CN103666603A - Environment friendly low-sulfur diesel antiwear agent - Google Patents
Environment friendly low-sulfur diesel antiwear agent Download PDFInfo
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- CN103666603A CN103666603A CN201310723776.1A CN201310723776A CN103666603A CN 103666603 A CN103666603 A CN 103666603A CN 201310723776 A CN201310723776 A CN 201310723776A CN 103666603 A CN103666603 A CN 103666603A
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- butyl oleate
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Abstract
An environment friendly low-sulfur diesel antiwear agent is prepared from butyl oleate and 100SN, and the mass ratio of the butyl oleate to the 100SN is (85-90) to (10-15); the preparation method of the environment friendly low-sulfur diesel antiwear agent is as follows: preparation of butyl oleate: adding oleic acid and butanol into a reaction kettle, then adding solvent oil and a catalyst in sequence for esterification reaction, stirring and rising the temperature to 140 to 150 DEG C, removing water for 2 to 4 hours under a backflow state, neutralizing generated materials and removing an acid catalyst after the esterification reaction, and finally carrying out distillation at reduced pressure so as to enable the materials to be dewatered to obtain the butyl oleate, wherein the mass ratio of the oleic acid, to the butanol, to the catalyst, namely toluenesulfonic acid, and to the miscella is (26-29) to (7-9) to (1-2) to (9-13); composition: adding the butyl oleate into the reaction kettle, rising the temperature to 100 DEG C, keeping the temperature for 1 hour, separating away water, then cooling to 65 to 70 DEG C, adding the 100SN and stirring uniformly, so as to obtain the diesel antiwear agent. The mass ratio of the butyl oleate to the 100SN is (85-90) to (10-15).
Description
Technical field
The invention belongs to a kind of diesel-dope, be specifically related to a kind of environment-friendly type low-sulfur diesel-oil anti-wear agent.
Background technology
In recent years, state of enforcement's four diesel quality standards (GB252-2011 ordinary diesel oil standard).State's four emission standards are national fourth stage motor vehicle emission standards, automotive emissions mainly contain HC (hydrocarbon polymer), NOx (nitrogen oxygenate), CO (carbon monoxide), PM (particulate) etc., active coating by better catalytic converter, air injection reaction and with the application of the technology such as exhaust gas recycling system of refrigerating unit, control and reduce automotive emissions and reach below standard specified value.Owing to carrying out above-mentioned standard, require sulphur content lower than 150 μ g/g, and sulfocompound is natural lubricant, once diesel oil is after sulfocompound is taken off in hydrofining, its oilness is also lost thereupon, during diesel motor operation, there will be wearing and tearing, oil accident occurs when serious.Therefore, in state's four diesel quality standards, newly increased the requirement of an oilness quality, with wear scar diameter, weighed.Diesel oil through hydrofining sulphur content lower than 150 μ g/g, wear scar diameter is between 500～800 μ m, and sulphur content is lower, and wear scar diameter is larger.In order to make the oilness of diesel oil reach requirement, must add diesel antiwear additive.Add diesel antiwear additive, require wear scar diameter to be less than 460 μ m.
Summary of the invention
The object of the invention is to solve the problem that prior art exists; a kind of environment-friendly type low-sulfur diesel-oil anti-wear agent is provided; using and change that alone oleic acid was too high as acid number that diesel antiwear additive is caused in the past; and cause the problem of wear scar diameter, filter net jam; reduce the discharge of objectionable impurities; protection of the environment, improves again diesel fuel lubricity, reaches the oilness quality requirement of state's four diesel quality standard regulations.
Technical scheme of the present invention is: a kind of environment-friendly type low-sulfur diesel-oil anti-wear agent, by butyl oleate and 100SN, formed, and its two mass ratio is (85～90): (10～15); The compound method of this environment-friendly type low-sulfur diesel-oil anti-wear agent is: by above-mentioned mass ratio, butyl oleate is added in reactor, be warming up to 100 ℃, keep 1h that water is isolated, be then cooled to 65～70 ℃, the 100SN that adds fromula ratio, stirs and obtains environment-friendly type low-sulfur diesel-oil anti-wear agent.
The preparation method of diesel antiwear additive described above, is comprised of following process and step:
1) preparation of butyl oleate: vegetable oil acid and butanols are added in reactor, add successively again solvent oil, catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with in sodium hydroxide and generate material and remove an acidic catalyst, last underpressure distillation makes material dewatering obtain butyl oleate; Wherein, the mass ratio of oleic acid, butanols, catalyzer toluenesulphonic acids, solvent oil toluene is (26～29): (7～9): (1～2): (9～1).Catalyzer: sodium hydroxide=1:(4.7～5.0).
2) composite: butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that water is separated, be then cooled to 65～70 ℃, add gasoline 100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent; Wherein, the mass ratio of oleic oil acid butyl ester and 100SN is (85～90): (10～15).
Above-mentioned 100SN, SN refers to " solvent treatment neutral base oil ", the kinematic viscosity 100cSt (centistoke) when numeral is above 40 ℃ of base oils.
The present invention compared with prior art has outstanding substantive distinguishing features and marked improvement and positively effect: the diesel antiwear additive that the present invention makes is lubricated, compares with commercial like product, has significant effect.The present invention be take vegetable oil acid and is prepared environment-friendly type low-sulfur diesel-oil anti-wear agent as raw material, has changed that alone oleic acid was too high as acid number that diesel antiwear additive causes in the past, and causes that mill spot radius exceeds standard, the problem of filter net jam; Obviously reduce discharge, the protection of the environment of objectionable impurities, can greatly improve diesel fuel lubricity again, see following attached table 1.
Before table 1. environment-friendly type low-sulfur diesel-oil anti-wear agent adds, add rear mill spot radius contrast table
From upper table 1, diesel fuel lubricity of the present invention is obvious, and wear scar diameter is all significantly less than 460 μ m.
Embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
A kind of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 26Kg vegetable oil acid and 7Kg butanols are added in reactor, add successively again 9Kg solvent oil toluene, 1Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～the 4h that dewaters under reflux state, after esterification finishes, with in 5Kg sodium hydroxide and generate material, to remove an acidic catalyst, last underpressure distillation makes material dewatering obtain butyl oleate.
2) composite: first 85Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 10Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.
Embodiment 2
A kind of preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 26Kg vegetable oil acid and 8Kg butanols are added in reactor, add successively again 10Kg solvent oil toluene, 1.5Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with removing an acidic catalyst with generation material in 7Kg sodium hydroxide, last underpressure distillation makes material dewatering obtain low sulfur oil acid butyl ester.
2) composite: first 90Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 10Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.
Embodiment 3
A kind of preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 27Kg vegetable oil acid and 7Kg butanols are added in reactor, add successively the more oily toluene of the molten profit of 9Kg, 1Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with removing an acidic catalyst with generation material in 5Kg sodium hydroxide, last underpressure distillation makes material dewatering obtain low sulfur oil acid butyl ester.
2) composite: first 85Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 15Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.
Embodiment 4
A kind of preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 27Kg vegetable oil acid and 8Kg butanols are added in reactor, add successively again 11Kg solvent oil toluene, 1.5Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with removing an acidic catalyst with generation material in 10Kg sodium hydroxide, last underpressure distillation makes material dewatering obtain low sulfur oil acid butyl ester.
2) composite: first 90Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 15Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.
Embodiment 5
A kind of preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 28Kg vegetable oil acid and 8Kg butanols are added in reactor, add successively again 11Kg solvent oil toluene, 1Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with removing an acidic catalyst with generation material in 7Kg sodium hydroxide, last underpressure distillation makes material dewatering obtain low sulfur oil acid butyl ester;
2) composite: first 90Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 15Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.
Embodiment 6
A kind of preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent, by following process and step, formed: the 1) preparation of butyl oleate: 29Kg vegetable oil acid and 9Kg butanols are added in reactor, add successively again 12Kg solvent oil toluene, 2Kg catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with removing an acidic catalyst with generation material in 10Kg sodium hydroxide, last underpressure distillation makes material dewatering obtain low sulfur oil acid butyl ester.
2) composite: first 90Kg butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that moisture is removed, be then cooled to 65～70 ℃, add 15Kg100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent.The raw materials used specification of environment-friendly type low-sulfur diesel-oil anti-wear agent of the present invention is as follows.
Claims (2)
1. an environment-friendly type low-sulfur diesel-oil anti-wear agent, is comprised of butyl oleate and 100SN, and its two mass ratio is 85～90:10～15; The compound method of the anti-anti-wear agent of this environment-friendly type low-sulfur diesel-oil is: by above-mentioned mass ratio, butyl oleate is added in reactor, be warming up to 100 ℃, keep 1h that moisture is gone out, be then cooled to 65～70 ℃, the 100SN that adds fromula ratio, stirs and obtains environment-friendly type low-sulfur diesel-oil anti-wear agent.
2. the preparation method of environment-friendly type low-sulfur diesel-oil anti-wear agent as claimed in claim 1, is comprised of following process and step:
1) preparation of butyl oleate: oleic acid and butanols are added to reactor, add successively again solvent oil, catalyzer to carry out esterification, stirring is warming up to 140～150 ℃, 2～4h dewaters under reflux state, after esterification finishes, with in sodium hydroxide and generate material and remove an acidic catalyst, last underpressure distillation makes material dewatering obtain butyl oleate; Wherein, the mass ratio of oleic acid, butanols, catalyzer toluenesulphonic acids, solvent oil toluene is (26～29): (7～9): (1～2): (9～13); Catalyzer: sodium hydroxide=1:(4.7～5.0);
2) composite: butyl oleate to be added to reactor, be warming up to 100 ℃, keep 1h that water is separated, be then cooled to 65～70 ℃, add gasoline 100SN, stir and obtain environment-friendly type low-sulfur diesel-oil anti-wear agent; Wherein, the mass ratio of oleic oil acid butyl ester and 100SN is (85～90): (10～15).
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| CN201310723776.1A CN103666603A (en) | 2013-12-19 | 2013-12-19 | Environment friendly low-sulfur diesel antiwear agent |
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| CN201310723776.1A CN103666603A (en) | 2013-12-19 | 2013-12-19 | Environment friendly low-sulfur diesel antiwear agent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593104A (en) * | 2014-03-31 | 2015-05-06 | 江苏创新石化有限公司 | Fatty acid ester diesel fuel anti-wear agent preparation method |
| CN106520218A (en) * | 2016-10-29 | 2017-03-22 | 骆公予 | Ecological fuel oil and preparation method thereof |
| WO2021134602A1 (en) * | 2019-12-31 | 2021-07-08 | 中国石油化工股份有限公司 | Low sulfur diesel blockage inhibitor, preparation method therefor and use thereof |
| CN113121336A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Compound, clogging inhibitor, preparation method of compound, clogging-inhibiting low-sulfur diesel oil and method for improving clogging-inhibiting performance of low-sulfur diesel oil |
-
2013
- 2013-12-19 CN CN201310723776.1A patent/CN103666603A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593104A (en) * | 2014-03-31 | 2015-05-06 | 江苏创新石化有限公司 | Fatty acid ester diesel fuel anti-wear agent preparation method |
| CN106520218A (en) * | 2016-10-29 | 2017-03-22 | 骆公予 | Ecological fuel oil and preparation method thereof |
| CN106520218B (en) * | 2016-10-29 | 2018-06-08 | 骆公予 | Ecological fuel oil and preparation method thereof |
| WO2021134602A1 (en) * | 2019-12-31 | 2021-07-08 | 中国石油化工股份有限公司 | Low sulfur diesel blockage inhibitor, preparation method therefor and use thereof |
| CN113121336A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Compound, clogging inhibitor, preparation method of compound, clogging-inhibiting low-sulfur diesel oil and method for improving clogging-inhibiting performance of low-sulfur diesel oil |
| CN113121336B (en) * | 2019-12-31 | 2022-08-12 | 中国石油化工股份有限公司 | Compound, clogging inhibitor, preparation method of compound, clogging-inhibiting low-sulfur diesel oil and method for improving clogging-inhibiting performance of low-sulfur diesel oil |
| JP2023509413A (en) * | 2019-12-31 | 2023-03-08 | 中国石油化工股▲ふん▼有限公司 | Low-sulphur diesel fouling inhibitor, method of manufacture and use thereof |
| US11912657B2 (en) | 2019-12-31 | 2024-02-27 | China Petroleum & Chemical Corporation | Low sulfur diesel blockage inhibitor, preparation method therefor and use thereof |
| JP7494304B2 (en) | 2019-12-31 | 2024-06-03 | 中国石油化工股▲ふん▼有限公司 | Anti-clogging agent for low sulfur diesel, its manufacturing method and use |
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