WO2022262217A1 - Lithium-based lubricating grease and saponification method thereof - Google Patents
Lithium-based lubricating grease and saponification method thereof Download PDFInfo
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- WO2022262217A1 WO2022262217A1 PCT/CN2021/137126 CN2021137126W WO2022262217A1 WO 2022262217 A1 WO2022262217 A1 WO 2022262217A1 CN 2021137126 W CN2021137126 W CN 2021137126W WO 2022262217 A1 WO2022262217 A1 WO 2022262217A1
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- Prior art keywords
- lithium
- reaction
- preparation
- temperature
- grease
- Prior art date
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- 239000004519 grease Substances 0.000 title claims abstract description 68
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 67
- 238000007127 saponification reaction Methods 0.000 title claims abstract description 39
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 71
- 238000010008 shearing Methods 0.000 claims abstract description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 34
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 23
- 238000007670 refining Methods 0.000 claims abstract description 16
- 238000007872 degassing Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000002199 base oil Substances 0.000 claims description 18
- 235000021355 Stearic acid Nutrition 0.000 claims description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 13
- 239000008117 stearic acid Substances 0.000 claims description 13
- SGHWILJCQCTGGE-UHFFFAOYSA-N 2-dodecyl-2-hydroxyoctadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)(C(O)=O)CCCCCCCCCCCC SGHWILJCQCTGGE-UHFFFAOYSA-N 0.000 claims description 12
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 12
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 12
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 12
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 238000000265 homogenisation Methods 0.000 claims description 3
- 239000002562 thickening agent Substances 0.000 abstract description 7
- 238000001816 cooling Methods 0.000 abstract description 6
- 230000035515 penetration Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 3
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010689 synthetic lubricating oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
-
- 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
- C10M169/02—Mixtures of base-materials and thickeners
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
-
- 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
- C10M2207/1265—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 used as thickening agent
-
- 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
- C10M2207/128—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 containing hydroxy groups; Ethers thereof
- C10M2207/1285—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 containing hydroxy groups; Ethers thereof used as thickening agents
-
- 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
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/02—Bearings
-
- 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
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Definitions
- the invention relates to the technical field of lubricating grease, in particular to a preparation method of lithium-based lubricating grease and a preparation method thereof.
- Lithium-based grease is made from natural fatty acid (stearic acid or 12-hydroxystearic acid) lithium soap, thickened medium viscosity mineral oil or synthetic lubricating oil, while synthetic lithium-based grease is made from synthetic fatty acid lithium soap , Thickened medium viscosity mineral oil made.
- General-purpose lithium-based grease (GB7324-1994) is divided into 1#, 2#, and 3# according to the consistency grade. It has good water resistance, mechanical stability, corrosion resistance and oxidation stability, and is suitable for working temperature -20°C- Lubrication of rolling bearings and sliding bearings and other friction parts of various mechanical equipment at 120°C.
- lithium-based grease affects its performance. In general, it is necessary to add a thickener to ensure its consistency and penetration during preparation, but adding a thickener will increase the cost of the product.
- the present invention provides a preparation method of lithium-based lubricating grease, which can reduce the addition of thickener while ensuring the penetration, thereby reducing product cost.
- the invention also provides a lithium-based lubricating grease.
- the invention discloses a preparation method of lithium-based lubricating grease, in which raw materials are subjected to cyclic shearing treatment during saponification reaction.
- the preparation method of the above-mentioned lithium-based lubricating grease realizes simultaneous cyclic shearing during the saponification reaction, makes the reaction process more complete, can effectively improve the consistency of the lubricating grease, reduce the amount of thickening agent added, and thereby reduce product costs.
- the preparation method of described lithium base grease comprises the following steps:
- the raw materials in the reaction device undergo saponification reaction while carrying out cyclic shearing treatment
- the temperature is raised again for high-temperature refining, and then cooled to obtain the reaction liquid;
- the reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
- the temperature of the reaction device is raised to 90°C-104°C.
- the temperature of the high-temperature refining is 180°C-220°C.
- the step subjecting the reaction solution to cyclic shearing, and performing degassing treatment to obtain lithium-based grease, specifically: subjecting the reaction solution to cyclic shearing, and performing homogenization and degassing Gas treatment to obtain lithium-based grease.
- the reaction device is equipped with a circulation shearing pipeline connected with the reaction device, so as to realize the circulation shearing treatment while the saponification reaction is carried out.
- the lithium-based grease includes the following components by weight: 88-95 parts of base oil, 0.8-1.5 parts of lithium hydroxide monohydrate, 1-2 parts of stearic acid and lauryl hydroxystearic acid 3-10 servings.
- the preparation method of described lithium base grease comprises the following steps:
- the reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
- the base oil is 500N Group II base oil.
- the present invention also provides a lithium-based lubricating grease, which is prepared by the preparation method of the lithium-based lubricating grease.
- the invention provides a preparation method of lithium-based lubricating grease, wherein raw materials are subjected to cyclic shearing treatment during saponification reaction.
- the above-mentioned preparation method of lithium-based lubricating grease realizes simultaneous cyclic shearing during the saponification reaction, which can make the reaction process more complete, and can reduce the addition of thickener while ensuring the cone penetration, thereby reducing product cost .
- the preparation method of above-mentioned lithium base lubricating grease comprises the steps:
- the raw materials are put into the reaction device, and the reaction device is heated up while stirring;
- the raw material in the reaction device undergoes saponification reaction while undergoing cyclic shearing treatment
- the temperature is raised again for high-temperature refining, and then cooled to obtain the reaction liquid;
- the reaction solution is subjected to circular shearing and degassing treatment to obtain lithium-based grease.
- the temperature of the reaction device is raised to 90°C-104°C. Under this temperature condition, the raw materials can be fully dissolved and reach the conditions of saponification reaction.
- the temperature of high-temperature refining is 180°C-220°C.
- the reaction solution is subjected to cyclic shearing and degassing treatment to obtain lithium-based grease, specifically: the reaction solution is subjected to cyclic shearing, homogenization and degassing treatment to obtain lithium-based grease. That is, after the reaction liquid is circulated and sheared, it is first homogenized and then degassed to make the product more uniform and of higher quality.
- the above reaction device is additionally equipped with a circulation shearing pipeline connected with the reaction device, so as to realize the circulation shearing treatment while the saponification reaction is carried out.
- the current saponification reaction device that is, the saponification reaction kettle, is generally not equipped with a circulating shearing pipeline. After installation, the circulating shearing can be directly realized through the reaction device, and the entire process can be completed at the lowest cost.
- the above-mentioned lithium-based grease may include the following components by weight: 88-95 parts of base oil, 0.8-1.5 parts of lithium hydroxide monohydrate, 1-2 parts of stearic acid and 3-3 parts of lauryl hydroxystearic acid 10 servings.
- the reaction solution is subjected to circular shearing and degassing treatment to obtain lithium-based grease.
- the base oil is 500N Group II base oil.
- the present invention also provides a lithium-based lubricating grease, which is prepared by the above-mentioned preparation method of lithium-based lubricating grease.
- the present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 91.4 parts of 500N (Class II) base oil, 1.5 parts of stearic acid and 6 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated up to 100°C while stirring; to maintain the temperature, add 1.1 parts of lithium hydroxide monohydrate to the reaction device for saponification reaction, and at the same time open the circulating shearing tube for cyclic shearing treatment; after the saponification reaction, heat up to 210°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
- 500N Class II
- the present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 90 parts of 500N (Class II) base oil, 1 part of stearic acid and 8 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube to carry out circular shearing treatment; after the saponification reaction, heat up to 220°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
- 500N Class II
- the device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube to carry out circular shearing treatment; after the
- the present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 88 parts of 500N (second class) base oil, 1 part of stearic acid and 3 parts of lauryl hydroxystearic acid into the reaction device, and reacting
- the device is heated to 90°C while stirring; to maintain the temperature, add 0.8 parts of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulation shearing tube to carry out circulation shearing treatment; after saponification reaction, heat up to 200°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
- the present embodiment provides a preparation method of lithium-based grease, comprising the steps of: putting 95 parts of 500N (Class II) base oil, 2 parts of stearic acid and 10 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated up to 100°C while stirring; to maintain the temperature, add 1.5 parts of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube for cyclic shearing treatment; after the saponification reaction, heat up to 200°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
- 500N Class II
- the device is heated up to 100°C while stirring; to maintain the temperature, add 1.5 parts of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube for cyclic shearing treatment; after the saponification reaction,
- the present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 90 parts of 500N (Class II) base oil, 1 part of stearic acid and 8 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulation shearing tube for circulation shearing treatment; after saponification reaction, heat up to 220°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
- 500N Class II
- the device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulation shearing tube for circulation shearing treatment; after saponification reaction, heat up to
- This comparative example provides a kind of preparation method of lithium-based lubricating grease, comprises the steps: 91.4 parts of 500N (second class) base oils, 1.5 parts of stearic acid and 6 parts of lauryl hydroxystearic acid are put into reaction device, react The device was heated up to 100°C while stirring; while maintaining the temperature, 1.1 parts of lithium hydroxide monohydrate was added to the reaction device for saponification reaction; after the saponification reaction, the temperature was raised to 210°C again for high-temperature refining, and then cooled to obtain a reaction solution; The reaction solution is subjected to cyclic shearing and degassing treatment to obtain lithium-based grease.
- 500N second class
- the lithium-based grease prepared by the present invention has less thickening agent added and low consistency, but can achieve the same cone penetration, which can significantly reduce the formulation cost.
Abstract
The present invention relates to the technical field of lubricating grease, and relates in particular to a lithium-based lubricating grease and a preparation method therefor; the preparation method for the lithium-based lubricating grease comprises: performing cyclic shearing processing whilst raw materials are undergoing a saponification reaction, specifically: placing the raw materials in a reaction apparatus, and simultaneously heating the reaction apparatus and stirring; maintaining the temperature, and performing cyclic shearing processing whilst the raw materials in the reaction apparatus are undergoing a saponification reaction; after the saponification reaction, raising the temperature again for high-temperature refining, and then cooling to obtain a reaction solution; performing cyclic shearing on the reaction solution, and performing degassing treatment to obtain lithium-based lubricating grease; the lithium-based lubricating grease is prepared by said method. The preparation method for the lithium-based lubricating grease provided by the present invention can reduce the amount of thickening agent added whilst ensuring the cone penetration, thereby reducing the product cost.
Description
本发明涉及润滑脂技术领域，特别是涉及锂基润滑脂的制备方法及其制备方法。The invention relates to the technical field of lubricating grease, in particular to a preparation method of lithium-based lubricating grease and a preparation method thereof.
锂基润滑脂是由天然脂肪酸(硬脂酸或12-羟基硬脂酸)锂皂，稠化中等粘度的矿物润滑油或合成润滑油制成，而合成锂基润滑脂是由合成脂肪酸锂皂，稠化中等粘度的矿物润滑油制成。通用锂基润滑脂(GB7324-1994)按稠度等级分为1#、2#、3#，具有良好的抗水性、机械安定性、防腐蚀性和氧化安定性，适用于工作温度-20℃-120℃内各种机械设备的滚动轴承和和滑动轴承及其他摩擦部位的润滑。Lithium-based grease is made from natural fatty acid (stearic acid or 12-hydroxystearic acid) lithium soap, thickened medium viscosity mineral oil or synthetic lubricating oil, while synthetic lithium-based grease is made from synthetic fatty acid lithium soap , Thickened medium viscosity mineral oil made. General-purpose lithium-based grease (GB7324-1994) is divided into 1#, 2#, and 3# according to the consistency grade. It has good water resistance, mechanical stability, corrosion resistance and oxidation stability, and is suitable for working temperature -20℃- Lubrication of rolling bearings and sliding bearings and other friction parts of various mechanical equipment at 120°C.
锂基润滑脂的稠度影响着其使用性能，一般情形下制备时需要加入稠化剂保证其稠度和锥入度，而加入稠化剂会提高产品的成本。The consistency of lithium-based grease affects its performance. In general, it is necessary to add a thickener to ensure its consistency and penetration during preparation, but adding a thickener will increase the cost of the product.
发明内容Contents of the invention
基于此，本发明提供一种锂基润滑脂的制备方法，可保证锥入度的同时减少稠化剂的加入量，从而降低产品成本。Based on this, the present invention provides a preparation method of lithium-based lubricating grease, which can reduce the addition of thickener while ensuring the penetration, thereby reducing product cost.
本发明还提供一种锂基润滑脂。The invention also provides a lithium-based lubricating grease.
一种锂基润滑脂的制备方法，原料在皂化反应的同时进行循环剪切处理。The invention discloses a preparation method of lithium-based lubricating grease, in which raw materials are subjected to cyclic shearing treatment during saponification reaction.
上述的锂基润滑脂的制备方法，实现了在皂化反应时可同时进行循环剪切，使反应过程更充分，可有效提高润滑脂的稠度，减少稠化剂的加入量，从而降 低产品成本。The preparation method of the above-mentioned lithium-based lubricating grease realizes simultaneous cyclic shearing during the saponification reaction, makes the reaction process more complete, can effectively improve the consistency of the lubricating grease, reduce the amount of thickening agent added, and thereby reduce product costs.
一实施例中，所述锂基润滑脂的制备方法包括以下步骤：In one embodiment, the preparation method of described lithium base grease comprises the following steps:
将原料投入反应装置内，将所述反应装置升温同时搅拌；Putting the raw materials into the reaction device, heating the reaction device while stirring;
保持温度，所述反应装置内的原料进行皂化反应的同时进行循环剪切处理；Keeping the temperature, the raw materials in the reaction device undergo saponification reaction while carrying out cyclic shearing treatment;
皂化反应后再次升温进行高温炼制，然后冷却，得反应液；After the saponification reaction, the temperature is raised again for high-temperature refining, and then cooled to obtain the reaction liquid;
将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
一实施例中，所述反应装置升温至90℃-104℃。In one embodiment, the temperature of the reaction device is raised to 90°C-104°C.
一实施例中，所述高温炼制的温度为180℃-220℃。In one embodiment, the temperature of the high-temperature refining is 180°C-220°C.
一实施例中，所述步骤：将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂，具体是：将所述反应液进行循环剪切，并进行均质和脱气处理，得锂基润滑脂。In one embodiment, the step: subjecting the reaction solution to cyclic shearing, and performing degassing treatment to obtain lithium-based grease, specifically: subjecting the reaction solution to cyclic shearing, and performing homogenization and degassing Gas treatment to obtain lithium-based grease.
一实施例中，所述反应装置加装一条与所述反应装置连通的循环剪切管道，以实现在皂化反应的同时进行循环剪切处理。In one embodiment, the reaction device is equipped with a circulation shearing pipeline connected with the reaction device, so as to realize the circulation shearing treatment while the saponification reaction is carried out.
一实施例中，所述锂基润滑脂包括如下重量份的组分：基础油88-95份、单水氢氧化锂0.8-1.5份、硬脂酸1-2份及十二羟基硬脂酸3-10份。In one embodiment, the lithium-based grease includes the following components by weight: 88-95 parts of base oil, 0.8-1.5 parts of lithium hydroxide monohydrate, 1-2 parts of stearic acid and lauryl hydroxystearic acid 3-10 servings.
一实施例中，所述的锂基润滑脂的制备方法，包括以下步骤：In one embodiment, the preparation method of described lithium base grease, comprises the following steps:
将基础油、硬脂酸及十二羟基硬脂酸投入反应装置内，将所述反应装置升温至90℃-104℃，同时搅拌；Put the base oil, stearic acid and lauryl hydroxystearic acid into the reaction device, raise the temperature of the reaction device to 90°C-104°C, and stir at the same time;
保持温度，在所述反应装置内加入单水氢氧化锂，进行皂化反应，同时进行循环剪切处理；Maintaining the temperature, adding lithium hydroxide monohydrate into the reaction device, carrying out saponification reaction, and carrying out cyclic shearing treatment at the same time;
皂化反应后再次升温至180℃-220℃进行高温炼制，然后冷却，得反应液；After the saponification reaction, heat up again to 180°C-220°C for high-temperature refining, and then cool to obtain the reaction liquid;
将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
一实施例中，所述基础油为500N二类基础油。In one embodiment, the base oil is 500N Group II base oil.
本发明还提供一种锂基润滑脂，采用所述的锂基润滑脂的制备方法制备形成。The present invention also provides a lithium-based lubricating grease, which is prepared by the preparation method of the lithium-based lubricating grease.
为了便于理解本发明，下面将对本发明进行更全面的描述。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。In order to facilitate the understanding of the present invention, the following will describe the present invention more fully. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention.
本发明提供一种锂基润滑脂的制备方法，原料在皂化反应的同时进行循环剪切处理。The invention provides a preparation method of lithium-based lubricating grease, wherein raw materials are subjected to cyclic shearing treatment during saponification reaction.
上述的锂基润滑脂的制备方法，实现了在皂化反应时可同时进行循环剪切，可使反应的过程更充分，可保证锥入度的同时减少稠化剂的加入量，从而降低产品成本。The above-mentioned preparation method of lithium-based lubricating grease realizes simultaneous cyclic shearing during the saponification reaction, which can make the reaction process more complete, and can reduce the addition of thickener while ensuring the cone penetration, thereby reducing product cost .
具体地，上述的锂基润滑脂的制备方法，包括如下步骤：Specifically, the preparation method of above-mentioned lithium base lubricating grease, comprises the steps:
将原料投入反应装置内，将反应装置升温同时搅拌；The raw materials are put into the reaction device, and the reaction device is heated up while stirring;
保持温度，反应装置内的原料进行皂化反应的同时进行循环剪切处理；Keeping the temperature, the raw material in the reaction device undergoes saponification reaction while undergoing cyclic shearing treatment;
皂化反应后再次升温进行高温炼制，然后冷却，得反应液；After the saponification reaction, the temperature is raised again for high-temperature refining, and then cooled to obtain the reaction liquid;
将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is subjected to circular shearing and degassing treatment to obtain lithium-based grease.
其中，反应装置升温至90℃-104℃。在该温度条件下，原料可以充分地溶解并达到皂化反应的条件。Wherein, the temperature of the reaction device is raised to 90°C-104°C. Under this temperature condition, the raw materials can be fully dissolved and reach the conditions of saponification reaction.
其中，高温炼制的温度为180℃-220℃。Among them, the temperature of high-temperature refining is 180°C-220°C.
将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂，具体是：将反应液进行循环剪切，并进行均质和脱气处理，得锂基润滑脂。即，反应液循环剪切后，先进行均质，再进行脱气处理，使得产品更均匀，质量更高。The reaction solution is subjected to cyclic shearing and degassing treatment to obtain lithium-based grease, specifically: the reaction solution is subjected to cyclic shearing, homogenization and degassing treatment to obtain lithium-based grease. That is, after the reaction liquid is circulated and sheared, it is first homogenized and then degassed to make the product more uniform and of higher quality.
上述的反应装置加装一条与该反应装置连通的循环剪切管道，以实现在皂化反应的同时进行循环剪切处理。目前的皂化反应装置即皂化反应釜一般都没有安装循环剪切管道，加装后可以直接通过该反应装置实现循环剪切，在最低的成本下完成整个工艺过程。The above reaction device is additionally equipped with a circulation shearing pipeline connected with the reaction device, so as to realize the circulation shearing treatment while the saponification reaction is carried out. The current saponification reaction device, that is, the saponification reaction kettle, is generally not equipped with a circulating shearing pipeline. After installation, the circulating shearing can be directly realized through the reaction device, and the entire process can be completed at the lowest cost.
上述的锂基润滑脂，例如可以包括如下重量份的组分：基础油88-95份、单水氢氧化锂0.8-1.5份、硬脂酸1-2份及十二羟基硬脂酸3-10份。The above-mentioned lithium-based grease, for example, may include the following components by weight: 88-95 parts of base oil, 0.8-1.5 parts of lithium hydroxide monohydrate, 1-2 parts of stearic acid and 3-3 parts of lauryl hydroxystearic acid 10 servings.
基于该锂基润滑脂，采用如下的制备方法，Based on the lithium-based grease, the following preparation method is adopted,
将基础油、硬脂酸及十二羟基硬脂酸投入反应装置内，将反应装置升温至90℃-104℃，同时搅拌；Put the base oil, stearic acid and lauryl hydroxystearic acid into the reaction device, raise the temperature of the reaction device to 90°C-104°C, and stir at the same time;
保持温度，在反应装置内加入单水氢氧化锂，进行皂化反应，同时进行循环剪切处理；Keep the temperature, add lithium hydroxide monohydrate in the reaction device, carry out saponification reaction, and carry out cyclic shearing treatment at the same time;
皂化反应后再次升温至180℃-220℃进行高温炼制，然后冷却，得反应液；After the saponification reaction, heat up again to 180°C-220°C for high-temperature refining, and then cool to obtain the reaction liquid;
将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is subjected to circular shearing and degassing treatment to obtain lithium-based grease.
一实施例中，基础油为500N二类基础油。In one embodiment, the base oil is 500N Group II base oil.
本发明还提供一种锂基润滑脂，采用上述的锂基润滑脂的制备方法制备形成。The present invention also provides a lithium-based lubricating grease, which is prepared by the above-mentioned preparation method of lithium-based lubricating grease.
以下将通过几个实施例来进一步说明本发明的实施方式。The implementation of the present invention will be further described through several examples below.
实施例一Embodiment one
本实施例提供一种锂基润滑脂的制备方法，包括如下步骤：将91.4份500N(二类)基础油、1.5份硬脂酸及6份十二羟基硬脂酸投入反应装置内，将反应 装置升温至100℃，同时搅拌；保持温度，在反应装置内加入1.1份单水氢氧化锂，进行皂化反应，同时开启循环剪切管进行循环剪切处理；皂化反应后再次升温至210℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 91.4 parts of 500N (Class II) base oil, 1.5 parts of stearic acid and 6 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated up to 100°C while stirring; to maintain the temperature, add 1.1 parts of lithium hydroxide monohydrate to the reaction device for saponification reaction, and at the same time open the circulating shearing tube for cyclic shearing treatment; after the saponification reaction, heat up to 210°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
实施例二Embodiment two
本实施例提供一种锂基润滑脂的制备方法，包括如下步骤：将90份500N(二类)基础油、1份硬脂酸及8份十二羟基硬脂酸投入反应装置内，将反应装置升温至104℃，同时搅拌；保持温度，在反应装置内加入1份单水氢氧化锂，进行皂化反应，同时开启循环剪切管进行循环剪切处理；皂化反应后再次升温至220℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 90 parts of 500N (Class II) base oil, 1 part of stearic acid and 8 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube to carry out circular shearing treatment; after the saponification reaction, heat up to 220°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
实施例三Embodiment three
本实施例提供一种锂基润滑脂的制备方法，包括如下步骤：将88份500N(二类)基础油、1份硬脂酸及3份十二羟基硬脂酸投入反应装置内，将反应装置升温至90℃，同时搅拌；保持温度，在反应装置内加入0.8份单水氢氧化锂，进行皂化反应，同时开启循环剪切管进行循环剪切处理；皂化反应后再次升温至200℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 88 parts of 500N (second class) base oil, 1 part of stearic acid and 3 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated to 90°C while stirring; to maintain the temperature, add 0.8 parts of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulation shearing tube to carry out circulation shearing treatment; after saponification reaction, heat up to 200°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
实施例四Embodiment Four
本实施例提供一种锂基润滑脂的制备方法，包括如下步骤：将95份500N(二类)基础油、2份硬脂酸及10份十二羟基硬脂酸投入反应装置内，将反应装置升温至100℃，同时搅拌；保持温度，在反应装置内加入1.5份单水氢氧化锂，进行皂化反应，同时开启循环剪切管进行循环剪切处理；皂化反应后再次 升温至200℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The present embodiment provides a preparation method of lithium-based grease, comprising the steps of: putting 95 parts of 500N (Class II) base oil, 2 parts of stearic acid and 10 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated up to 100°C while stirring; to maintain the temperature, add 1.5 parts of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulating shearing tube for cyclic shearing treatment; after the saponification reaction, heat up to 200°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
实施例五Embodiment five
本实施例提供一种锂基润滑脂的制备方法，包括如下步骤：将90份500N(二类)基础油、1份硬脂酸及8份十二羟基硬脂酸投入反应装置内，将反应装置升温至104℃，同时搅拌；保持温度，在反应装置内加入1份单水氢氧化锂，进行皂化反应，同时开启循环剪切管进行循环剪切处理；皂化反应后再次升温至220℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The present embodiment provides a preparation method of lithium-based lubricating grease, comprising the steps of: putting 90 parts of 500N (Class II) base oil, 1 part of stearic acid and 8 parts of lauryl hydroxystearic acid into the reaction device, and reacting The device is heated to 104°C while stirring; to maintain the temperature, add 1 part of lithium hydroxide monohydrate to the reaction device to carry out saponification reaction, and at the same time open the circulation shearing tube for circulation shearing treatment; after saponification reaction, heat up to 220°C again for Refining at high temperature, then cooling to obtain the reaction solution; cyclically shearing the reaction solution and performing degassing treatment to obtain lithium-based grease.
对比例comparative example
本对比例提供一种锂基润滑脂的制备方法，包括如下步骤：将91.4份500N(二类)基础油、1.5份硬脂酸及6份十二羟基硬脂酸投入反应装置内，将反应装置升温至100℃，同时搅拌；保持温度，在反应装置内加入1.1份单水氢氧化锂，进行皂化反应；皂化反应后再次升温至210℃进行高温炼制，然后冷却，得反应液；将反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。This comparative example provides a kind of preparation method of lithium-based lubricating grease, comprises the steps: 91.4 parts of 500N (second class) base oils, 1.5 parts of stearic acid and 6 parts of lauryl hydroxystearic acid are put into reaction device, react The device was heated up to 100°C while stirring; while maintaining the temperature, 1.1 parts of lithium hydroxide monohydrate was added to the reaction device for saponification reaction; after the saponification reaction, the temperature was raised to 210°C again for high-temperature refining, and then cooled to obtain a reaction solution; The reaction solution is subjected to cyclic shearing and degassing treatment to obtain lithium-based grease.
以下将对各个实施例以及对比例的效果进行检测，结果见表一。The effects of various embodiments and comparative examples will be tested below, and the results are shown in Table 1.
表一Table I
从上表数据可以看出，采用本发明所制备的锂基润滑脂，加入的稠化剂更少，稠度低，但可以达到同样的锥入度，可显著降低配方成本。It can be seen from the data in the above table that the lithium-based grease prepared by the present invention has less thickening agent added and low consistency, but can achieve the same cone penetration, which can significantly reduce the formulation cost.
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。The various technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the various technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be pointed out that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.
Claims (10)
- 一种锂基润滑脂的制备方法，其特征在于，原料在皂化反应的同时进行循环剪切处理。A preparation method of lithium-based lubricating grease is characterized in that raw materials are subjected to cyclic shearing treatment during saponification reaction.
- 根据权利要求1所述的锂基润滑脂的制备方法，其特征在于，所述的锂基润滑脂的制备方法包括如下步骤：The preparation method of lithium base grease according to claim 1, is characterized in that, the preparation method of described lithium base grease comprises the steps:将原料投入反应装置内，将所述反应装置升温同时搅拌；Putting the raw materials into the reaction device, heating the reaction device while stirring;保持温度，所述反应装置内的原料进行皂化反应的同时进行循环剪切处理；Keeping the temperature, the raw materials in the reaction device undergo saponification reaction while carrying out cyclic shearing treatment;皂化反应后再次升温进行高温炼制，然后冷却，得反应液；After the saponification reaction, the temperature is raised again for high-temperature refining, and then cooled to obtain the reaction liquid;将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
- 根据权利要求2所述的锂基润滑脂的制备方法，其特征在于，所述反应装置升温至90℃-104℃。The preparation method of lithium-based grease according to claim 2, characterized in that the temperature of the reaction device is raised to 90°C-104°C.
- 根据权利要求2所述的锂基润滑脂的制备方法，其特征在于，所述高温炼制的温度为180℃-220℃。The preparation method of lithium-based grease according to claim 2, characterized in that the temperature of the high-temperature refining is 180°C-220°C.
- 根据权利要求2所述的锂基润滑脂的制备方法，其特征在于，所述步骤：将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂，具体是：将所述反应液进行循环剪切，并进行均质和脱气处理，得锂基润滑脂。The preparation method of lithium-based grease according to claim 2, characterized in that, the step: subjecting the reaction solution to cyclic shearing and degassing treatment to obtain lithium-based grease, specifically: The reaction solution is subjected to cyclic shearing, homogenization and degassing treatment to obtain lithium-based grease.
- 根据权利要求2所述的锂基润滑脂的制备方法，其特征在于，所述反应装置加装一条与所述反应装置连通的循环剪切管道，以实现在皂化反应的同时进行循环剪切处理。The preparation method of lithium base lubricating grease according to claim 2, is characterized in that, described reaction device installs a circulation shear pipeline that is communicated with described reaction device additionally, to realize while saponification reaction, carry out circulation shear processing .
- 根据权利要求2所述的锂基润滑脂的制备方法，其特征在于，所述锂基润滑脂包括如下重量份的组分：基础油88-95份、单水氢氧化锂0.8-1.5份、硬脂酸1-2份及十二羟基硬脂酸3-10份。The preparation method of lithium-based grease according to claim 2 is characterized in that, the lithium-based grease comprises the following components by weight: 88-95 parts of base oil, 0.8-1.5 parts of lithium hydroxide monohydrate, 1-2 parts of stearic acid and 3-10 parts of lauryl hydroxystearic acid.
- 根据权利要求7所述的锂基润滑脂的制备方法，其特征在于，包括以下步骤：The preparation method of lithium base grease according to claim 7, is characterized in that, comprises the following steps:将基础油、硬脂酸及十二羟基硬脂酸投入反应装置内，将所述反应装置升温至90℃-104℃，同时搅拌；Put the base oil, stearic acid and lauryl hydroxystearic acid into the reaction device, raise the temperature of the reaction device to 90°C-104°C, and stir at the same time;保持温度，在所述反应装置内加入单水氢氧化锂，进行皂化反应，同时进行循环剪切处理；Maintaining the temperature, adding lithium hydroxide monohydrate into the reaction device, carrying out saponification reaction, and carrying out cyclic shearing treatment at the same time;皂化反应后再次升温至180℃-220℃进行高温炼制，然后冷却，得反应液；After the saponification reaction, heat up again to 180°C-220°C for high-temperature refining, and then cool to obtain the reaction liquid;将所述反应液进行循环剪切，并进行脱气处理，得锂基润滑脂。The reaction solution is cyclically sheared and degassed to obtain lithium-based grease.
- 根据权利要求7或8所述的锂基润滑脂的制备方法，其特征在于，所述基础油为500N二类基础油。The preparation method of lithium-based grease according to claim 7 or 8, characterized in that, the base oil is a 500N class II base oil.
- 一种锂基润滑脂，其特征在于，采用如权利要求1-8任一项所述的锂基润滑脂的制备方法制备形成。A lithium-based grease, characterized in that it is prepared by the preparation method of lithium-based grease as claimed in any one of claims 1-8.
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| CN101619260B (en) * | 2009-08-07 | 2013-01-09 | 安庆市中天石油化工有限公司 | Preparation method of high shear stability lithium grease |
| CN101993769B (en) * | 2010-11-25 | 2012-12-26 | 无锡中石油润滑脂有限责任公司 | Complex lithium base grease and preparation method thereof |
| CN102433214B (en) * | 2011-10-28 | 2014-02-12 | 无锡惠源高级润滑油有限公司 | Preparation method of lithium calcium lubricating grease |
| CN109810748B (en) * | 2019-02-25 | 2021-05-07 | 广西柳工机械股份有限公司 | Lithium-based lubricating grease and preparation method thereof |
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- 2021-06-18 CN CN202110677073.4A patent/CN113549492A/en active Pending
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