CN107201260A - A kind of preparation method of detergent for lubricating oil - Google Patents
A kind of preparation method of detergent for lubricating oil Download PDFInfo
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- CN107201260A CN107201260A CN201710337083.7A CN201710337083A CN107201260A CN 107201260 A CN107201260 A CN 107201260A CN 201710337083 A CN201710337083 A CN 201710337083A CN 107201260 A CN107201260 A CN 107201260A
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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
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
-
- 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
- C10M167/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound, a non-macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
-
- 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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- 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
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
-
- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/10—Amides of carbonic or haloformic acids
- C10M2215/102—Ureas; Semicarbazides; Allophanates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/02—Pour-point; Viscosity index
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/52—Base number [TBN]
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/64—Environmental friendly compositions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/72—Extended drain
-
- 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
- C10N2040/25—Internal-combustion engines
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a kind of preparation method of detergent for lubricating oil, belong to lube oil additive preparing technical field.The present invention first crushes attapulgite, dry and mixed after calcining with octadecylene, the reaction of salicylic acid ethanol solution is added dropwise, obtain attapulgite modified with dispersant after the hole and Surface Creation alkyl sodium salicylate of attapulgite, by itself and methanol, ammoniacal liquor, guar gum etc. reacts, gas is passed through again carries out carbonation reaction, filter residue and drying then is collected by filtration, crush to obtain detergent for lubricating oil, the present invention is matrix using attapulgite, the stable suspension not destroyed by electrolyte can be formed, its surface is modified that detergent for lubricating oil is added in lubricating oil, play and preferably disperse peace and quiet effect, and detersive of the present invention is after pollutant during adsorpting lubrication is oily, energy stable suspersion is in lubricating oil, it is not in depositional phenomenon, the secondary pollution of part and lubricating oil is not resulted in thus, have broad application prospects.
Description
Technical field
The invention discloses a kind of preparation method of detergent for lubricating oil, belong to lube oil additive preparing technical field.
Background technology
Detersive is the main additive of I. C. engine oil, is a kind of material with surface-active, it have base number it is high,
The characteristic that rust-preventing characteristic is good, acid neutralization capacity is strong, is mainly used in modulating medium-to-high grade I. C. engine oil.In detersive energy adsorpting lubrication oil
Solid grain contamination, and make pollutant be suspended in the surface of lubricating oil, with ensure the oil for participating in greasing cycle be it is peace and quiet, with
The formation of high temperature and paint film is reduced, so that the insoluble matter such as jelly, carbon deposit that lubricating oil is generated after being oxidized or outstanding
Float in oil, form stable colloidal state and be difficult to be deposited on part, or the glue that will be deposited on engine components
Shape thing, carbon deposit etc., by lubricating oil cleaning function in washing.Because above-mentioned substance can play a part of dispersant simultaneously,
Therefore using the detersive also known as detergent-dispersant additive of above-mentioned substance.
At present, conventional detergent for lubricating oil mainly has traditional lubrication such as sulfonate, naphthenate, alkylbenzenesulfonate
Oily detersive product.Jelly or carbon distribution that these detersives are generated after the solid grain contamination in adsorpting lubrication oil etc. are no
What molten thing can not be stablized is suspended in lubricating oil, can be deposited on part, make cheek and lubricating oil secondary pollution.Thus,
Exploitation meet environmental requirement, stable suspersion, detergent for lubricating oil that peace and quiet effect is good will be following developing direction.
The content of the invention
Present invention mainly solves technical problem：For solid particle of the oily detersive of conventional lubrication in adsorpting lubrication oil
What the insoluble matters such as the jelly or carbon distribution that are generated after pollutant can not be stablized is suspended in lubricating oil, can be deposited on part, make
There is provided a kind of preparation method of detergent for lubricating oil for cheek and the defect of lubricating oil secondary pollution.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh attapulgite and add crushing in pulverizer, attapulgite powder is obtained after sieving, is put into baking oven and dries, will be dry
Attapulgite powder after dry is placed in crucible, and crucible is put into Muffle furnace, under nitrogen atmosphere protection, is calcined,
Attapulgite powder after room temperature is cooled to after calcining must calcining；
（2）In mass ratio 1:5 mix the attapulgite powder after calcining with octadecylene, be added dropwise after stirring octadecylene quality 60~
65% salicylic acid ethanol solution, is heated after completion of dropwise addition, be subsequently added the mass fraction of octadecylene quality 3~5% for 5% calcium chloride and
The polyvinylpyrrolidone of octadecylene quality 3~5%, is stirred after reaction, reaction under nitrogen atmosphere protection and is cooled to room temperature and goes out
Material, obtains and is filtered after reactant, removes and obtains attapulgite modified after filtrate；
（3）Count by weight, 15~20 parts of attapulgite modified, 50~70 parts of toluene, 20~25 parts of methanol, 8 are weighed respectively
~12 parts of ammoniacal liquor, 10~15 parts of magnesia and 15~20 parts of deionized waters, are warming up to 70~80 DEG C after mixing, and stirring reaction 2~
Reduced after 4h temperature to 40~50 DEG C reactant, and sequentially add urea, guar gum C14S and deionized water, insulated and stirred；
（4）After end to be mixed, nitrogen is passed through, is passed through after 2~4min and stops being passed through nitrogen, then change into and be passed through carbon dioxide gas
Body, is passed through after 2~3h and stops being passed through carbon dioxide, filter, be put into after collecting filter residue in baking oven, crushed after being dried, sieving,
Collect powder, you can obtain a kind of detergent for lubricating oil.
Step（1）Described in calcining heat be 500~600 DEG C, calcination time be 20~30min.
Step（2）Described in salicylic acid ethanol solution mass fraction be 10%.
Step（2）Described in heating-up temperature be 60~80 DEG C, time of stirring reaction is 2~3h.
Step（3）Described in ammoniacal liquor mass fraction be 15%.
Step（3）Described in urea quality be reactant quality 1~3%, guar gum C14S mass be reactant quality 2
~4%, deionized water quality is reactant quality 10~15%.
The beneficial effects of the invention are as follows：
（1）The present invention first crushes attapulgite, dry after calcined, the attapulgite powder after must calcining is last and octadecylene
Mix and the reaction of salicylic acid ethanol solution is added dropwise, with dispersant after the hole and Surface Creation alkyl sodium salicylate of attapulgite
Mix attapulgite modified, due to load alkyl sodium salicylate in modified attapulgite, due to alkyl sodium salicylate sheet
Body is main metal detergent product, with excellent heat resistance, high temperature detergency, good acid neutralization capacity, load
It can allow what particle stablized to be suspended in oil phase after attapulgite, and be difficult to be polymerized to bulky grain and produce precipitation, thus
The problem of detergent for lubricating oil is unstable in lubricating oil can be solved with stable for extended periods of time；
（2）The reaction such as attapulgite modified and methanol, ammoniacal liquor is added the stirring such as urea, guar gum by the present invention, in stirring knot
Carbon dioxide is passed through after beam and carries out carbonation reaction, filter residue and drying is then collected by filtration, detergent for lubricating oil is crushed to obtain, this
Invention, which is added after ammoniacal liquor, to occur neutralization reaction with organic acid, so as to improve the base number of detergent for lubricating oil so that made
Standby detergent for lubricating oil, with minimum and more uniform colloid carbonate dispersive property, viscosity is low, with preferably peace and quiet
Dispersiveness and the ability for neutralizing corrosive acid, and the present invention can be uniformly dispersed in lubricating oil, plays a part of cleaning lubricating oil, has
Effect extends Working Life of Lubricating Oil.
Embodiment
Weigh 15~20g attapulgites and add crushing in pulverizer, cross 100~120 mesh sieves and obtain attapulgite powder, will be recessed
The native powder of convex rod is put into baking oven, and 6~8h is dried under the conditions of 80~100 DEG C, dried attapulgite powder is placed in into earthenware
In crucible, and crucible is put into Muffle furnace, under nitrogen atmosphere protection, 500 are warming up to 8~10 DEG C/min heating rates~
600 DEG C, insulation 20~30min of calcining is cooled to the attapulgite powder after room temperature must be calcined, in mass ratio 1 after calcining:5 will
Attapulgite powder after calcining is fitted into four-hole boiling flask after being mixed with octadecylene, is stirred with 400~500r/min rotating speed
20~30min is mixed, the salicylic acid ethanol solution of mass fraction 10% of octadecylene quality 60~65% is added dropwise after stirring, speed is added dropwise in control
Rate is 1~2g/min, is stirred, four-hole boiling flask is put into water-bath while dropwise addition after completion of dropwise addition, it is warming up to 60~
The mass fraction of octadecylene quality 3~5% is added after 80 DEG C for 5% calcium chloride and the polyvinylpyrrolidone of octadecylene quality 3~5%, and
Nitrogen is passed through into four-hole boiling flask, speed is passed through for 6~8mL/min, insulated and stirred is reacted to be stopped being passed through nitrogen and cold after 3~5h
But discharged to room temperature, obtain and filtered after reactant, removed and obtain attapulgite modified after filtrate, count by weight, 15 are weighed respectively
~20 parts attapulgite modified, 50~70 parts of toluene, 20~25 parts of methanol, 8~12 parts of ammoniacal liquor of mass fraction 15%, 10~15 parts
Magnesia and 15~20 parts of deionized waters, are warming up to 2~4h of stirring reaction after 70~80 DEG C after mixing, reaction reduces temperature after terminating
Degree to 40~50 DEG C reactant, and sequentially add into three-necked flask the urea of reactant quality 1~3%, reactant quality 2~
4% guar gum C14S and the deionized water of reactant quality 10~15%, continue 1~2h of insulated and stirred, after end to be mixed, Xiang Sankou
Nitrogen is passed through in flask, speed is passed through for 10~15mL/min, is passed through after 2~4min and stops being passed through nitrogen, and continue to be passed through two
Carbon oxide gas, are passed through speed for 20~30mL/min, are passed through after 2~3h and stop being passed through carbon dioxide, filter, collect filter
It is put into after slag in baking oven, 6~8h is dried at a temperature of 40~50 DEG C, crushed after being dried crosses 600~620 mesh sieves, collects powder,
It can obtain a kind of detergent for lubricating oil.
Example 1
Weigh 15g attapulgites and add crushing in pulverizer, cross 100 mesh sieves and obtain attapulgite powder, attapulgite powder is put
Enter in baking oven, 6h is dried under the conditions of 80 DEG C, dried attapulgite powder is placed in crucible, and crucible is put into Muffle
In stove, under nitrogen atmosphere protection, 500 DEG C are warming up to 8 DEG C/min heating rates, insulation calcining 20min is cooled to after calcining
Room temperature must calcine after attapulgite powder, in mass ratio 1:5 the attapulgite powder after calcining is mixed with octadecylene after fill
Enter in four-hole boiling flask, 20min is stirred with 400r/min rotating speed, the mass fraction of octadecylene quality 60% is added dropwise after stirring
10% salicylic acid ethanol solution, it is 1g/min to control drop rate, is stirred while dropwise addition, by four mouthfuls of burnings after completion of dropwise addition
Bottle is put into water-bath, and it is that 5% calcium chloride and octadecylene quality 3% are poly- to be warming up to after 60 DEG C and add the mass fraction of octadecylene quality 3%
Vinylpyrrolidone, and nitrogen is passed through into four-hole boiling flask, speed is passed through for 6mL/min, is stopped after insulated and stirred reaction 3h logical
Enter nitrogen and be cooled to room temperature discharging, obtain and filtered after reactant, remove and obtain attapulgite modified after filtrate, count by weight,
15 parts of attapulgite modified, 50 parts of toluene, 20 parts of methanol, 8 parts of ammoniacal liquor of mass fraction 15%, 10 parts of magnesia and 15 are weighed respectively
Part deionized water, is warming up to stirring reaction 2h after 70 DEG C after mixing, after reaction terminates reduction temperature to 40 DEG C reactant, and to
Sequentially added in three-necked flask the urea of reactant quality 1%, the guar gum C14S of reactant quality 2% and reactant quality 10% go from
Sub- water, continues insulated and stirred 1h, after end to be mixed, nitrogen is passed through into three-necked flask, is passed through speed for 10mL/min, is passed through
Stop being passed through nitrogen after 2min, and continue to be passed through carbon dioxide, be passed through speed for 20mL/min, be passed through after 2h and stop being passed through
Carbon dioxide, filtering is put into baking oven after collecting filter residue, and 6h is dried at a temperature of 40 DEG C, and crushed after being dried crosses 600 mesh
Sieve, collects powder, you can obtain a kind of detergent for lubricating oil.
First in mass ratio 1:50, by detergent for lubricating oil produced by the present invention and auto lubrication oil base oil 40 DEG C,
10min is mixed under the conditions of 80r/min, lubricating composition is obtained, then takes 2L lubricant oil composites funnel to load automobile engine
In the oil sump of oil tank, it is to be added after the completion of, start engine operating 5min, it is ensured that can run automobile without oil leakage phenomenon.
After testing, the base number of detergent for lubricating oil detersive produced by the present invention is 310mgKOH/g, and 100 DEG C of kinematic viscosity are 15mm2/
S, while detersive heat endurance of the present invention and high temperature detergency are preferably, initial pyrolyzation temperature is 220 DEG C, and the present invention is made
Detersive there is preferable suspension stability, pollutant and stable suspersion in lubricating oil, can make effectively in adsorpting lubrication oil
Working Life of Lubricating Oil is extended 4 months compared with conventional lubrication oil, so as to play a part of guard block, in addition, the present invention is peace and quiet
Preferably, the discarded object discharged after use can voluntarily be degraded agent biodegradability in 24 months, and environment will not be polluted.
Example 2
Weigh 18g attapulgites and add crushing in pulverizer, cross 110 mesh sieves and obtain attapulgite powder, attapulgite powder is put
Enter in baking oven, 7h is dried under the conditions of 90 DEG C, dried attapulgite powder is placed in crucible, and crucible is put into Muffle
In stove, under nitrogen atmosphere protection, 550 DEG C are warming up to 9 DEG C/min heating rates, insulation calcining 25min is cooled to after calcining
Room temperature must calcine after attapulgite powder, in mass ratio 1:5 the attapulgite powder after calcining is mixed with octadecylene after fill
Enter in four-hole boiling flask, 25min is stirred with 450r/min rotating speed, the mass fraction of octadecylene quality 63% is added dropwise after stirring
10% salicylic acid ethanol solution, it is 1g/min to control drop rate, is stirred while dropwise addition, by four mouthfuls of burnings after completion of dropwise addition
Bottle is put into water-bath, and it is that 5% calcium chloride and octadecylene quality 4% are poly- to be warming up to after 70 DEG C and add the mass fraction of octadecylene quality 4%
Vinylpyrrolidone, and nitrogen is passed through into four-hole boiling flask, speed is passed through for 7mL/min, is stopped after insulated and stirred reaction 4h logical
Enter nitrogen and be cooled to room temperature discharging, obtain and filtered after reactant, remove and obtain attapulgite modified after filtrate, count by weight,
18 parts of attapulgite modified, 60 parts of toluene, 23 parts of methanol, 10 parts of ammoniacal liquor of mass fraction 15%, 13 parts of magnesia and 18 are weighed respectively
Part deionized water, is warming up to stirring reaction 3h after 75 DEG C after mixing, after reaction terminates reduction temperature to 45 DEG C reactant, and to
Sequentially added in three-necked flask the urea of reactant quality 2%, the guar gum C14S of reactant quality 3% and reactant quality 13% go from
Sub- water, continues insulated and stirred 1h, after end to be mixed, nitrogen is passed through into three-necked flask, is passed through speed for 13mL/min, is passed through
Stop being passed through nitrogen after 3min, and continue to be passed through carbon dioxide, be passed through speed for 25mL/min, be passed through after 2h and stop being passed through
Carbon dioxide, filtering is put into baking oven after collecting filter residue, and 7h is dried at a temperature of 45 DEG C, and crushed after being dried crosses 610 mesh
Sieve, collects powder, you can obtain a kind of detergent for lubricating oil.
First in mass ratio 1:55, by detergent for lubricating oil produced by the present invention and auto lubrication oil base oil 45 DEG C,
13min is mixed under the conditions of 85r/min, lubricating composition is obtained, then takes 3L lubricant oil composites funnel to load automobile engine
In the oil sump of oil tank, it is to be added after the completion of, start engine operating 7min, it is ensured that can run automobile without oil leakage phenomenon.
After testing, the base number of detergent for lubricating oil detersive produced by the present invention is 335mgKOH/g, and 100 DEG C of kinematic viscosity are 20mm2/
S, while detersive heat endurance of the present invention and high temperature detergency are preferably, initial pyrolyzation temperature is 225 DEG C, and the present invention is made
Detersive there is preferable suspension stability, pollutant and stable suspersion in lubricating oil, can make effectively in adsorpting lubrication oil
Working Life of Lubricating Oil is extended 5 months compared with conventional lubrication oil, so as to play a part of guard block, in addition, the present invention is peace and quiet
Preferably, the discarded object discharged after use can voluntarily be degraded agent biodegradability in 30 months, and environment will not be polluted.
Example 3
Weigh 20g attapulgites and add crushing in pulverizer, cross 120 mesh sieves and obtain attapulgite powder, attapulgite powder is put
Enter in baking oven, 8h is dried under the conditions of 100 DEG C, dried attapulgite powder is placed in crucible, and crucible is put into horse
Not in stove, under nitrogen atmosphere protection, 600 DEG C are warming up to 10 DEG C/min heating rates, 30min is calcined in insulation, cold after calcining
But the attapulgite powder after must being calcined to room temperature, in mass ratio 1:5 mix the attapulgite powder after calcining with octadecylene
It is fitted into afterwards in four-hole boiling flask, 30min is stirred with 500r/min rotating speed, the quality of octadecylene quality 65% is added dropwise after stirring
The salicylic acid ethanol solution of fraction 10%, it is 2g/min to control drop rate, is stirred while dropwise addition, by four after completion of dropwise addition
Mouth flask is put into water-bath, and it is 5% calcium chloride and octadecylene quality to be warming up to after 80 DEG C and add the mass fraction of octadecylene quality 5%
5% polyvinylpyrrolidone, and nitrogen is passed through into four-hole boiling flask, speed is passed through for 8mL/min, is stopped after insulated and stirred reaction 5h
Only it is passed through nitrogen and is cooled to room temperature discharging, obtains and filtered after reactant, remove and obtain attapulgite modified after filtrate, by weight
Meter, weighs 20 parts of attapulgite modified, 70 parts of toluene, 25 parts of methanol, 12 parts of ammoniacal liquor of mass fraction 15%, 15 parts of magnesia respectively
With 20 parts of deionized waters, be warming up to stirring reaction 4h after 80 DEG C after mixing, after reaction terminates reduction temperature to 50 DEG C reactant,
And the urea of reactant quality 3%, the guar gum C14S of reactant quality 4% and reactant quality 15% are sequentially added into three-necked flask
Deionized water, continues insulated and stirred 2h, after end to be mixed, nitrogen is passed through into three-necked flask, is passed through speed for 15mL/min,
It is passed through after 4min and stops being passed through nitrogen, and continue to be passed through carbon dioxide, be passed through speed for 30mL/min, is passed through after 3h and stops
Carbon dioxide is passed through, is filtered, is put into after collecting filter residue in baking oven, 8h, crushed after being dried, mistake are dried at a temperature of 50 DEG C
620 mesh sieves, collect powder, you can obtain a kind of detergent for lubricating oil.
First in mass ratio 1:60, by detergent for lubricating oil produced by the present invention and auto lubrication oil base oil 50 DEG C,
15min is mixed under the conditions of 90r/min, lubricating composition is obtained, then takes 4L lubricant oil composites funnel to load automobile engine
In the oil sump of oil tank, it is to be added after the completion of, start engine operating 8min, it is ensured that can run automobile without oil leakage phenomenon.
After testing, the base number of detergent for lubricating oil detersive produced by the present invention is 360mgKOH/g, and 100 DEG C of kinematic viscosity are 25mm2/
S, while detersive heat endurance of the present invention and high temperature detergency are preferably, initial pyrolyzation temperature is 230 DEG C, and the present invention is made
Detersive there is preferable suspension stability, pollutant and stable suspersion in lubricating oil, can make effectively in adsorpting lubrication oil
Working Life of Lubricating Oil is extended 6 months compared with conventional lubrication oil, so as to play a part of guard block, in addition, the present invention is peace and quiet
Preferably, the discarded object discharged after use can voluntarily be degraded agent biodegradability in 36 months, and environment will not be polluted.
Claims (6)
1. a kind of preparation method of detergent for lubricating oil, it is characterised in that specifically preparation process is：
（1）Weigh attapulgite and add crushing in pulverizer, attapulgite powder is obtained after sieving, is put into baking oven and dries, will be dry
Attapulgite powder after dry is placed in crucible, and crucible is put into Muffle furnace, under nitrogen atmosphere protection, is calcined,
Attapulgite powder after room temperature is cooled to after calcining must calcining；
（2）In mass ratio 1:5 mix the attapulgite powder after calcining with octadecylene, be added dropwise after stirring octadecylene quality 60~
65% salicylic acid ethanol solution, is heated after completion of dropwise addition, be subsequently added the mass fraction of octadecylene quality 3~5% for 5% calcium chloride and
The polyvinylpyrrolidone of octadecylene quality 3~5%, is stirred after reaction, reaction under nitrogen atmosphere protection and is cooled to room temperature and goes out
Material, obtains and is filtered after reactant, removes and obtains attapulgite modified after filtrate；
（3）Count by weight, 15~20 parts of attapulgite modified, 50~70 parts of toluene, 20~25 parts of methanol, 8 are weighed respectively
~12 parts of ammoniacal liquor, 10~15 parts of magnesia and 15~20 parts of deionized waters, are warming up to 70~80 DEG C after mixing, and stirring reaction 2~
Reduced after 4h temperature to 40~50 DEG C reactant, and sequentially add urea, guar gum C14S and deionized water, insulated and stirred；
（4）After end to be mixed, nitrogen is passed through, is passed through after 2~4min and stops being passed through nitrogen, then change into and be passed through carbon dioxide gas
Body, is passed through after 2~3h and stops being passed through carbon dioxide, filter, be put into after collecting filter residue in baking oven, crushed after being dried, sieving,
Collect powder, you can obtain a kind of detergent for lubricating oil.
2. a kind of preparation method of detergent for lubricating oil according to claim 1, it is characterised in that：Step（1）Described in
Calcining heat be 500~600 DEG C, calcination time be 20~30min.
3. a kind of preparation method of detergent for lubricating oil according to claim 1, it is characterised in that：Step（2）Described in
Salicylic acid ethanol solution mass fraction be 10%.
4. a kind of preparation method of detergent for lubricating oil according to claim 1, it is characterised in that：Step（2）Described in
Heating-up temperature be 60~80 DEG C, time of stirring reaction is 2~3h.
5. a kind of preparation method of detergent for lubricating oil according to claim 1, it is characterised in that：Step（3）Described in
Ammoniacal liquor mass fraction be 15%.
6. a kind of preparation method of detergent for lubricating oil according to claim 1, it is characterised in that：Step（3）Described in
Urea quality be reactant quality 1~3%, guar gum C14S mass be reactant quality 2~4%, deionized water quality is anti-
Answer amount of substance 10~15%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377944A (en) * | 2002-03-07 | 2002-11-06 | 中国石油天然气股份有限公司 | Process for preparing compound metal type lubricating oil cleaning agent |
| CN104496786A (en) * | 2014-12-11 | 2015-04-08 | 青岛佰众化工技术有限公司 | Synthesis method of calcium-magnesium salicylate composite detergent |
| CN104531273A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Synthesis method of salicylic acid/sulfonic acid mixed medium calcium-magnesium composite clearing agent |
| CN105505523A (en) * | 2015-12-20 | 2016-04-20 | 仇颖超 | Method for preparing compounded lubricating oil detergent on basis of modified calcite |
| CN107118824A (en) * | 2017-05-05 | 2017-09-01 | 西安石油大学 | A kind of mixed-matrix lubricating oil magnesium salts detersive and preparation method thereof |
-
2017
- 2017-05-14 CN CN201710337083.7A patent/CN107201260A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377944A (en) * | 2002-03-07 | 2002-11-06 | 中国石油天然气股份有限公司 | Process for preparing compound metal type lubricating oil cleaning agent |
| CN104496786A (en) * | 2014-12-11 | 2015-04-08 | 青岛佰众化工技术有限公司 | Synthesis method of calcium-magnesium salicylate composite detergent |
| CN104531273A (en) * | 2014-12-11 | 2015-04-22 | 青岛佰众化工技术有限公司 | Synthesis method of salicylic acid/sulfonic acid mixed medium calcium-magnesium composite clearing agent |
| CN105505523A (en) * | 2015-12-20 | 2016-04-20 | 仇颖超 | Method for preparing compounded lubricating oil detergent on basis of modified calcite |
| CN107118824A (en) * | 2017-05-05 | 2017-09-01 | 西安石油大学 | A kind of mixed-matrix lubricating oil magnesium salts detersive and preparation method thereof |
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