CN108017566B - Purification method of lubricating oil additive mixed solution - Google Patents
Purification method of lubricating oil additive mixed solution Download PDFInfo
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- CN108017566B CN108017566B CN201610967011.6A CN201610967011A CN108017566B CN 108017566 B CN108017566 B CN 108017566B CN 201610967011 A CN201610967011 A CN 201610967011A CN 108017566 B CN108017566 B CN 108017566B
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- mixed solution
- lubricating oil
- oil additive
- additive mixed
- purification method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/18—Esters of dithiocarbamic acids
- C07C333/20—Esters of dithiocarbamic acids having nitrogen atoms of dithiocarbamate groups bound to hydrogen atoms or to acyclic carbon atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the field of fine chemical engineering, and relates to a novel purification process of a mixed solution of a lubricating oil additive. The water content in the mixed solution of the lubricating oil additive can be reduced to below 50ppm, the NaCl content can be reduced to below 10ppm, and the pH value is neutral through ceramic membrane filtration equipment.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, and relates to a novel purification process of a mixed solution of a lubricating oil additive.
Background
It is known that oil products inevitably contact with oxygen in air and metal surfaces during use to undergo oxidation reaction and deteriorate, so that the viscosity of the oil products is increased, the acid value is increased, sludge and precipitate are generated, and corrosion and abrasion are caused to metal parts. The antioxidant is added into the oil product, so that the oxidation reaction can be effectively inhibited, the service life of the oil product is prolonged, and the service performance of the oil product is improved. The dialkyl dithiocarbamate is used in oil products, has outstanding oxidation resistance, good abrasion resistance and extreme pressure performance, has the characteristics of good oil solubility, no ash and the like, and is widely applied to various oil products such as turbine oil, hydraulic oil, gear oil, internal combustion engine oil and the like and lubricating grease.
Chinese patent application CN2013104658627 describes a continuous synthesis method of dialkyl dithiocarbamate in a tubular reactor: setting the temperature of a micro-tube type reactor, pumping mixed solution of di-n-butylamine and sodium hydroxide into a micro-channel reactor through a constant flow pump after the temperature is stable, simultaneously pumping mixed solution of di-fluidized carbon and dichloromethane into the micro-channel, reacting materials in the micro-channel, discharging the materials into a four-mouth flask with a condenser pipe and stirring, keeping the temperature, raising the temperature to react for 0.5 hour, and separating the liquid. To obtain a dialkyl dithiocarbamate mixture with a water content of more than 0.9%, a pH of 11, and a certain amount of NaCl.
The prior art adopts water washing or filtration after distillation. In chinese patent CN1132813C, a toluene extraction organic phase desalting process or a water washing process is proposed; chinese patent CN1159294C proposes a process of adding solvent gasoline for extraction, separating NaCl and then distilling to remove water. The old process is either carried with solvent to be treated or is a water washing distillation process. The ceramic membrane filtration equipment is adopted, free water and NaCl in the mixed solution can be removed at one time, the operation is convenient, and the effect is good.
Disclosure of Invention
The technical problem to be solved by the invention is to solve the technical problems of the prior art of dehydration, desalination and NaOH removal of the mixed solution of the lubricating oil additive, the process is simple to operate, the water content in the mixed solution can be treated to be below 50ppm, the NaCl content is treated to be below 10ppm, the pH is neutral, and the process has obvious advantages compared with the prior art.
The technical scheme of the invention is as follows: the purification method of the mixed liquid of the lubricating oil additive is characterized in that the mixed liquid of the lubricating oil additive is heated to increase the fluidity of the mixed liquid, the mixed liquid is pumped into ceramic membrane filtration equipment by a pump, the pressure in a channel of the equipment is kept, and the liquid is discharged and collected after being circulated in the equipment to obtain the purified lubricating oil additive.
Generally, the method comprises the steps of heating the mixed solution to a certain temperature, namely 70-90 ℃, pumping the mixed solution into ceramic membrane filtering equipment for circulating filtration by using a pump, controlling the flow rate of the pump to ensure that the pressure in the filtering equipment is not higher than 1MPa, circulating the mixed solution in the filter for 0.1-2 hours, and receiving the filtered clear solution for later use. The method is easy to operate, rapid, low in labor intensity and high in safety.
The lubricating oil additive disclosed by the invention comprises the following components: dialkyl dithiocarbamates.
In the invention, ceramic membrane filtration equipment is used for removing water, NaCl and NaOH in the mixed liquid of the lubricating oil additive.
The invention has the beneficial effects that: the water content in the mixed solution of the lubricating oil additive can be reduced to below 50ppm, the NaCl content can be reduced to below 10ppm, and the pH value is neutral through ceramic membrane filtration equipment.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to these examples.
Example 1
Maintaining the temperature of the mixed solution at 80 ℃, pumping the mixed solution into ceramic membrane filtering equipment by a pump, adjusting the flow rate to maintain the pressure in a filtering system to be about 0.2MPa, circulating the liquid in the filter for 1.5 hours, and collecting filtrate. The filtrate was clear, with a water content of 40ppm, a pH of about 7, and no NaCl was detected.
Example 2
Heating the mixed solution to 90 ℃, pumping into a filtering device, adjusting the pump speed to maintain the pressure in the filtering system to be about 0.7MPa, circulating the liquid in the filter for 0.2 hour, and collecting the filtrate. The filtrate was clear, with a water content of 50ppm, a pH of approximately 7, and no NaCl was detected.
Example 3
Heating the mixed solution to 70 ℃, pumping into a filtering device, adjusting the speed of a pump to maintain the pressure in the filtering system to be about 1MPa, circulating the liquid in the filter for 2 hours, and collecting the filtrate. The filtrate was clear, with a water content of 50ppm, a pH of approximately 7, and no NaCl was detected.
Comparative example
The conventional mixed liquid water and salt removing process comprises the following steps: adding 500ml of deionized water into the mixed solution, stirring and maintaining for 5min, separating, and repeating the operation for three times, wherein the pH value of the organic phase is approximately equal to 7. The water is removed by distillation under reduced pressure, and the water content is reduced to 80 ppm. The mixture was cloudy after the distillation treatment. After heating to 80 ℃ it was filtered using a G4 sand core funnel and the filtrate collected. The filtrate is transparent, and salt is precipitated on the surface of the sand core of the funnel.
Compared with the conventional purification process, the operation steps of the purification treatment process of the mixed solution by using the ceramic membrane filtration equipment are far less than those of the conventional treatment process, the amount of waste water is greatly reduced, and the water removal treatment effect is better than that of a distillation treatment mode.
Claims (1)
1. A purification method of a lubricating oil additive mixed solution is characterized in that the heating temperature of the lubricating oil additive mixed solution is maintained at 70-90 ℃ to increase the fluidity of the lubricating oil additive mixed solution, the lubricating oil additive mixed solution is pumped into ceramic membrane filtration equipment by a pump, the pressure in a channel of the equipment is kept to be not higher than 1MPa, and the liquid is discharged and collected after circulating in the equipment for 0.1-2 hours to obtain the purified lubricating oil additive; the lubricating oil additive is a dialkyl dithiocarbamate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610967011.6A CN108017566B (en) | 2016-10-28 | 2016-10-28 | Purification method of lubricating oil additive mixed solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610967011.6A CN108017566B (en) | 2016-10-28 | 2016-10-28 | Purification method of lubricating oil additive mixed solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108017566A CN108017566A (en) | 2018-05-11 |
| CN108017566B true CN108017566B (en) | 2020-06-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201610967011.6A Active CN108017566B (en) | 2016-10-28 | 2016-10-28 | Purification method of lubricating oil additive mixed solution |
Country Status (1)
| Country | Link |
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| CN (1) | CN108017566B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364759A (en) * | 2001-01-18 | 2002-08-21 | 中国石油化工股份有限公司 | preparation of dialkyl dithio amino formate |
| CN105968362A (en) * | 2016-07-25 | 2016-09-28 | 江苏久吾高科技股份有限公司 | Purifying method and device for hydroxyl silicone oil |
-
2016
- 2016-10-28 CN CN201610967011.6A patent/CN108017566B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1364759A (en) * | 2001-01-18 | 2002-08-21 | 中国石油化工股份有限公司 | preparation of dialkyl dithio amino formate |
| CN105968362A (en) * | 2016-07-25 | 2016-09-28 | 江苏久吾高科技股份有限公司 | Purifying method and device for hydroxyl silicone oil |
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| Publication number | Publication date |
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| CN108017566A (en) | 2018-05-11 |
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Address after: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee after: China Petroleum & Chemical Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: China Petroleum & Chemical Corp. Patentee before: Nanhua Group Research Institute |