CN106146368A - A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive - Google Patents
A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive Download PDFInfo
- Publication number
- CN106146368A CN106146368A CN201510136349.2A CN201510136349A CN106146368A CN 106146368 A CN106146368 A CN 106146368A CN 201510136349 A CN201510136349 A CN 201510136349A CN 106146368 A CN106146368 A CN 106146368A
- Authority
- CN
- China
- Prior art keywords
- castor oil
- sulfur
- nitrogen
- bearing
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Lubricants (AREA)
Abstract
The present invention relates to a kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive, comprise the following steps: in flask, add Oleum Ricini and alkaline solution, fully separate upper strata organic solvent after reaction, it is washed, after vacuum dehydration, add diethanolamine to react, after the organic solvent of separating-purifying upper strata, obtain nitrogenous modified castor oil；S is dropwise instilled in the there-necked flask of nitrogenous modified castor oil2Cl2, after fully reacting, add NH4Sx, add reduced iron powder, after being centrifuged separating, use accurate filter paper that the supernatant is filtered, obtain amber sulfur-bearing, nitrogen castor oil-base lubricating additive.The present invention provides a kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive, solves the technical problem that lubricating additive cannot be degraded, preparation cost is high, synthesis path is complicated.
Description
Technical field
The present invention relates to the preparation method of additive, in particular, the present invention relates to be applied to a kind of sulfur-bearing of lubricant preparation field, the preparation method of nitrogen castor oil-base green lubrication additive.
Background technology
Lubricating additive, is directed in lubricant add one or more compounds, so that it obtains the characteristic that certain is new.The effect of additive is to improve the existing performance of base oil and increase new performance.
Base oil most content of wax comparison of ingredients that industry distillation produces is high, it is directly produced out I. C. engine oil with this crude oil and adds in locomotive fuel tank, condensation point is higher, temperature is than relatively low area in the winter time, wax is easy to crystallization at low temperatures, and then cause oil product solidification not flowed, cause motor vehicle starting difficulty, therefore must add the additive reducing condensation point.
Comparing humid region, moisture in air and oxygen at rainy, weather can enter in machine oil, consequent bubble makes oil product pressure transient, and bubble is easy to lack of lubrication in oil product and causes sintering, the most also must be added to the additive of anti-bubble.And water and oil the most easily form emulsion, causing oil product mobility to be deteriorated, this needs to add anti emulsifier.
Some oil product uses for a long time in humid air, easily causes corrosion, and oil product have to eliminate rust, and this will add rust-inhibiting additive.Oil product is also easy to ingress of air in storing and using and causes oxidation, and some oil product also requires that certain shelf life, and this is to be accomplished by adding oxidation and corrosion inhibitor, these all have to add, otherwise oil product lost efficacy with regard to as easy as rolling off a log corruption, and service life is the shortest, causes the waste of resource.
The preparation method of conventional mineral oil additive is mainly followed the most both at home and abroad in the preparation of green lubrication additive, i.e. by research lubricant on the basis of the rules such as the absorption of surface of friction pair, tribochemistry behavior, screen some nontoxic or low toxicities and be prone to adsorb at frictional interface and friction chemical reaction occurs, generate shear strength is low, extreme pressure property is good adsorbed film or the functional element of friction chemical reaction film or group, carry out " group assembling ", synthesizing green lubrication additive nontoxic, biodegradable, additive preparation cost is high, synthesis path is complicated.
Summary of the invention
It is an advantage of the invention to provide a kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive, solve the technical problem that lubricating additive cannot be degraded, preparation cost is high, synthesis path is complicated.
The above-mentioned purpose of the present invention and other purposes solve by the following technical programs:
A kind of sulfur-bearing of the present invention, the preparation method of nitrogen castor oil-base green lubrication additive, it is characterised in that described sulfur-bearing, the structural formula of nitrogen castor oil-base green lubrication additive be:
Including step in detail below:
1. adding Oleum Ricini and the alkaline solution of mass ratio 1:1 in flask, control temperature to be stirred at 90～95 DEG C, fully react 2h, wherein chemical equation is:
2. the solution from above-mentioned steps A flask separates upper strata organic solvent, above-mentioned organic solvent is washed by the hot water using temperature to be 90～95 DEG C, above-mentioned washing step is iteratively repeated three times, after then the above-mentioned organic solvent through washing being heated to 95 DEG C, carries out vacuum dehydration；
3. in above-mentioned steps B flask, add the diethanolamine of Oleum Ricini quality 8%, control temperature fully to react 1h at about 90～95 DEG C, carry out cooling process, after using separatory funnel to be separated by upper strata organic solvent, use column chromatography technology that the above-mentioned upper strata organic solvent separated is carried out separating-purifying, and then obtain nitrogenous modified castor oil, chemical equation therein is:
4., after a certain amount of nitrogenous modified castor oil above-mentioned steps C obtained loads there-necked flask, there-necked flask is put in mixture of ice and water, in there-necked flask, dropwise instill the S of nitrogenous modified castor oil quality 5%2Cl2, stirring at a temperature of less than 40 DEG C, fully react 3h, chemical equation therein is:
5. the mixture in above-mentioned steps D there-necked flask is removed, in said mixture, add the NH of nitrogenous modified castor oil quality 1%4SxAfter being sufficiently stirred for 5 minutes, the reduced iron powder of nitrogenous modified castor oil quality 1% is added again in there-necked flask, after stirring reaction 20 minutes, high speed centrifuge is used to be centrifuged separating, using accurate filter paper to filter the supernatant, obtain amber sulfur-bearing, nitrogen castor oil lubricating additive, its chemical equation is:
A kind of sulfur-bearing of present invention offer, the preparation method of nitrogen castor oil-base green lubrication additive, it is preferable that the preferably concentration of the alkaline solution in described step A is the sodium hydroxide solution of 3%.
Advantages of the present invention and having the beneficial effects that:
1. a kind of sulfur-bearing of present invention offer, the preparation method of nitrogen castor oil-base green lubrication additive, directly the Oleum Ricini that biodegradability is excellent is implemented chemical modification, triethanolamine functional group is introduced at its molecule afterbody, castor oil molecule double bond introduces element sulphur, obtaining sulfur-bearing, nitrogen modified castor oil green lubrication additive, the biological degradation rate of this additive reaches more than 90%.
2. a kind of sulfur-bearing of present invention offer, the preparation method of nitrogen castor oil-base green lubrication additive, use this patent synthesis sulfur-bearing, the modified castor oil green lubrication additive of nitrogen, synthesis technique is simple, raw material sources enriches, relative low price, and the green lubrication additive biodegradability that obtains is good, tradition sulfur-bearing, phosphorus, the lubricating additive of chlorine can be replaced.
Detailed description of the invention
The present invention provides a kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive, it is characterised in that described sulfur-bearing, the structural formula of nitrogen castor oil-base green lubrication additive be:
Including step in detail below:
1. adding Oleum Ricini and the alkaline solution of mass ratio 1:1 in flask, control temperature, 90～95 DEG C of stirrings, fully to react 2h, wherein chemical equation is:
2. the solution from above-mentioned steps A flask separates upper strata organic solvent, above-mentioned organic solvent is washed by the hot water using temperature to be 90～95 DEG C, above-mentioned washing step is iteratively repeated three times, after then the above-mentioned organic solvent through washing being heated to 95 DEG C, carries out vacuum dehydration；
3. above-mentioned steps B flask adds the diethanolamine of Oleum Ricini quality 8%, control temperature fully to react 1h at about 90～95 DEG C, carry out cooling process, separatory funnel is used to be separated by upper strata organic solvent, use column chromatography technology that the above-mentioned upper strata organic solvent separated is carried out separating-purifying, and then obtain nitrogenous modified castor oil, chemical equation therein is:
4. a certain amount of nitrogenous modified castor oil above-mentioned steps C obtained loads there-necked flask, puts in mixture of ice and water by above-mentioned there-necked flask, dropwise instills the S of nitrogenous modified castor oil quality 5% in there-necked flask2Cl2, stirring at a temperature of less than 40 DEG C, fully react 3h, chemical equation therein is:
5. the mixture in above-mentioned steps D there-necked flask is removed, in said mixture, add the NH of nitrogenous modified castor oil quality 1%4SxAfter being sufficiently stirred for 5 minutes, the reduced iron powder of nitrogenous modified castor oil quality 1% is added again in there-necked flask, after stirring reaction 20 minutes, use high speed centrifuge centrifugation, using accurate filter paper to filter the supernatant, obtain amber sulfur-bearing, nitrogen castor oil lubricating additive, its chemical equation is:
Technical scheme is further illustrated in conjunction with the embodiments.
Embodiment
A. in flask, add Oleum Ricini and the alkaline solution that mass ratio is 1:1, control temperature to be stirred at 90～95 DEG C, fully react 2h.
B. use separatory funnel that the solution in above-mentioned steps A flask is separated upper strata organic solvent, above-mentioned organic solvent is washed by the hot water using temperature to be 90～95 DEG C, above-mentioned washing step is iteratively repeated three times, after then the above-mentioned organic solvent through washing being heated to 95 DEG C, carries out vacuum dehydration.
C. in above-mentioned steps B flask, add the diethanolamine of Oleum Ricini quality 8%, temperature is controlled at 90～95 DEG C of abundant reaction 1h, then cooling process is carried out, to the mixture in the most cooled flask, separatory funnel is used to be separated by upper strata organic solvent, use column chromatography technology that the above-mentioned upper strata organic solvent separated is carried out separating-purifying, and then obtain nitrogenous modified castor oil.
D. a certain amount of nitrogenous modified castor oil obtained in above-mentioned steps C is loaded there-necked flask, above-mentioned there-necked flask is put in mixture of ice and water, in there-necked flask, dropwise instills the S of nitrogenous modified castor oil quality 5%2Cl2, stir at a temperature of less than 40 DEG C, fully react 3h.
E. the mixture in above-mentioned steps D there-necked flask is removed, in said mixture, add the NH of nitrogenous modified castor oil quality 1%4SxAfter being sufficiently stirred for 5 minutes, the reduced iron powder of nitrogenous modified castor oil quality 1% is added again in there-necked flask, after stirring reaction 20 minutes, use high speed centrifuge centrifugation, using accurate filter paper to filter the supernatant, obtain amber sulfur-bearing, nitrogen castor oil lubricating additive, sulfur-bearing, the productivity of nitrogen castor oil lubricating additive are 81.4% after testing.
According to technical scheme, in the case of the connotation not changing the present invention, those of ordinary skill in the art can propose multiple frame modes of the present invention.Therefore technical scheme is simply illustrated by detailed description below, and is not to be construed as the whole of the present invention or is considered as defining or limiting technical solution of the present invention.
Claims (2)
1. a sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive, it is characterised in that described sulfur-bearing, nitrogen castor oil-base are green
The chemical structural formula of color lubricating additive is:
Including step in detail below:
A. in flask, add Oleum Ricini and the alkaline solution of mass ratio 1:1, temperature is controlled 90～95 DEG C of stirrings, fully
Reaction 2h, wherein chemical equation is:
B. the solution from above-mentioned steps A flask separates upper strata organic solvent, and using temperature is that the hot water of 90～95 DEG C is to above-mentioned
Organic solvent washs, and is iteratively repeated by above-mentioned washing step three times, is then added by the above-mentioned organic solvent through washing
Heat carries out vacuum dehydration after 95 DEG C；
C. in above-mentioned steps B flask, add the diethanolamine of Oleum Ricini quality 8%, control temperature to fill at about 90～95 DEG C
Divide reaction 1h, carry out cooling process, use separatory funnel to be separated by upper strata organic solvent, use column chromatography technology to above-mentioned
The upper strata organic solvent separated carries out separating-purifying, and then obtains nitrogenous modified castor oil, chemical equation therein
For:
D. a certain amount of nitrogenous modified castor oil above-mentioned steps C obtained loads there-necked flask, and above-mentioned there-necked flask is put into ice
In aqueous mixtures, in there-necked flask, dropwise instill the S of nitrogenous modified castor oil quality 5%2Cl2, in the temperature less than 40 DEG C
The lower stirring of degree, fully reacts 3h, and chemical equation therein is:
E. the mixture in above-mentioned steps D there-necked flask is removed, in said mixture, add nitrogenous modified castor oil quality 1%
NH4Sx, after being sufficiently stirred for 5 minutes, then in there-necked flask, add the reduced iron powder of nitrogenous modified castor oil quality 1%,
After stirring reaction 20 minutes, use high speed centrifuge to be centrifuged separating, use accurate filter paper that the supernatant is filtered,
Obtaining amber sulfur-bearing, nitrogen castor oil lubricating additive, chemical equation therein is:
A kind of sulfur-bearing the most according to claim 1, the preparation method of nitrogen castor oil-base green lubrication additive, it is characterised in that
Alkaline solution in described step A preferably concentration is the sodium hydroxide solution of 3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510136349.2A CN106146368A (en) | 2015-03-26 | 2015-03-26 | A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510136349.2A CN106146368A (en) | 2015-03-26 | 2015-03-26 | A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106146368A true CN106146368A (en) | 2016-11-23 |
Family
ID=57340201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510136349.2A Pending CN106146368A (en) | 2015-03-26 | 2015-03-26 | A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106146368A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353965A (en) * | 2016-12-26 | 2017-11-17 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of castor oil-base extreme pressure aqueous lubricating additive |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0448129A2 (en) * | 1986-11-07 | 1991-09-25 | The Lubrizol Corporation | Sulfur-containing compositions, lubricant fuel and functional fluid compositions |
| CN1084552A (en) * | 1992-09-04 | 1994-03-30 | 鲁布里佐尔公司 | Sulfurized overbased compositions |
| CN1150971A (en) * | 1995-05-26 | 1997-06-04 | 埃尔弗安塔法国公司 | Lubricants with molybdenum containing compositions and method of using the same |
| CN104194740A (en) * | 2014-08-01 | 2014-12-10 | 中国石油集团渤海钻探工程有限公司 | Oil-based drilling fluid lubricant and preparation method thereof |
-
2015
- 2015-03-26 CN CN201510136349.2A patent/CN106146368A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0448129A2 (en) * | 1986-11-07 | 1991-09-25 | The Lubrizol Corporation | Sulfur-containing compositions, lubricant fuel and functional fluid compositions |
| CN1084552A (en) * | 1992-09-04 | 1994-03-30 | 鲁布里佐尔公司 | Sulfurized overbased compositions |
| CN1150971A (en) * | 1995-05-26 | 1997-06-04 | 埃尔弗安塔法国公司 | Lubricants with molybdenum containing compositions and method of using the same |
| CN104194740A (en) * | 2014-08-01 | 2014-12-10 | 中国石油集团渤海钻探工程有限公司 | Oil-based drilling fluid lubricant and preparation method thereof |
Non-Patent Citations (5)
| Title |
|---|
| 念合新 等: "蓖麻油在润滑领域中的应用", 《合成润滑材料》 * |
| 方建华 等: "硫化菜籽油润滑添加剂对钢－镁摩擦副摩擦学性能的影响", 《石油炼制与化工》 * |
| 李云飞: "季铵硫酸化蓖麻油的制备", 《河南职工医学院学报》 * |
| 焦叶叶: "含氮、硫润滑油添加剂的合成、表征和润滑性能研究", 《湘潭大学硕士学位论文》 * |
| 胡志孟: "硫化植物油脂肪酸的合成", 《中国油脂》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353965A (en) * | 2016-12-26 | 2017-11-17 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of castor oil-base extreme pressure aqueous lubricating additive |
| CN107353965B (en) * | 2016-12-26 | 2020-08-25 | 中国林业科学研究院林产化学工业研究所 | Preparation method of castor oil-based extreme pressure water-based lubricating additive |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107090327B (en) | A kind of oleic acid boric acid modification lanthanum-stannic oxide/graphene nano composite lubricating oil and preparation method thereof | |
| CN101597535A (en) | A kind of novel organic nitrogen-containing borate ester lubricating oil additive | |
| CN105254663A (en) | Long-chain alkyl imidazole phosphate ionic liquid, preparation method and application thereof | |
| CN106146368A (en) | A kind of sulfur-bearing, the preparation method of nitrogen castor oil-base green lubrication additive | |
| CN115353922A (en) | Carbon nitride quantum dot-based polyethylene glycol lubricating additive and preparation method thereof | |
| CN112920218A (en) | Tert-butyl phenyl phosphate and preparation method and application thereof | |
| CN104437236A (en) | Preparation and purification methods of quaternary ammonium salt type dimeric surfactant | |
| CN106146562B (en) | A kind of production method of phosphorous nitride methyl oleate green lubrication additive | |
| CN102164897B (en) | Method for preparing montelukast sodium salts | |
| CN103880658A (en) | Direct esterification synthesis method of pentaerythritol oleate | |
| CA2524602A1 (en) | Improved seal swell agent and process therefor | |
| CN104804798A (en) | Method for preparing calcium sulfonate complex grease and calcium sulfonate complex grease prepared by using method | |
| CN103739516A (en) | Method for synthesizing adiponitrile by isomerization liquid of 2-methyl-3-crotononitrile | |
| CN106187759A (en) | Guerbet alcohol cyclopentane carboxylic acid ester lubricant and preparation method thereof | |
| CN105777568A (en) | Preparation method of vinyl distearamide | |
| CN103160363A (en) | Lubricant composition containing ionic liquid and manufacture method thereof | |
| CN115646660A (en) | Compound collecting agent capable of being used for lepidolite ore flotation based on anion-cation effect and application thereof | |
| CN106242934A (en) | Oxidation synthesis method for beta-position C-H bond acetyl of ketone | |
| CN106147928B (en) | A kind of production method of boron nitridation methyl oleate green lubrication additive | |
| CN101775326A (en) | Synthesis method of ester oil | |
| CN104326976B (en) | Preparation method of montelukast sodium intermediate | |
| CN106147927A (en) | A kind of preparation method of boronation Rap Oil-based green lubrication additive | |
| CN108165329A (en) | A kind of preparation method of the low water type diesel fuel lubricity modifier of low acid | |
| CN104926845B (en) | A kind of borate ester derivative containing polysulfide bond and its production and use | |
| CN102382142A (en) | High-sulfur phosphorus-free trinuclear molybdenum compound, its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161123 |