CN107011997B - Fatty acid type diesel antiwear agent and preparation method thereof - Google Patents
Fatty acid type diesel antiwear agent and preparation method thereof Download PDFInfo
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- CN107011997B CN107011997B CN201710428029.3A CN201710428029A CN107011997B CN 107011997 B CN107011997 B CN 107011997B CN 201710428029 A CN201710428029 A CN 201710428029A CN 107011997 B CN107011997 B CN 107011997B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/10—Liquid carbonaceous fuels containing additives
- C10L1/14—Organic compounds
- C10L1/18—Organic compounds containing oxygen
- C10L1/188—Carboxylic acids; metal salts thereof
- C10L1/1881—Carboxylic acids; metal salts thereof carboxylic group attached to an aliphatic carbon atom
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/08—Use of additives to fuels or fires for particular purposes for improving lubricity; for reducing wear
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0083—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils with addition of auxiliary substances, e.g. cristallisation promotors, filter aids, melting point depressors
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/005—Splitting up mixtures of fatty acids into their constituents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
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Abstract
The invention relates to a fatty acid type diesel antiwear agent and a preparation method thereof, and the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator; washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent. The invention has no waste gas, waste water and waste residue in the production process, and has the characteristics of simple operation, short process flow, energy saving, environmental protection, high product yield, good quality and the like.
Description
Technical Field
The invention relates to a diesel oil antiwear agent, in particular to a fatty acid type diesel oil antiwear agent and a preparation method thereof.
Background
At present, the preparation process of the fatty acid type antiwear agent mainly comprises a molecular distillation method, a freeze-squeezing method, a solvent freeze-separation method and the like. The molecular distillation method is to separate saturated fatty acid and unsaturated fatty acid in crude fatty acid by multi-stage molecular distillation under the condition of high vacuum, and because the physical properties of each component in the crude fatty acid have small difference, the yield and the quality of the antiwear agent product obtained by separation by the molecular distillation method are not fully satisfactory; the freezing and squeezing method is to directly freeze the crude fatty acid into paste and then squeeze the paste to obtain unsaturated fatty acid, and the method has the advantages of difficult realization of continuous production, lower production efficiency, higher energy consumption and large labor amount; the solvent freezing separation method is to directly freeze a mixed solution of crude fatty acid and an organic solvent into paste, and then obtain unsaturated fatty acid through centrifugal separation.
Therefore, the existing preparation processes of various fatty acid type antiwear agents have defects, and the economic benefit in actual production is poor.
Disclosure of Invention
The invention aims to provide a fatty acid type diesel antiwear agent and a preparation method thereof, which have the advantages of simpler operation, higher product yield, no discharge of waste gas, waste liquid, waste residue and the like, energy conservation and environmental protection.
The technical scheme adopted by the invention is as follows:
the preparation method of the fatty acid type diesel antiwear agent is characterized by comprising the following steps:
the method comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator;
step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent.
In the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct.
The crude fatty acid in the step one is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
In the first step, the emulsifier is an aqueous solution containing 3-7% of a surfactant and 1-5% of an electrolyte;
the surfactant is alkyl benzene sulfonate, alkyl sulfonate or fatty acid sulfate;
the electrolyte is sodium sulfate, magnesium sulfate or sodium chloride.
In the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is respectively 10-15 ℃ and 0-5 ℃, the amount of the emulsifier used in each emulsifying process is 5-15% of the mass of the crude fatty acid, and the crude fatty acid is stirred and emulsified for 15-30 min under the condition of constant temperature.
And in the second step, washing the crude fatty acid clear liquid with water at 60-65 ℃ for 2 times, then carrying out oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the product, namely the fatty acid type diesel antiwear agent.
Adding 30-60% of water by mass into the emulsified solid, heating to 80 ℃, stirring at a constant temperature for 20-30 min to perform demulsification, and finally performing oil-water separation to obtain a byproduct, namely saturated fatty acid.
The fatty acid type diesel oil antiwear agent is prepared by the preparation method of the fatty acid type diesel oil antiwear agent.
The invention has the following advantages:
1. in the invention, after the crude fatty acid is emulsified, the saturated fatty acid is easier to separate out and separate, the unsaturated fatty acid content in the emulsified solid is lower, the yield of the product is improved to more than 80 percent, the saturated fatty acid content in the obtained antiwear agent product is lower than 2 percent, and the condensation point and the cloud point are respectively lower than minus 9 ℃ and minus 13 ℃.
2. In the invention, the emulsified crude fatty acid solution is separated by adopting a butterfly centrifugal separator, the equipment has the most important characteristics that the crude oil acid clear solution, the emulsified solid and water in the emulsion can be separated at one time, the separation effect is better, the whole feeding and discharging process is a continuous mode, the process has certain automatic control technology, the production efficiency is high, the labor amount of workers is reduced, and the labor intensity is reduced.
3. In the invention, the separated emulsifier and water can be recycled, so that the method is energy-saving and environment-friendly and has better economical efficiency.
4. In the invention, the purity of the saturated fatty acid obtained by demulsifying the separated emulsified solid is relatively high, and the emulsified solid can be used for preparing soap or other related products of the company.
5. The preparation process disclosed by the invention has the characteristics of no waste gas, waste water and waste residues in the production process, simplicity in operation, short process flow, energy conservation, environmental friendliness and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The invention relates to a preparation method of a fatty acid type diesel antiwear agent, which comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator; the crude fatty acid is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
The emulsified mixed liquid is separated by a butterfly centrifuge, the centrifuge can efficiently divide the mixed liquid into three phases, and the separated mixed liquid is divided into a crude fatty acid clear liquid, emulsified solid and water. The feeding and discharging of the butterfly centrifuge are both continuous operations, and the operations are remote automatic control.
Step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent.
In the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct. The specific process is as follows: adding 30-60% of water by mass into the emulsified solid, heating to 80 ℃, stirring at a constant temperature for 20-30 min to perform demulsification, and finally performing oil-water separation to obtain a byproduct, namely saturated fatty acid.
In the first step, the emulsifier is an aqueous solution containing 3-7% of a surfactant and 1-5% of an electrolyte; the surfactant is alkyl benzene sulfonate, alkyl sulfonate or fatty acid sulfate; the electrolyte is sodium sulfate, magnesium sulfate or sodium chloride. The surfactant and electrolyte must be selected so that they do not chemically react.
In the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is respectively 10-15 ℃ and 0-5 ℃, the amount of the emulsifier used in each emulsifying process is 5-15% of the mass of the crude fatty acid, and the crude fatty acid is stirred and emulsified for 15-30 min under the condition of constant temperature.
And in the second step, washing the crude fatty acid clear liquid with water at 60-65 ℃ for 2 times, then carrying out oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the product, namely the fatty acid type diesel antiwear agent.
And (4) recycling the centrifugal water and the washing water in all the steps as water for preparing the emulsifier, and continuously recycling the water after demulsification for demulsification. The oil-water separation devices respectively take out oil and water after standing and layering.
Example 1:
the preparation method of the fatty acid type diesel antiwear agent comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator; the crude fatty acid is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
The emulsified mixed liquid is separated by a butterfly centrifuge, the centrifuge can efficiently divide the mixed liquid into three phases, and the separated mixed liquid is divided into a crude fatty acid clear liquid, emulsified solid and water. The feeding and discharging of the butterfly centrifuge are both continuous operations, and the operations are remote automatic control.
Step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent.
In the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct. The specific process is as follows: adding 30% water into the emulsified solid, heating to 80 deg.C, stirring at constant temperature for 30min to demulsify, and performing oil-water separation to obtain saturated fatty acid as byproduct.
In the first step, the emulsifier is an aqueous solution containing 3% of surfactant and 5% of electrolyte; the surfactant is alkyl benzene sulfonate; the electrolyte is sodium sulfate. The surfactant and electrolyte must be selected so that they do not chemically react.
In the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is respectively 10 ℃ and 5 ℃, the amount of the emulsifier used in each emulsifying process is 5 percent of the mass of the crude fatty acid, and the crude fatty acid is stirred and emulsified for 30min under the condition of constant temperature.
In the second step, the crude fatty acid clear liquid is washed for 2 times by 60 ℃ water, then oil-water separation is carried out, and then the water content is reduced to be below 0.03 percent by thin film distillation, so that the obtained product is the fatty acid type diesel antiwear agent.
Example 2:
the preparation method of the fatty acid type diesel antiwear agent comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator; the crude fatty acid is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
The emulsified mixed liquid is separated by a butterfly centrifuge, the centrifuge can efficiently divide the mixed liquid into three phases, and the separated mixed liquid is divided into a crude fatty acid clear liquid, emulsified solid and water. The feeding and discharging of the butterfly centrifuge are both continuous operations, and the operations are remote automatic control.
Step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent.
In the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct. The specific process is as follows: adding water with the mass of 60% into the emulsified solid, heating to 80 ℃, stirring at constant temperature for 20min for demulsification, and finally performing oil-water separation to obtain a byproduct, namely saturated fatty acid.
In the first step, the emulsifier is an aqueous solution containing 7% of surfactant and 1% of electrolyte; the surfactant is alkyl sulfonate; the electrolyte is magnesium sulfate. The surfactant and electrolyte must be selected so that they do not chemically react.
In the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is 15 ℃ and 0 ℃, the amount of the emulsifier used in each emulsifying process is 15% of the mass of the crude fatty acid, and the crude fatty acid is stirred and emulsified for 15min under the condition of constant temperature.
In the second step, the crude fatty acid clear liquid is washed for 2 times by using 65 ℃ water and then subjected to oil-water separation, and then the water content is reduced to be below 0.03 percent by using thin film distillation, so that the obtained product is the fatty acid type diesel antiwear agent.
Example 3:
the preparation method of the fatty acid type diesel antiwear agent comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator; the crude fatty acid is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
The emulsified mixed liquid is separated by a butterfly centrifuge, the centrifuge can efficiently divide the mixed liquid into three phases, and the separated mixed liquid is divided into a crude fatty acid clear liquid, emulsified solid and water. The feeding and discharging of the butterfly centrifuge are both continuous operations, and the operations are remote automatic control.
Step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the fatty acid type diesel antiwear agent.
In the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct. The specific process is as follows: adding water with the mass of 45% into the emulsified solid, heating to 80 ℃, stirring at constant temperature for 25min for demulsification, and finally performing oil-water separation to obtain a byproduct, namely saturated fatty acid.
In the first step, the emulsifier is an aqueous solution containing 5% of surfactant and 3% of electrolyte; the surfactant is fatty acid sulfate; the electrolyte is sodium chloride. The surfactant and electrolyte must be selected so that they do not chemically react.
In the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is respectively 12 ℃ and 2 ℃, the amount of the emulsifier used in each emulsification is 10 percent of the mass of the crude fatty acid, and the emulsification is stirred for 22min under the constant temperature condition.
In the second step, the crude fatty acid clear liquid is washed for 2 times by 62 ℃ water and then subjected to oil-water separation, and then the water content is reduced to below 0.03 percent by thin film distillation, so that the obtained product is the fatty acid type diesel antiwear agent.
In the invention, after the crude fatty acid is emulsified, the saturated fatty acid is easier to separate out and separate, the unsaturated fatty acid content in the emulsified solid is lower, the yield of the product is improved to more than 80 percent, the saturated fatty acid content in the obtained antiwear agent product is lower than 2 percent, and the condensation point and the cloud point are respectively lower than minus 9 ℃ and minus 13 ℃.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (6)
1. The preparation method of the fatty acid type diesel antiwear agent is characterized by comprising the following steps:
the method comprises the following steps:
the method comprises the following steps: emulsifying the crude fatty acid by using an emulsifier, and separating the emulsified crude fatty acid into a crude fatty acid clear liquid, an emulsified solid and water by using a butterfly separator;
step two: washing the crude fatty acid clear solution with hot water, performing oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain a fatty acid type diesel antiwear agent;
in the first step, the emulsifier is an aqueous solution containing 3-7% of a surfactant and 1-5% of an electrolyte;
the surfactant is alkyl benzene sulfonate, alkyl sulfonate or fatty acid sulfate;
the electrolyte is sodium sulfate, magnesium sulfate or sodium chloride;
in the first step, the crude fatty acid is emulsified twice, the emulsifying temperature of the two times is respectively 10-15 ℃ and 0-5 ℃, the amount of the emulsifier used in each emulsifying process is 5-15% of the mass of the crude fatty acid, and the crude fatty acid is stirred and emulsified for 15-30 min under the condition of constant temperature.
2. The method for preparing the fatty acid type diesel antiwear agent according to claim 1, characterized in that:
in the first step, the emulsified solid is demulsified by hot water and then subjected to oil-water separation to obtain a saturated fatty acid byproduct.
3. The method for preparing the fatty acid type diesel antiwear agent according to claim 1, characterized in that:
the crude fatty acid in the step one is obtained by preheating to completely dissolve the solid in the crude fatty acid and then slowly cooling and crystallizing.
4. The method for preparing the fatty acid type diesel antiwear agent according to claim 1, characterized in that:
and in the second step, washing the crude fatty acid clear liquid with water at 60-65 ℃ for 2 times, then carrying out oil-water separation, and then reducing the water content to below 0.03% by using thin film distillation to obtain the product, namely the fatty acid type diesel antiwear agent.
5. The method for preparing the fatty acid type diesel antiwear agent according to claim 2, characterized in that:
adding 30-60% of water by mass into the emulsified solid, heating to 80 ℃, stirring at a constant temperature for 20-30 min to perform demulsification, and finally performing oil-water separation to obtain a byproduct, namely saturated fatty acid.
6. The fatty acid type diesel antiwear agent prepared by the method for preparing the fatty acid type diesel antiwear agent according to claim 1.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4204481A (en) * | 1979-02-02 | 1980-05-27 | Ethyl Corporation | Anti-wear additives in diesel fuels |
| CN104130809A (en) * | 2014-08-19 | 2014-11-05 | 安庆市中创生物工程有限公司 | Diesel oil anti-wear agent and preparation method thereof |
| CN106350217A (en) * | 2016-11-01 | 2017-01-25 | 中海油天津化工研究设计院有限公司 | Preparation method of low-cloud-point fatty acid type diesel antiwear additive |
| CN206051965U (en) * | 2016-09-05 | 2017-03-29 | 西安万德能源化学股份有限公司 | A kind of process units of fatty acid type diesel antiwear additive |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4204481A (en) * | 1979-02-02 | 1980-05-27 | Ethyl Corporation | Anti-wear additives in diesel fuels |
| CN104130809A (en) * | 2014-08-19 | 2014-11-05 | 安庆市中创生物工程有限公司 | Diesel oil anti-wear agent and preparation method thereof |
| CN206051965U (en) * | 2016-09-05 | 2017-03-29 | 西安万德能源化学股份有限公司 | A kind of process units of fatty acid type diesel antiwear additive |
| CN106350217A (en) * | 2016-11-01 | 2017-01-25 | 中海油天津化工研究设计院有限公司 | Preparation method of low-cloud-point fatty acid type diesel antiwear additive |
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