CN105368542A - Preparation method of modified calcium sulfonate complex grease - Google Patents
Preparation method of modified calcium sulfonate complex grease Download PDFInfo
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- CN105368542A CN105368542A CN201510865144.8A CN201510865144A CN105368542A CN 105368542 A CN105368542 A CN 105368542A CN 201510865144 A CN201510865144 A CN 201510865144A CN 105368542 A CN105368542 A CN 105368542A
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Abstract
The invention discloses a preparation method of modified calcium sulfonate complex grease, and belongs to the field of lubricant additives. Aiming at the problems at present that the appearance and color of the grease become light after the calcium sulfonate complex grease is in contact with water and the surface hardening of the grease is quickened due to nonuniform particle size distribution in the storage process of the calcium sulfonate complex grease, the invention provides the calcium sulfonate complex grease prepared by taking diatomite as basic particles, carrying out surface modification on the diatomite to improve the hydrophobicity, then taking the diatomite as a modifier to prepare modified calcium sulfonate with high base number in the preparation process of adding the calcium sulfonate with high base number and then taking the modified calcium sulfonate with high base number and the particles as raw materials, so that the calcium sulfonate complex grease with uniform particle size distribution and high hydrophobicity is obtained.
Description
Technical field
The invention discloses a kind of preparation method of improved Calcium Sulfonate Complex Lubricating Grease, belong to lubricating oil additive field.
Background technology
Calcium sulphonate is commonly used for sanitising agent and the rust-preventive agent of lubricating oil, there is the calcium sulfonate grease of the high dropping point using calcium sulphonate as viscosifying agent the 1950's, but the solution thickened ability of oil soluble newton body calcium sulphonate now used is little, can only use with less ratio together with traditional fatty acid soaps viscosifying agent.To the sixties, people by newton's body calcium sulphonate solution transition for having thixotropic non-newtonian fluid calcium sulphonate, and the height alkalization technology introducing calcium sulphonate in the preparation process of calcium sulfonate grease has prepared overbasic calcium sulfonate grease, its dropping point is more than 300 DEG C, cylinder stability, at 1 ~ 2 unit, has good shear stability, but suitable thickness, low temperature pumpmg quality is very poor, hampers it and applies further.The mid-80, non newtonian sulfonic acid calcium soap and other soap compounds is adopted to prepare complex calcium sulfonate grease, its low temperature pumpmg quality is not only made to improve, there is excellent high temperature performance, mechanical stability, colloid stability and oxidation stability simultaneously, be called as " high-efficiency lubricating fat of new generation ".
The production technique of calcium sulfonate grease finalizes the design almost, the calcium sulfonate grease excellent property of production, and indices is all good, but after it contacts with large water gaging, in fat, water content is higher, and the appearance color of fat is shoaled.Complex calcium sulfonate grease is in storage process, and because size distribution is uneven, can there is the trend that particle phase total surface area reduces, small-particle is consumed gradually, and macroparticle is grown up gradually, thus accelerates the surface hardening phenomenon of this type of lubricating grease.
Summary of the invention
The technical problem that the present invention mainly solves: for current calcium sulfonate grease after contact with water, the appearance color of fat can be made to shoal, calcium sulfonate grease is in storage process simultaneously, due to the problem that size distribution inequality can make the surface hardening of lubricating grease accelerate, the invention provides a kind of is basic granules with diatomite, surface modification is carried out to it, increase hydrophobicity, it can be used as properties-correcting agent again, add in the preparation process of calcium sulfonate with high base number, obtained modification calcium sulfonate with high base number, again modification calcium sulfonate with high base number and particle are prepared calcium sulfonate grease as raw material, thus obtain even particle size distribution, the complex calcium sulfonate grease that hydrophobicity is high.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) get 300 ~ 600g diatomite and put into retort furnace, set temperature is 900 ~ 1100 DEG C, keep temperature 40 ~ 70min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 100 ~ 120 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 20 ~ 30g sucrose fatty ester and 60 ~ 90g calcium chloride, use carbonic acid gas to seal container;
(2) after above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 120 ~ 130 DEG C, with rotating speed for 150 ~ 180r/min, after stirring 30 ~ 50min, container being placed in frequency is under the environment of 10 ~ 15KHz, leave standstill 10 ~ 15min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use;
(3) by quality hundred parts of ratios, 40 ~ 50 parts of heavy alkylbenzene sulfonic acids are got, 27 ~ 30 parts of calcium hydroxides, 18 ~ 20 parts of calcium oxide and 5 ~ 10 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 60 ~ 70 DEG C, with rotating speed 160 ~ 180r/min, after stirring reaction 2 ~ 5h, naturally cool to room temperature, leave standstill 10 ~ 15min;
(4) after above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 50 ~ 60mL/min, aeration time 30 ~ 45min, after ventilation terminates, adds sodium acetate in container, add-on is 20 ~ 40% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 50 ~ 70 DEG C, stirs 1 ~ 3h;
(5) filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 40 ~ 45 parts of above-mentioned obtained modification calcium sulfonate with high base number, 30 ~ 40 parts of base oils, 5 ~ 10 part of 200 order calcium carbonate, 0.5 ~ 1 part of antioxidant di-tertiary butyl methyl phenol, the particulate matter obtained by 2 ~ 4 parts, 1 ~ 1.5 part of polyoxyethylene glycol, the Glacial acetic acid of 1.5 ~ 2 parts, 2 ~ 3 parts of dehydrated alcohols;
(6) by above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, carbonic acid gas is used to be discharged by the air in reactor, temperature is set as 60 ~ 70 DEG C, speed setting is 160 ~ 180r/min, stir 20 ~ 30min, in whipping process, dehydrated alcohol is added in reactor;
(7) after above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 150 ~ 160 DEG C, speed setting is 200 ~ 300r/min, stirs until transform completely, then keeps temperature 30 ~ 50min, be cooled to 50 ~ 80 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
Application method of the present invention is: by grease made for the present invention and water by volume 3:1 mix, leave standstill after 5 ~ 15 days, observe its appearance color not to be any change, there is not obvious surface hardening phenomenon in grease surface, reduces 50 ~ 62% than the surface hardening speed of traditional calcium sulfonate grease.
The invention has the beneficial effects as follows:
(1) the improved Calcium Sulfonate Complex Lubricating Grease even particle size distribution that the present invention is made;
(2) production cost of the present invention is low, produces non-environmental-pollution in the process of improved Calcium Sulfonate Complex Lubricating Grease.
Embodiment
Get 300 ~ 600g diatomite and put into retort furnace, set temperature is 900 ~ 1100 DEG C, keep temperature 40 ~ 70min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 100 ~ 120 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 20 ~ 30g sucrose fatty ester and 60 ~ 90g calcium chloride, use carbonic acid gas to seal container; After above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 120 ~ 130 DEG C, with rotating speed for 150 ~ 180r/min, after stirring 30 ~ 50min, container being placed in frequency is under the environment of 10 ~ 15KHz, leave standstill 10 ~ 15min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use; By quality hundred parts of ratios, get 40 ~ 50 parts of heavy alkylbenzene sulfonic acids, 27 ~ 30 parts of calcium hydroxides, 18 ~ 20 parts of calcium oxide and 5 ~ 10 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 60 ~ 70 DEG C, with rotating speed 160 ~ 180r/min, after stirring reaction 2 ~ 5h, naturally cool to room temperature, leave standstill 10 ~ 15min; After above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 50 ~ 60mL/min, aeration time 30 ~ 45min, after ventilation terminates, adds sodium acetate in container, add-on is 20 ~ 40% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 50 ~ 70 DEG C, stirs 1 ~ 3h; Filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 40 ~ 45 parts of above-mentioned obtained modification calcium sulfonate with high base number, 30 ~ 40 parts of base oils, 5 ~ 10 part of 200 order calcium carbonate, the antioxidant di-tertiary butyl methyl phenol of 0.5 ~ 1 part, the particulate matter obtained by 2 ~ 4 parts, 1 ~ 1.5 part of polyoxyethylene glycol, the Glacial acetic acid of 1.5 ~ 2 parts, 2 ~ 3 parts of dehydrated alcohols; By above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, carbonic acid gas is used to be discharged by the air in reactor, temperature is set as 60 ~ 70 DEG C, speed setting is 160 ~ 180r/min, stir 20 ~ 30min, in whipping process, dehydrated alcohol is added in reactor; After above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 150 ~ 160 DEG C, speed setting is 200 ~ 300r/min, stirs until transform completely, then keeps temperature 30 ~ 50min, be cooled to 50 ~ 80 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
Example 1
Get 300g diatomite and put into retort furnace, set temperature is 900 DEG C, keep temperature 40min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 100 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 20g sucrose fatty ester and 60g calcium chloride, use carbonic acid gas to seal container; After above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 120 DEG C, take rotating speed as 150r/min, after stirring 30min, container being placed in frequency is under the environment of 10KHz, leave standstill 10min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use; By quality hundred parts of ratios, get 40 parts of heavy alkylbenzene sulfonic acids, 30 parts of calcium hydroxides, 20 parts of calcium oxide and 10 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 60 DEG C, with rotating speed 160r/min, after stirring reaction 2h, naturally cool to room temperature, leave standstill 10min; After above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 60mL/min, aeration time 30min, after ventilation terminates, in container, add sodium acetate, add-on is 20% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 50 DEG C, stirs 1h; Filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 40 parts of above-mentioned obtained modification calcium sulfonate with high base number, 40 parts of base oils, 10 part of 200 order calcium carbonate, the antioxidant di-tertiary butyl methyl phenol of 1 part, the particulate matter obtained by 4 parts, 1.5 parts of polyoxyethylene glycol, the Glacial acetic acid of 2 parts, 3 parts of dehydrated alcohols; By above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, use carbonic acid gas to be discharged by the air in reactor, temperature is set as 60 DEG C, speed setting is 160r/min, stirs 20min, adds in reactor in whipping process by dehydrated alcohol; After above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 150 DEG C, speed setting is 200r/min, stirs until transform completely, then keeps temperature 30min, be cooled to 50 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
By grease made for the present invention and water by volume 3:1 mix, leave standstill after 5 days, observing its appearance color and be not any change, there is not obvious surface hardening phenomenon in grease surface, reduces 50% than the surface hardening speed of traditional calcium sulfonate grease.
Example 2
Get 600g diatomite and put into retort furnace, set temperature is 1100 DEG C, keep temperature 70min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 120 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 30g sucrose fatty ester and 90g calcium chloride, use carbonic acid gas to seal container; After above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 130 DEG C, take rotating speed as 180r/min, after stirring 40min, container being placed in frequency is under the environment of 15KHz, leave standstill 15min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use; By quality hundred parts of ratios, get 50 parts of heavy alkylbenzene sulfonic acids, 27 parts of calcium hydroxides, 18 parts of calcium oxide and 5 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 70 DEG C, with rotating speed 180r/min, after stirring reaction 5h, naturally cool to room temperature, leave standstill 15min; After above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 60mL/min, aeration time 45min, after ventilation terminates, adds sodium acetate in container, add-on is 40% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 50 ~ 70 DEG C, stirs 3h; Filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 45 parts of above-mentioned obtained modification calcium sulfonate with high base number, 30 parts of base oils, 5 part of 200 order calcium carbonate, the antioxidant di-tertiary butyl methyl phenol of 0.5 part, the particulate matter obtained by 2 parts, 1 part of polyoxyethylene glycol, the Glacial acetic acid of 1.5 parts, 2 parts of dehydrated alcohols; By above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, use carbonic acid gas to be discharged by the air in reactor, temperature is set as 70 DEG C, speed setting is 180r/min, stirs 30min, adds in reactor in whipping process by dehydrated alcohol; After above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 160 DEG C, speed setting is 300r/min, stirs until transform completely, then keeps temperature 50min, be cooled to 80 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
By grease made for the present invention and water by volume 3:1 mix, leave standstill after 15 days, observing its appearance color and be not any change, there is not obvious surface hardening phenomenon in grease surface, reduces 62% than the surface hardening speed of traditional calcium sulfonate grease.
Example 3
Get 500g diatomite and put into retort furnace, set temperature is 950 DEG C, keep temperature 50min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 110 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 25g sucrose fatty ester and 70g calcium chloride, use carbonic acid gas to seal container; After above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 125 DEG C, take rotating speed as 170r/min, after stirring 40min, container being placed in frequency is under the environment of 12KHz, leave standstill 12min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use; By quality hundred parts of ratios, get 45 parts of heavy alkylbenzene sulfonic acids, 28 parts of calcium hydroxides, 20 parts of calcium oxide and 8 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 65 DEG C, with rotating speed 170r/min, after stirring reaction 3h, naturally cool to room temperature, leave standstill 12min; After above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 55mL/min, aeration time 40min, after ventilation terminates, in container, add sodium acetate, add-on is 30% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 60 DEG C, stirs 2h; Filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 44 parts of above-mentioned obtained modification calcium sulfonate with high base number, 37 parts of base oils, 9 part of 200 order calcium carbonate, the antioxidant di-tertiary butyl methyl phenol of 1 part, the particulate matter obtained by 4 parts, 1 part of polyoxyethylene glycol, the Glacial acetic acid of 2 parts, 2 parts of dehydrated alcohols; By above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, use carbonic acid gas to be discharged by the air in reactor, temperature is set as 65 DEG C, speed setting is 170r/min, stirs 25min, adds in reactor in whipping process by dehydrated alcohol; After above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 155 DEG C, speed setting is 250r/min, stirs until transform completely, then keeps temperature 40min, be cooled to 70 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
By grease made for the present invention and water by volume 3:1 mix, leave standstill after 10 days, observing its appearance color and be not any change, there is not obvious surface hardening phenomenon in grease surface, reduces 58% than the surface hardening speed of traditional calcium sulfonate grease.
Claims (1)
1. a preparation method for improved Calcium Sulfonate Complex Lubricating Grease, is characterized in that concrete preparation process is:
(1) get 300 ~ 600g diatomite and put into retort furnace, set temperature is 900 ~ 1100 DEG C, keep temperature 40 ~ 70min, then be cooled to room temperature, taken out and put into pulverizer and pulverize, sieve to obtain 100 ~ 120 order particles, gained particle is put into container, add the hydrochloric acid soln immersion particulate matter that massfraction is 45% wherein, then respectively to wherein adding 20 ~ 30g sucrose fatty ester and 60 ~ 90g calcium chloride, use carbonic acid gas to seal container;
(2) after above-mentioned sealing, heated and stirred is carried out to container, temperature is set as 120 ~ 130 DEG C, with rotating speed for 150 ~ 180r/min, after stirring 30 ~ 50min, container being placed in frequency is under the environment of 10 ~ 15KHz, leave standstill 10 ~ 15min, then filter, the filtrate of gained is put into air dryer and carries out air-dry, collect air-dry after particulate matter, for subsequent use;
(3) by quality hundred parts of ratios, 40 ~ 50 parts of heavy alkylbenzene sulfonic acids are got, 27 ~ 30 parts of calcium hydroxides, 18 ~ 20 parts of calcium oxide and 5 ~ 10 parts above-mentioned air-dry after particulate matter, put into container, add the methyl alcohol immersion mixture that massfraction is 80% wherein, stir, then container is heated, temperature is set as 60 ~ 70 DEG C, with rotating speed 160 ~ 180r/min, after stirring reaction 2 ~ 5h, naturally cool to room temperature, leave standstill 10 ~ 15min;
(4) after above-mentioned standing end, pass into carbonic acid gas wherein, passing into speed is 50 ~ 60mL/min, aeration time 30 ~ 45min, after ventilation terminates, adds sodium acetate in container, add-on is 20 ~ 40% of heavy alkylbenzene sulfonic acid quality, then heat container, being heated to temperature is 50 ~ 70 DEG C, stirs 1 ~ 3h;
(5) filtered while hot after above-mentioned stirring terminates, puts into whizzer by the filtered liquid of gained and carries out centrifugation, collects supernatant liquor, obtain modification calcium sulfonate with high base number, by quality hundred parts of ratios, get 42 ~ 45 parts of above-mentioned obtained modification calcium sulfonate with high base number, 37 ~ 40 parts of base oils, 8 ~ 10 part of 200 order calcium carbonate, 0.5 ~ 1 part of antioxidant di-tertiary butyl methyl phenol, the particulate matter obtained by 2.5 ~ 4 parts, 1 ~ 1.5 part of polyoxyethylene glycol, the Glacial acetic acid of 1.5 ~ 2 parts, 2 ~ 3 parts of dehydrated alcohols;
(6) by above-mentioned mass fraction, base oil, modification calcium sulfonate with high base number and calcium carbonate are put into reactor, carbonic acid gas is used to be discharged by the air in reactor, temperature is set as 60 ~ 70 DEG C, speed setting is 160 ~ 180r/min, stir 20 ~ 30min, in whipping process, dehydrated alcohol is added in reactor;
(7) after above-mentioned stirring terminates, in container, add obtained particulate matter, Glacial acetic acid and polyoxyethylene glycol, stir, be warming up to 150 ~ 160 DEG C, speed setting is 200 ~ 300r/min, stirs until transform completely, then keeps temperature 30 ~ 50min, be cooled to 50 ~ 80 DEG C subsequently, add antioxidant di-tertiary butyl methyl phenol wherein, after stirring, naturally cool to room temperature discharging, by the discharging thing of gained after filtration, degassedly improved Calcium Sulfonate Complex Lubricating Grease can be obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510865144.8A CN105368542A (en) | 2015-12-01 | 2015-12-01 | Preparation method of modified calcium sulfonate complex grease |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510865144.8A CN105368542A (en) | 2015-12-01 | 2015-12-01 | Preparation method of modified calcium sulfonate complex grease |
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| CN105368542A true CN105368542A (en) | 2016-03-02 |
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| CN201510865144.8A Withdrawn CN105368542A (en) | 2015-12-01 | 2015-12-01 | Preparation method of modified calcium sulfonate complex grease |
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Application publication date: 20160302 |