CN110951531A - Method for preparing composite calcium sulfonate-based lubricating grease - Google Patents
Method for preparing composite calcium sulfonate-based lubricating grease Download PDFInfo
- Publication number
- CN110951531A CN110951531A CN201911273337.9A CN201911273337A CN110951531A CN 110951531 A CN110951531 A CN 110951531A CN 201911273337 A CN201911273337 A CN 201911273337A CN 110951531 A CN110951531 A CN 110951531A
- Authority
- CN
- China
- Prior art keywords
- calcium sulfonate
- saponification
- conversion
- base
- lubricating grease
- 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
Classifications
-
- 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
- C10M173/00—Lubricating compositions containing more than 10% water
-
- 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
- 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
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/046—Overbasedsulfonic acid salts
- C10M2219/0466—Overbasedsulfonic acid salts used as thickening agents
Abstract
The invention discloses a preparation method of composite calcium sulfonate-based lubricating grease, which comprises a conversion stage, a saponification stage, a thickening grease-forming and high-temperature refining stage and a post-treatment stage. The invention monitors the completion degree of conversion and saponification; and by controlling the cooling speed in the grease making process, the grease with satisfactory colloid stability and mechanical stability is obtained.
Description
Technical Field
The invention relates to the field of lubricating oil, in particular to a method for preparing composite calcium sulfonate-based lubricating grease.
Background
The composite calcium sulfonate-based lubricating grease has good high temperature resistance, extreme pressure wear resistance, water resistance, shear stability, rust resistance and low-temperature pumping property, and is a kind of all-round high-efficiency lubricating grease. The composite calcium sulfonate-based lubricating grease is widely applied to the industries of steel, smelting, paper pulp, shipping, railways, power generation, automobiles, buildings, food machinery and the like.
However, an efficient and quick manufacturing method of the composite calcium sulfonate-based lubricating grease is still lacked.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects of the prior art, the invention provides a method for preparing composite calcium sulfonate-based lubricating grease, which comprises a conversion stage, a saponification stage, a thickening grease-forming and high-temperature refining stage and a post-treatment stage; monitoring the completion degree of the conversion and saponification; and by controlling the cooling speed in the grease making process, the grease with satisfactory colloid stability and mechanical stability is obtained.
The technical scheme is as follows: the invention relates to a method for preparing composite calcium sulfonate-based lubricating grease, which comprises the following steps:
(1) and (3) a conversion stage: diluting high-base-number calcium sulfonate with 50 wt% of base oil, uniformly stirring the base oil and the high-base-number calcium sulfonate, heating to over 80 ℃, adding an acetic acid conversion agent diluted by 2 times of water for conversion, controlling the conversion temperature to be between 80 and 100 ℃, and controlling the conversion time to be between 50 and 70 min;
(2) and (3) saponification stage: after the conversion of the high-base-number calcium sulfonate is finished, adding the rest 50 wt% of base oil, 12-hydroxystearic acid, calcium hydroxide solution and boric acid solution, controlling the saponification temperature below 100 ℃ and the saponification time between 50min and 70 min;
(3) thickening grease and high-temperature refining: after saponification, heating the soap base in the reaction kettle to above 130 ℃, after dehydration of soap water, heating the temperature to 160-170 ℃, keeping the temperature for 50-70 min, then compounding, and heating to above 220 ℃ after compounding and keeping the temperature for above 3 min;
(4) and (3) post-treatment stage: and cooling the grease to obtain the final compound calcium sulfonate-based lubricating grease product.
Wherein, in the step (1), the Newtonian high-base-number calcium sulfonate is converted into non-Newtonian bodies by a conversion agent.
Wherein, the completeness of the transformation is identified by the transformation progress of the crystal form of the calcium carbonate in the step (1).
Wherein, the calcium hydroxide solution in the step (2) is a calcium hydroxide solution diluted by 10 times of water; the boric acid solution is 4 times of boric acid solution diluted by water.
When the saponification in the step (2) is completed, a viscous substance is formed in the refining kettle by the soap base and the base oil, a viscous substance sample is taken from the kettle, and the content of free acid and alkali is measured to identify the completeness of the saponification reaction.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the invention provides a method for preparing efficient and quick composite calcium sulfonate-based lubricating grease, which comprises a conversion stage, a saponification stage, a thickening grease-forming and high-temperature refining stage and a post-treatment stage; monitoring the completion degree of the conversion and saponification; and by controlling the cooling speed in the grease making process, the grease with satisfactory colloid stability and mechanical stability is obtained.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
The invention discloses a method for preparing composite calcium sulfonate-based lubricating grease, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) and (3) a conversion stage: diluting high-base-number calcium sulfonate with 50 wt% of base oil, uniformly stirring the base oil and the high-base-number calcium sulfonate, heating to over 80 ℃, adding an acetic acid conversion agent diluted by 2 times of water for conversion, controlling the conversion temperature to be between 80 and 100 ℃, and controlling the conversion time to be between 50 and 70 min; transforming Newtonian high-base-number calcium sulfonate into non-Newtonian bodies by a transforming agent; the completeness of transformation is identified by the progress of the transformation of the crystalline form of calcium carbonate.
The acetic acid conversion agent is diluted by 2 times of water, and the conversion time is too high when excessive water is added; the high base number calcium sulfonate is diluted by 50 wt% of base oil, the excessive conversion time of the base oil is too long, and the excessive conversion of the base oil is too hard, so that the stirring and the subsequent reaction are not facilitated; the conversion of newtonian overbased calcium sulfonate to non-newtonian is an endothermic process that requires constant heating.
(2) And (3) saponification stage: after the conversion of the high-base-number calcium sulfonate is finished, adding the rest 50 wt% of base oil, 12-hydroxystearic acid, calcium hydroxide solution and boric acid solution, controlling the saponification temperature below 100 ℃ and the saponification time between 50min and 70 min; the calcium hydroxide solution is 10 times of calcium hydroxide solution diluted by water; the boric acid solution is 4 times of boric acid solution diluted by water; when saponification is completed, a viscous substance is formed in the refining kettle by the soap base and the base oil, and a viscous substance sample is taken from the kettle, and the content of free acid and alkali is measured to identify the completeness of saponification reaction.
The saponification process is carried out in the presence of alkali, namely fatty acid hydrolysis, so the process is required to be carried out in the presence of water, and in order to quickly and uniformly disperse the soap prepared after saponification in the base oil in the subsequent process, a certain amount of base oil is simultaneously added in the soap base manufacturing process, and the base oil plays a role in dilution in the saponification reaction; when the saponification reaction is substantially complete, the soap base and the base oil form a viscous mass in the refining kettle, and the completeness of the saponification reaction needs to be identified. The identification method comprises the following steps: taking a viscous substance sample from the kettle, rapidly determining the content of free acid and alkali, and calculating whether the free organic acid and alkali meet the default index after the finished product fat is prepared.
(3) Thickening grease and high-temperature refining: after saponification, heating the soap base in the reaction kettle to above 130 ℃, after dehydration of the soap water, heating the temperature to 160-170 ℃, keeping the temperature for 50-70 min, then compounding, and after compounding, heating the temperature to above 220 ℃ and keeping the temperature for above 3 min.
(4) And (3) post-treatment stage: and cooling the grease to obtain the final compound calcium sulfonate-based lubricating grease product.
The soap fiber shape and size generating conditions are controlled by the cooling speed in the grease manufacturing process, the soap fiber is rapidly cooled, the generated soap fiber is small, the area is large, the grease consistency is large, the oil separation is small, but the mechanical stability is poor; the soap fiber produced by slow cooling is larger, the area is small, the consistency of grease is small, the oil separation is large, and the mechanical stability is good. Therefore, in order to obtain a grease satisfactory in both colloid stability and mechanical stability, the cooling rate is strictly controlled.
Claims (5)
1. A method for preparing composite calcium sulfonate-based lubricating grease is characterized by comprising the following steps: the method comprises the following steps:
(1) and (3) a conversion stage: diluting high-base-number calcium sulfonate with 50 wt% of base oil, uniformly stirring the base oil and the high-base-number calcium sulfonate, heating to over 80 ℃, adding an acetic acid conversion agent diluted by 2 times of water for conversion, controlling the conversion temperature to be between 80 and 100 ℃, and controlling the conversion time to be between 50 and 70 min;
(2) and (3) saponification stage: after the conversion of the high-base-number calcium sulfonate is finished, adding the rest 50 wt% of base oil, 12-hydroxystearic acid, calcium hydroxide solution and boric acid solution, controlling the saponification temperature below 100 ℃ and the saponification time between 50min and 70 min;
(3) thickening grease and high-temperature refining: after saponification, heating the soap base in the reaction kettle to above 130 ℃, after dehydration of soap water, heating the temperature to 160-170 ℃, keeping the temperature for 50-70 min, then compounding, and heating to above 220 ℃ after compounding and keeping the temperature for above 3 min;
(4) and (3) post-treatment stage: and cooling the grease to obtain the final compound calcium sulfonate-based lubricating grease product.
2. The method for manufacturing the composite calcium sulfonate-based lubricating grease according to claim 1, characterized in that: in the step (1), Newtonian high-base-number calcium sulfonate is converted into non-Newtonian bodies through a conversion agent.
3. The method for manufacturing the composite calcium sulfonate-based lubricating grease according to claim 1, characterized in that: in the step (1), the completeness of the transformation is identified by the transformation progress of the crystal form of the calcium carbonate.
4. The method for manufacturing the composite calcium sulfonate-based lubricating grease according to claim 1, characterized in that: the calcium hydroxide solution in the step (2) is a calcium hydroxide solution diluted by 10 times of water; the boric acid solution is 4 times of boric acid solution diluted by water.
5. The method for manufacturing the composite calcium sulfonate-based lubricating grease according to claim 1, characterized in that: and (3) when the saponification in the step (2) is finished, forming a viscous substance in the refining kettle by the soap base and the base oil, taking a viscous substance sample from the kettle, and measuring the content of free acid and alkali so as to identify the completeness of the saponification reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911273337.9A CN110951531A (en) | 2019-12-12 | 2019-12-12 | Method for preparing composite calcium sulfonate-based lubricating grease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911273337.9A CN110951531A (en) | 2019-12-12 | 2019-12-12 | Method for preparing composite calcium sulfonate-based lubricating grease |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110951531A true CN110951531A (en) | 2020-04-03 |
Family
ID=69981262
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911273337.9A Pending CN110951531A (en) | 2019-12-12 | 2019-12-12 | Method for preparing composite calcium sulfonate-based lubricating grease |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110951531A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319164A (en) * | 2008-07-18 | 2008-12-10 | 杭州得润宝油脂有限公司 | Composite calcium sulphonic consistent grease and preparation method thereof |
| CN101824357A (en) * | 2010-05-27 | 2010-09-08 | 李墨菊 | High-performance complex calcium sulfonate grease and preparation method thereof |
| CN101921653A (en) * | 2010-09-02 | 2010-12-22 | 北京奥力助兴石化有限公司 | Synthetic high-temperature lubricating grease and preparation method thereof |
| CN102268323A (en) * | 2011-07-08 | 2011-12-07 | 苏州惠丰润滑油有限公司 | Compound calcium sulfonate based lubricating grease and preparation method thereof |
| CN102311846A (en) * | 2011-04-26 | 2012-01-11 | 东莞市安美润滑科技有限公司 | High-temperature-resistant universal extreme-pressure grease lubricant and preparation method thereof |
| CN102703185A (en) * | 2012-06-15 | 2012-10-03 | 新乡市恒星化工有限责任公司 | Compound calcium sulfonate base lubricating grease and preparation method thereof |
| CN103103012A (en) * | 2011-11-09 | 2013-05-15 | 中国石油化工股份有限公司 | Modified composite calcium sulfonate base lubricating grease and preparation method thereof |
-
2019
- 2019-12-12 CN CN201911273337.9A patent/CN110951531A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319164A (en) * | 2008-07-18 | 2008-12-10 | 杭州得润宝油脂有限公司 | Composite calcium sulphonic consistent grease and preparation method thereof |
| CN101824357A (en) * | 2010-05-27 | 2010-09-08 | 李墨菊 | High-performance complex calcium sulfonate grease and preparation method thereof |
| CN101921653A (en) * | 2010-09-02 | 2010-12-22 | 北京奥力助兴石化有限公司 | Synthetic high-temperature lubricating grease and preparation method thereof |
| CN102311846A (en) * | 2011-04-26 | 2012-01-11 | 东莞市安美润滑科技有限公司 | High-temperature-resistant universal extreme-pressure grease lubricant and preparation method thereof |
| CN102268323A (en) * | 2011-07-08 | 2011-12-07 | 苏州惠丰润滑油有限公司 | Compound calcium sulfonate based lubricating grease and preparation method thereof |
| CN103103012A (en) * | 2011-11-09 | 2013-05-15 | 中国石油化工股份有限公司 | Modified composite calcium sulfonate base lubricating grease and preparation method thereof |
| CN102703185A (en) * | 2012-06-15 | 2012-10-03 | 新乡市恒星化工有限责任公司 | Compound calcium sulfonate base lubricating grease and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱廷彬主编: "《润滑脂技术大全》", 30 April 2004, 中国石化出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792689B (en) | High-performance complex lithium-calcium base grease composition and method for preparing same | |
| CN101153239B (en) | Method for producing compound sulphonic acid albany grease | |
| RU2564020C2 (en) | Method of obtaining lubricating grease composition | |
| CN101824357A (en) | High-performance complex calcium sulfonate grease and preparation method thereof | |
| CN102977979A (en) | Composite lithium-calcium base lubricating grease and preparation method thereof | |
| CN108165356B (en) | Cotton picker spindle lubricating grease and preparation method thereof | |
| GB537615A (en) | Improved grease composition and method for making the same | |
| CN104711080B (en) | modified composite calcium sulfonate grease lubricant and preparation method thereof | |
| CN111423920A (en) | High-dropping-point high-mechanical-stability composite lithium-based grease and preparation process thereof | |
| CN103031181A (en) | Composite calcium-based lubrication grease and its preparation method | |
| CN102703185B (en) | Compound calcium sulfonate base lubricating grease and preparation method thereof | |
| CN104312665B (en) | A kind of double complex lithium grease and preparation method thereof | |
| CN110951531A (en) | Method for preparing composite calcium sulfonate-based lubricating grease | |
| CN104498131A (en) | Method for preparing lithium-based (lithium-based calcium-based) lubricating grease by using waste vegetable oil and application | |
| CN1252434A (en) | Composite lithium- and calcium-base lubricating grease and its preparation | |
| CN106701259A (en) | Shield tunneling machine shield tail lubricating grease and preparation method thereof | |
| CN107287004A (en) | A kind of efficient and environment-friendly type complex calcium sulfonate grease and preparation method thereof | |
| CN102533420A (en) | Emulsified oil for lubricating drawing of H68 brass tubes and preparation method | |
| CN101619260B (en) | Preparation method of high shear stability lithium grease | |
| CN104109568B (en) | Biodiesel is for the preparation of the application of environment-friendly metal working fluid | |
| US2188863A (en) | Grease and method of making the same | |
| CN103045323A (en) | Preparation method for environment-friendly lubricant through oxosynthesis of hexadecanoic acid methyl ester epoxy | |
| CN112410102A (en) | High-temperature lubricating grease synthesized by high polymer and preparation method thereof | |
| CN109880682B (en) | Method for preparing composite lithium-calcium grease by using waste lithium-based lubricating grease as raw material | |
| CN107955668B (en) | Special composite lithium-based lubricating grease and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | 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 |
Application publication date: 20200403 |
|
| RJ01 | Rejection of invention patent application after publication |