐风华
韦淡平
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

The preparation process of lubricating oil extreme pressure wear resistant additive includes the following steps: 1) reaction between silicon tetrachloride and C2-C16 fatty amine in the molar ratio of 1 to 4-10 in the presence of non-polar solvent at 0-100 deg.c and 0.01-0.1 MPa to obtain the intermediate product; and 2) mixing the intermediate product in 100 weight portions with lubricant oil dispersant in 10 weight portions, non-ionic surfactant in 1-10 weight portions and lubricant oil base oil in 20-70 weight portions and reaction at 50-180 deg.c and 0.01-0.1 MPa. The prepared additive has excellent extreme pressure wear resistant effect and excellent dispersivity and stability in lubricant oil.

Description

The preparation method of lubrication oil anti-wear extreme pressure additive
Technical field
The present invention relates to a kind of lubricating oil additive, definite says, is the preparation method of lubrication oil anti-wear extreme pressure additive.
Background technology
Past, the research of adopting nanotechnology to improve the lubricating oil extreme pressure anti-wear obtained tangible progress for over ten years.From kind, can be divided into Inorganic Nanometer Antiwear Agents, the organic and inorganic matrix material anti-wear agent of finishing, and ashless nano antiwear agent.The general ultra-fine grain that adopts various physics and chemical process to prepare metal, metal oxide, metallic sulfide etc. of Inorganic Nanometer Antiwear Agents, and then they are distributed in the base oil as additive go.Many metal oxides such as Lithium Oxide 98min, zirconium white, titanium oxide and silicon oxide etc., very high fusing point and hardness are arranged itself, it is the presoma of preparation pottery, be used for the anti-caking power that lubricating oil can significantly improve lubricating oil, and the nanometer superfine powder body of preparation can not resemble the problem that has easy oxidation the metal powder.Introduced the good result that nano size rare earth hydroxide has obtained as lubricating oil additive among the CN1218103A; CN1346873A then introduces the method for utilizing friction to form ceramic structure in the metallic surface; US6,243,669 have introduced the natural crystal that will contain multiple metal oxide handles the nanometer state, adds after the specific catalyst as lubricating oil additive again, but does not introduce anti-wear effect in detail.
The nano-metal-oxide or the metal hydroxides of method for preparing are used for lubricating oil, the solid-liquid separation phenomenon can occur after depositing certain hour, cause losing lubricant effect, and extreme pressure anti-wear are not good, P BUsually have only 300~600N, limited its application in lubricating oil.
Summary of the invention
The invention provides a kind of preparation method of lubrication oil anti-wear extreme pressure additive, prepared additive has excellent extreme-pressure anti-wear effect, and good dispersiveness and stable is arranged in lubricating oil.
Put it briefly, preparation process lubricant oil additive provided by the invention comprises:
1) in the presence of solvent, silicon tetrachloride and aliphatic amide at 0~100 ℃, are reacted under the condition of 0.01~0.1MPa, obtain intermediate product;
2) intermediate product is mixed with lubricating oil dispersant, emulsifying agent and lubricant base, stirring reaction under 50 ℃~180 ℃, 0.01~0.1MPa, become translucent thickness state up to product, wherein, weight in intermediate product is 100%, the consumption of dispersion agent, nonionogenic tenside and base oil is respectively 1~10%, and 1~10%, 20~70%.
Specifically, lubricating oil additive provided by the invention can prepare in accordance with the following methods:
1) silicon tetrachloride being dissolved in the non-polar solvent, under agitation adding the C2-C16 aliphatic amide, is 0~100 ℃ in temperature, preferred 25~70 ℃, pressure is 0.01~0.1MPa, reacts under the condition of preferred 0.05~0.08MPa 1~8 hour, preferred 2~4 hours, obtain intermediate product.Wherein, the mol ratio of silicon tetrachloride and aliphatic amide is 1: 4~1: 10, preferred 1: 5~1: 8.The consumption of solvent is 5~30 times of silicon tetrachloride weight, preferred 10~25 times.
2) lubricating oil dispersant, nonionogenic tenside and lubricant base are mixed with intermediate product, at 50 ℃~180 ℃, preferred 75~150 ℃ were stirred 0.5~6 hour down, preferred 1~4 hour, reaction pressure 0.01~0.1MPa, preferred 0.05~0.08MPa obtains the additive of translucent thickness state.Wherein, be 100% in the weight of intermediate product, dispersant dosage is 1~10%, preferred 2~6%; The nonionogenic tenside consumption is 1~10%, preferred 2~6%; The consumption of base oil is 20~70%, preferred 30~50%.
Said C2-C16 aliphatic amide is the C2-C16 alkylamine, preferred ethylamine, n-butylamine, n-hexyl amine, dodecyl amine; Or polyamines polyene, as diethylenetriamine, triethylene tetramine etc.It also can be one or more mixture wherein.
Said solvent is a non-polar solvent, preferred benzene,toluene,xylene, hexanaphthene, sherwood oil or their mixture.
Said lubricating oil dispersant is allyl butyrate imide, petroleum sodium sulfonate, calcium mahogany sulfonate or their mixture.
Said nonionogenic tenside is as emulsifying agent, and the single, double fatty acid ester of preferably glycerine is as the single, double fatty acid ester of the glycerine of citric acid, succsinic acid, lactic acid; The Sorbitol Powder fatty acid ester is as sorbityl monododecanoate, Sorbitol Powder monopalmitate, sorbitol monooleate; And the polyvinyl chloride ether of Sorbitol Powder fatty acid ester,, polyvinyl chloride (20) Sorbitol Powder monostearate sorbityl monododecanoate etc. as polyvinyl chloride (20).
Said base oil is mineral oil, ucon oil, vegetables oil or their mixture.40 ℃ of viscosity of its mineral oil in fluid, ucon oil, vegetables oil are 5~50mm 2/ s, preferred 10~30mm 2/ s, ucon oil are ester class oil, polyethers, alkylbenzene, synthetic hydrocarbon or their mixture.Vegetables oil is Oleum Gossypii semen, rapeseed oil, peanut oil or their mixture.
In order to remove the hydrogenchloride that dereaction produces, can also carry out underpressure distillation or in reaction product, add acidic substance trapping agent such as epoxy soybean oil or amido vinyl ether reaction product.
The lubrication oil anti-wear extreme pressure additive of the inventive method preparation can be applicable in mineral oil, synthetic oil or the plant wet goods lubricating oil, has excellent extreme-pressure anti-wear effect, and good dispersiveness and stable is arranged in lubricating oil.
Embodiment
Example 1
The 2.43g silicon tetrachloride is dissolved in the 35.58g benzene, under stirring, reducing pressure, adds the 8.6g di-n-butyl amine, under reduced pressure stir 2 hours (Heating temperature is 25 ℃, pressure 0.05MPa) again after adding finishes; (40 ℃ of viscosity are 22mm with 30g mineral oil 2/ s), the single succimide of hanging of sorbityl monododecanoate, the 2g of 1g mixes with above-mentioned substance, heated and stirred 4 hours (Heating temperature is 75 ℃, pressure 0.05MPa) reduces pressure; Add epoxy soybean oil 0.5g, get product A after stirring, the dosage of product A with 5w% is joined in the whiteruss, measure its supporting capacity, the results are shown in Table 1 by the GB3142-82 method.
Example 2
The 3.15g silicon tetrachloride is dissolved in the 38.63g sherwood oil, under stirring, normal pressure, adds the 13.5g triethylene tetramine, under normal pressure, stir 4 hours (Heating temperature is 45 ℃) after adding finishes again; (40 ℃ of viscosity are 25.3mm with the 38g Oleum Gossypii semen 2/ s), the single succimide of hanging of 2g Sorbitol Powder monopalmitate, 2g mixes with above-mentioned substance, normal pressure heated and stirred 5 hours (Heating temperature is 150 ℃), add amido vinyl ether 1g, get product B after stirring, the dosage of product B with 5w% is joined in the whiteruss, measure its supporting capacity by the GB3142-82 method, the results are shown in Table 1.
Example 3
The 4.23g silicon tetrachloride is dissolved in the 55.36g toluene, under stirring, normal pressure, adds 17.83g dodecyl amine, under normal pressure, stir 3.5 hours (Heating temperature is 30 ℃) after adding finishes again; (40 ℃ of viscosity are 20.6mm with the 38.7g rapeseed oil 2/ s), the polyvinyl chloride ether of 2g Sorbitol Powder fatty acid ester, the single succimide of hanging of 2g mixes with above-mentioned substance, normal pressure heated and stirred 5 hours (Heating temperature is 101 ℃), add amido vinyl ether 1g, get products C after stirring, the dosage of products C with 5w% is joined in the whiteruss, measure its supporting capacity by the GB3142-82 method, the results are shown in Table 1.
Comparative Examples
Press the embodiment 1 preparation nano size rare earth hydroxide additive of CN1218103A, the dosage of this additive with 5w% is joined in the whiteruss, measure its supporting capacity, the results are shown in Table 1 by the GB3142-82 method.
Table 1
Sequence number Oil sample ????P B/N ????P D/N Stability
????1 Whiteruss P ????372 ????1235 ????/
????2 The P+5w% product A ????980 ????1960 12 months
????3 The P+5w% product B ????1078 ????1960 12 months
The P+5w% products C ????1078 ????1960 12 months
????4 P+5w% Comparative Examples product ????882 ????/ ????/
1. refer to that system does not produce layering and immovable time of character

Claims (12)

1. the preparation method of lubrication oil anti-wear extreme pressure additive comprises:
1) in the presence of non-polar solvent, silicon tetrachloride and C2-C16 aliphatic amide at 0~100 ℃, are reacted under the condition of 0.01~0.1MPa, obtain intermediate product, wherein, the mol ratio of silicon tetrachloride and aliphatic amide is 1: 4~1: 10;
2) intermediate product is mixed with lubricating oil dispersant, nonionogenic tenside and lubricant base, stirring reaction under 50 ℃~180 ℃, 0.01~0.1MPa, become translucent thickness state up to product, wherein, weight in intermediate product is 100%, the consumption of dispersion agent, nonionogenic tenside and base oil is respectively 1~10%, and 1~10%, 20~70%.
2. according to the described preparation method of claim 1, it is characterized in that the reaction conditions of step 1) is: 25~70 ℃ of temperature of reaction, pressure 0.05~0.08MPa, 1~8 hour reaction times,
3. according to the described preparation method of claim 1, it is characterized in that in the step 1), the mol ratio of silicon tetrachloride and aliphatic amide is 1: 5~1: 8.
4. according to the described preparation method of claim 1, it is characterized in that step 2) reaction conditions be: 75~150 ℃ of temperature of reaction, reaction pressure 0.05~0.08MPa.
5. according to the described preparation method of claim 1, it is characterized in that step 2) in, be 100% in the weight of intermediate product, dispersant dosage is 2~6%, nonionogenic tenside consumption 2~6%, the consumption 30~50% of base oil.
6. according to the described preparation method of claim 1, it is characterized in that said C2-C16 aliphatic amide is selected from ethylamine, following butylamine, n-hexyl amine, dodecyl amine, diethylenetriamine, triethylene tetramine or their mixture.
7. according to the described preparation method of claim 1, it is characterized in that said solvent is selected from benzene,toluene,xylene, hexanaphthene, sherwood oil or their mixture.
8. according to the described preparation method of claim 1, it is characterized in that said lubricating oil dispersant is allyl butyrate imide, petroleum sodium sulfonate, calcium mahogany sulfonate or their mixture.
9. according to the described preparation method of claim 1, it is characterized in that said nonionogenic tenside is selected from the single, double fatty acid ester of glycerine, the fatty acid ester of Sorbitol Powder, the polyvinyl chloride ether of Sorbitol Powder fatty acid ester.
According to the described preparation method of claim 1, it is characterized in that 10, said lubricant base is mineral oil, ucon oil, vegetables oil or their mixture.
11. according to the described preparation method of claim 1, it is characterized in that, after reaction finishes, reaction product carried out underpressure distillation or add the acidic substance trapping agent in reaction product removing the hydrogenchloride that dereaction produces.
12., it is characterized in that said acidic substance trapping agent is epoxy soybean oil or amido vinyl ether according to the described preparation method of claim 11.
CNB2004100311859A 2004-04-14 2004-04-14 Process for preparing lubricating oil extreme pressure wear resistant additive Expired - Lifetime CN100338199C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100389184C (en) * 2005-08-31 2008-05-21 中国石油化工股份有限公司 Hot-rolled oil composition containing organosilicon antiwear slip-proofing agent
US7867960B2 (en) 2006-08-31 2011-01-11 Cherron Oronite Company LLC Method for forming tetraoxy-silane derived antiwear films and lubricating oil compositions therefrom
US8067346B2 (en) 2006-08-31 2011-11-29 Chevron Oronite Company Llc Tetraoxy-silane lubricating oil compositions
US8153566B2 (en) 2008-09-30 2012-04-10 Cherron Oronite Company LLC Lubricating oil compositions

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4663392A (en) * 1986-05-16 1987-05-05 Amoco Corporation Process for preparation of Mannich reaction products from oxidized polymers
CN1044918C (en) * 1996-04-05 1999-09-01 中国石化兰州炼油化工总厂 Preparation method for lubricating oil additive
CN1191342C (en) * 2001-10-30 2005-03-02 中国石油化工股份有限公司 Compsn. of rust inhibiting lubricant special for chain

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100389184C (en) * 2005-08-31 2008-05-21 中国石油化工股份有限公司 Hot-rolled oil composition containing organosilicon antiwear slip-proofing agent
US7867960B2 (en) 2006-08-31 2011-01-11 Cherron Oronite Company LLC Method for forming tetraoxy-silane derived antiwear films and lubricating oil compositions therefrom
US8067346B2 (en) 2006-08-31 2011-11-29 Chevron Oronite Company Llc Tetraoxy-silane lubricating oil compositions
US8153566B2 (en) 2008-09-30 2012-04-10 Cherron Oronite Company LLC Lubricating oil compositions

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