CN110106008B - Preparation method and application of lithium-based thickening agent - Google Patents
Preparation method and application of lithium-based thickening agent Download PDFInfo
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- CN110106008B CN110106008B CN201910454283.XA CN201910454283A CN110106008B CN 110106008 B CN110106008 B CN 110106008B CN 201910454283 A CN201910454283 A CN 201910454283A CN 110106008 B CN110106008 B CN 110106008B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/10—Phosphatides, e.g. lecithin, cephalin
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a preparation method and application of a lithium-based thickening agent, wherein the preparation method of the lithium-based thickening agent comprises the following steps: (1) 3-4 parts by mass of tannic acid, 60-80 parts by mass of 12 hydroxystearic acid, 0.1-0.2 part by mass of phospholipid, 0.1-0.2 part by mass of chain polyethylene glycol and 500 parts by mass of water are stirred for 1-2 hours at the normal pressure and the rotating speed of 200-; (2) adding 0.4-0.6 part by mass of lithium hydroxide, uniformly mixing, and keeping the mixture at the normal pressure of 60-80 ℃ for 0.5-1 hour for pre-reaction; (3) adjusting pH to 10-11, adding 4-6 parts by mass of lithium carbonate, keeping nitrogen pressure at 1-2Mpa, rapidly heating to 160-180 ℃, keeping for 0.1-0.2 h, filtering and washing. The lithium-based thickening agent can improve the dropping point and the antifriction and antiwear performances of the prepared lithium-based lubricating oil.
Description
Technical Field
The invention relates to the technical field of lubricating oil, and particularly relates to a preparation method and application of a lithium-based thickening agent.
Background
With the development of modern industrial technology, industries such as steel, automobiles and textile, higher requirements are provided for high and low temperature performance and antifriction and antiwear performance of lubricating grease, at present, lithium-based lubricating grease cannot meet the harsh working condition conditions of high temperature, high speed and heavy load, and although ordinary composite lithium-based lubricating grease has certain advantages compared with lithium-based lubricating grease in the use process, the common composite lithium-based lubricating grease has poor antifriction and antiwear performance due to low dropping point and is difficult to meet the use requirements, and in order to meet the requirements of the harsh working condition, a plurality of antiwear extreme pressure additives are required to be added into the composite lithium-based lubricating grease. At present, the complex lithium grease is developed rapidly in China, and basically replaces the lithium grease, a plurality of documents reporting the complex lithium grease at home and abroad exist, and patents related to the complex lithium grease continuously appear, such as U.S. patent application publications US3681242, US3711407 and US 3929651; chinese patent application publications CN1052890A and CN1052891A, the compositions of the compound lithium grease are basically the same, the compound lithium grease comprises two components of 12 hydroxystearic acid and dibasic acid (azelaic acid and sebacic acid), and also comprises three components of salicylic acid and boric acid, the preparation method is to add the materials together to react with lithium hydroxide to generate a compound, the dropping point of the compound lithium grease prepared in the way is not high, only reaches about 260 ℃ plus 280 ℃, the antifriction and antiwear properties are not outstanding, the PB value is not over 980N, the modern industrial equipment has higher requirements on the use temperature and the antifriction and antiwear properties, and the traditional preparation process of simultaneously adding the materials of 12 hydroxystearic acid, sebacic acid, boric acid and the like at one time needs to add an antiwear and antifriction agent to meet the use requirements. In order to improve the dropping point and the antifriction and antiwear performance of the lithium complex grease and to add no antifriction and antiwear agent, the preparation process of the lithium complex grease needs to be improved.
The Chinese patent with the application number of CN201510955845.0 discloses a thickening agent and composite lithium-based lubricating grease containing the thickening agent, wherein the thickening agent is a compound formed by compounding 12 hydroxy fatty acid lithium soap and binary acid lithium soap after saponification of 12 hydroxy stearic acid, binary acid, lithium hydroxide and water, and then boric acid, wherein the boric acid is added after the saponification is completed, the pressure in a pressure kettle is released to normal pressure, the temperature in the pressure kettle is 110-. The composite lithium-based lubricating grease comprises a thickening agent, base oil or synthetic oil and an additive consisting of an antioxidant and an antirust agent.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium-based thickening agent, which comprises the steps of adding a proper amount of phospholipid and chain-like polyethylene glycol into raw materials, pre-dispersing, adopting tannic acid and 12-hydroxystearic acid as ligands of lithium ions in a system, adding a small amount of lithium hydroxide to regulate alkalinity and pre-react to serve as a nucleation center, and then supplementing lithium carbonate to quickly finish the reaction, thereby improving the fineness of the prepared lithium-based thickening agent and simultaneously improving the dropping point and the friction-reducing and wear-resisting properties of lithium-based lubricating oil.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of preparing a lithium-based thickener, comprising: (1) 3-4 parts by mass of tannic acid, 60-80 parts by mass of 12 hydroxystearic acid, 0.1-0.2 part by mass of phospholipid, 0.1-0.2 part by mass of chain polyethylene glycol and 500 parts by mass of water are stirred for 1-2 hours at the normal pressure and the rotating speed of 200-; (2) adding 0.4-0.6 part by mass of lithium hydroxide, uniformly mixing, and keeping the mixture at the normal pressure of 60-80 ℃ for 0.5-1 hour for pre-reaction; (3) adjusting pH to 10-11, adding 4-6 parts by mass of lithium carbonate, keeping nitrogen pressure at 1-2Mpa, rapidly heating to 160-180 ℃, keeping for 0.1-0.2 h, filtering and washing.
Further, the molecular weight of the chain polyethylene glycol is 500-1000.
Further, the temperature increase rate of the rapid temperature increase in the step 3 is 10 ℃/min.
Further, the pH adjustment in step 3 is performed by adding sodium hydroxide.
Further, the adding mass ratio of the lithium hydroxide to the lithium carbonate is 1: 10.
The application of the lithium-based thickening agent is characterized in that the lithium-based thickening agent is used for preparing lithium-based lubricating grease, and the lithium-based lubricating grease comprises 75-90 parts by mass of base oil, 10-20 parts by mass of the lithium-based thickening agent, 0.1-0.2 part by mass of antioxidant and 0.1-0.2 part by mass of antirust agent.
The invention has the following beneficial effects:
according to the invention, 12-hydroxystearic acid is used as a reaction main body, tannic acid is used as an additive, the planar structure of macromolecules of tannic acid can be effectively utilized, on one hand, the tannic acid is used as a template agent to regulate and control the micro-morphology of lithium fatty acid, and meanwhile, after the tannic acid is chelated with lithium ions, the antifriction and antiwear performances of the lithium-based lubricating oil can be effectively improved.
The invention is characterized in that proper amount of phospholipid and chain polyethylene glycol are added into raw materials for pre-dispersion. The phospholipid has a surface activity effect, can have a certain emulsification effect and simultaneously has a certain antioxidation function, and when the polyethylene glycol is added and the molecular weight of the phospholipid is controlled within the range of 500-1000, the shape of the product can be effectively controlled, the performance of the product can be adjusted, the dispersion effect of the product is improved, and the product is not agglomerated.
According to the invention, proper lithium hydroxide is added firstly, after pre-reaction, microscopic lithium fatty acid formed by partial reaction can be used as a nucleation core, and cheap lithium carbonate is added, so that rapid reaction can be carried out in a short time at a higher temperature and pressure, the reaction is more sufficient, and the morphology and the particle size of the product are further controlled in the balance of dissolution and precipitation.
The preparation method adopts the pre-dispersion of a fatty acid system, can form a micro-phase emulsion, then takes partial saponification as a nucleation core to carry out full reaction at high temperature and high pressure, and can effectively improve the fineness of the lithium fatty acid by combining the methods.
Compared with the prior art, the preparation method has the advantages of low cost and high reaction speed, and the prepared thickening agent has better technical effect.
Detailed Description
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
Example 1
A method of preparing a lithium-based thickener, comprising: (1) heating 3.5 parts by mass of tannic acid, 70 parts by mass of 12-hydroxystearic acid, 0.15 part by mass of phospholipid, 0.15 part by mass of chain polyethylene glycol and 500 parts by mass of water at the rotating speed of 350 revolutions to 70 ℃, and stirring for 1.5 hours under normal pressure; (2) adding 0.5 part by mass of lithium hydroxide, uniformly mixing, and keeping the mixture at the normal pressure of 70 ℃ for 0.5 to 1 hour for pre-reaction; (3) adjusting pH to 10-11, adding 5 parts by mass of lithium carbonate, maintaining nitrogen pressure at 1.5Mpa, rapidly heating to 170 deg.C, maintaining for 0.1-0.2 hr, filtering, and washing. The molecular weight of the chain polyethylene glycol is 500-1000. The temperature rise rate of the rapid temperature rise in the step 3 is 10 ℃/min. The pH adjustment in step 3 is carried out by adding sodium hydroxide. The adding mass ratio of the lithium hydroxide to the lithium carbonate is 1: 10.
A lithium-based grease comprising the lithium-based thickener according to the above, which comprises 80 parts by mass of a base oil, 15 parts by mass of the lithium-based thickener, 1.5 parts by mass of an antioxidant alkyldiphenylamine and 1.5 parts by mass of an antirust barium petroleum sulfonate. The preparation method comprises the following steps: adding half of the base oil into the lithium-based thickening agent, continuing heating and stirring, stopping heating and heating when the temperature is raised to 230 ℃ under normal pressure, keeping the temperature constant for 0.5 hour, adding half of the base oil, transferring into a blending kettle, circularly cooling to 130 ℃ in the blending kettle, shearing to 110 ℃ through a mechanical pump, adding an antioxidant and an antirust agent at 110 ℃ of 105-.
Comparative example 1
The procedure was essentially the same as in example 1, except that the starting materials for the preparation of the lithium-based thickener were devoid of phospholipids.
Comparative example 2
The procedure was essentially the same as in example 1, except that tannic acid was absent from the raw material used to make the lithium-based thickener.
Comparative example 3
The procedure was essentially the same as in example 1, except that the raw materials for the preparation of the lithium-based thickener were devoid of chain polyethylene glycol.
Comparative example 4
The preparation process is basically the same as that of example 1, except that the raw materials for preparing the lithium-based thickening agent lack phospholipids, tannins and chain polyethylene glycols.
Comparative example 5
The preparation process was substantially the same as that of example 1, except that the 2 nd step was not performed in the preparation of the lithium-based thickener.
Comparative example 6
The preparation process is substantially the same as that of example 1, except that the lithium-based thickener is prepared by direct sealing reaction without applying pressure in step 3.
Comparative example 7
The preparation process was substantially the same as that of example 1, except that the pH was not adjusted in step 3 for preparing the lithium-based thickener.
Comparative example 8
The lithium complex grease was prepared by the method described in example 1 of the chinese patent application "a thickener and lithium complex grease (publication No. CN105542904B) containing the thickener".
Comparative example 9
The preparation process was substantially the same as that of example 1, except that the molecular weight of the chain polyethylene glycol in the raw material for preparing the lithium-based thickener was 4000.
The lithium-based greases prepared in examples and comparative examples were tested for dropping point and four-ball PB values according to GB/T3498, GB/T3142, and the results are shown in the following table.
| Experimental project | Particle size | Dropping Point C | PB value Kg |
| Example 1 | ～0.2um | 351 | 132 |
| Comparative example 1 | ～0.5um | 318 | 122 |
| Comparative example 2 | ～0.5um | 312 | 104 |
| Comparative example 3 | ～0.5um | 333 | 116 |
| Comparative example 4 | ～2um | 294 | 92 |
| Comparative example 5 | ～2um | 292 | 98 |
| Comparative example 6 | ～0.5um | 340 | 124 |
| Comparative example 7 | ～1um | 305 | 111 |
| Comparative example 8 | ～0.5um | 304 | 92 |
| Comparative example 9 | ～1um | 314 | 104 |
From the above table, it can be seen that: as can be seen from the data of the example 1 and the comparative examples 1, 2, 3 and 4, the addition of the phospholipid, the tannic acid and the chain polyethylene glycol has obvious technical improvement compared with the addition of the phospholipid, the tannic acid and the chain polyethylene glycol alone, and plays a role in synergistic improvement. It can be seen from the comparison of example 1 and comparative examples 5, 6 and 7 that the performance of the product can be effectively improved by applying a certain pressure and adjusting the pH in a small amount of lithium hydroxide as a nucleation core. As can be seen from example 1 and comparative example 9, the product performance can be effectively improved and the particle size can be effectively reduced by adding polyethylene glycol with a certain molecular weight.
The above description should not be taken as limiting the invention to the embodiments, but rather, as will be apparent to those skilled in the art to which the invention pertains, numerous simplifications or substitutions may be made without departing from the spirit of the invention, which shall be deemed to fall within the scope of the invention as defined by the claims appended hereto.
Claims (1)
1. The preparation method of the lithium-based thickening agent is characterized by comprising the following steps of:
(1) mixing 3-4 parts by mass of tannic acid, 60-80 parts by mass of 12-hydroxystearic acid, 0.1-0.2 part by mass of phospholipid, 0.1-0.2 part by mass of chain polyethylene glycol and 500 parts by mass of water at the rotation speed of 200-500 turns, heating to 60-80 ℃, and stirring for 1-2 hours under normal pressure;
(2) adding 0.4-0.6 part by mass of lithium hydroxide, uniformly mixing, and keeping the mixture at the normal pressure of 60-80 ℃ for 0.5-1 hour to carry out pre-reaction;
(3) after the pH value is adjusted to 10-11, 4-6 parts by mass of lithium carbonate is added, the nitrogen pressure is kept at 1-2Mpa, the temperature is quickly raised to 160-180 ℃ and kept for 0.1-0.2 hours, and then the mixture is filtered and washed;
the molecular weight of the chain polyethylene glycol is 500-1000; the temperature rise rate of the rapid temperature rise in the step (3) is 10 ℃/min; adjusting the pH value in the step (3) by adding sodium hydroxide; the adding mass ratio of the lithium hydroxide to the lithium carbonate is 1: 10.
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| CN201910454283.XA CN110106008B (en) | 2019-05-29 | 2019-05-29 | Preparation method and application of lithium-based thickening agent |
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| CN201910454283.XA CN110106008B (en) | 2019-05-29 | 2019-05-29 | Preparation method and application of lithium-based thickening agent |
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| CN110106008B true CN110106008B (en) | 2021-07-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560264A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Composite lithium-based lubricating grease and preparation method thereof |
| CN106479285A (en) * | 2016-09-12 | 2017-03-08 | 中国航空工业集团公司北京航空材料研究院 | A kind of Graphene strengthens waterborne rusted paint and its preparation and application |
| CN108998147A (en) * | 2017-06-07 | 2018-12-14 | 汪健 | A kind of 12- hydroxy stearic acid, boric acid complex lithium prefabricated soap lubricant composition and preparation method thereof |
| CN109292760A (en) * | 2018-11-30 | 2019-02-01 | 长江师范学院 | A method of preparing graphene |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6576298B2 (en) * | 2000-09-07 | 2003-06-10 | Ecolab Inc. | Lubricant qualified for contact with a composition suitable for human consumption including a food, a conveyor lubrication method and an apparatus using droplets or a spray of liquid lubricant |
| US7435708B2 (en) * | 2003-09-09 | 2008-10-14 | Lopes John A | Lubricant composition |
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- 2019-05-29 CN CN201910454283.XA patent/CN110106008B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560264A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Composite lithium-based lubricating grease and preparation method thereof |
| CN106479285A (en) * | 2016-09-12 | 2017-03-08 | 中国航空工业集团公司北京航空材料研究院 | A kind of Graphene strengthens waterborne rusted paint and its preparation and application |
| CN108998147A (en) * | 2017-06-07 | 2018-12-14 | 汪健 | A kind of 12- hydroxy stearic acid, boric acid complex lithium prefabricated soap lubricant composition and preparation method thereof |
| CN109292760A (en) * | 2018-11-30 | 2019-02-01 | 长江师范学院 | A method of preparing graphene |
Non-Patent Citations (1)
| Title |
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| 复合锂基润滑脂的研究进展;成思远等;《当代化工》;20190131;第152-158页 * |
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