CN1580211A - Method for preparing low-noise carbamido lubricating grease - Google Patents

Abstract

The invention is a kind of preparation methods to produce carbamido consistent grease with low noise. The approach follows this. Mix organo amine with isocyanic ester and base oil and they will reactive, when the batch heat rises to 100-150 degree, add cold oil in order to cool auxiliary product rapidly. Later, whet the outcome to produce fat. The organo amine is a kind of asmixture by fat amine which carbon number is 10-20 and aromatic amine which carbon number is 6-8, the both mol ratio is 0.25-4:1. The cold oil's use level is 5%-35% of base oil's. the base oil is mineral oil which temperature is 100 degree and coefficient of viscosity is 4-40cSt or assemble A-alkene oil. The carbamido consistent grease in this way has a equable libration value, the libration data can be got within 10-20 seconds exactly, so it can improve production efficiency of bearing obviously.

Description

The preparation method of low-noise urea-base grease

Technical field

The invention belongs to the preparation method of urea-base grease.

Technical background

Along with requirements such as mechanical means miniaturization, lightweight, precise treatment, low noiseization and long lifetimes, the rotational parts of machinery not only smaller volume, velocity of rotation is accelerated, and component dense arrangement, make envrionment temperature become very high, abominable like this working condition has proposed harsh requirement to the lubricating grease that uses.For general lithium soap grease,, can not satisfy thermotolerance and long-life requirement though have low noise characteristic preferably.Though and urea-base grease has a lot of premium propertiess, as heat-resistant quality, oxidation stability, colloid stability, mechanical stability or the like, also in a lot of industries, be used widely,, the sound equipment poor-performing of urea-base grease can not meet the demands.

Therefore people have taked thousand and one way to improve the acoustic characteristic of urea-base grease, for example, USP6136762, the drop size during by control isocyanic ester and organic amine reaction is controlled the length of viscosifying agent fiber, and then reduces noise; JP2077494 mixes by at least two kinds of urea-base greases and to reduce lubricating grease vibration; JP3243696 is by using the aliphatic amide more than 12 carbon and the mixed amine and the isocyanate reaction of 8 carbocyclic aliphatic amine, prepares urea-base grease; JP2208395 has introduced with aliphatic amide and has mixed the method for preparing low-noise urea-base grease with aromatic amine; JP02004895 prepares low-noise urea-base grease by changing grinding dispersive method.But generally all adopting, above patent places the lubricating grease cool to room temperature that the order of refrigerative method is in comparatively high temps (more than 140 ℃).The vibration values instability of the lubricating grease made from this quadrat method, initial vibration value is higher usually, along with running reduction gradually, needs 60-120 second even longer time just can detect vibration values data accurately, has influenced the production efficiency of bearing.

Summary of the invention

Defective at prior art, the present invention proposes a kind of preparation method of low-noise urea-base grease, the urea-base grease that adopts this method to make has stable vibration values, just can detect in second at 10-20 and obtain vibration values data accurately, and the production efficiency of bearing is significantly improved.

The preparation method of low-noise urea-base grease provided by the invention comprises: with organic amine and isocyanic ester and base oil is mixed and reaction, treat that temperature of charge is elevated to 100-150 ℃ after, add cold oil material cooled off rapidly, grind to form fat.

Specifically, can respectively organic amine and isocyanic ester be joined in the poly ﹠ Alpha ,-olefin oil, be heated to about 40-60 ℃, it is melted fully, again the oil solution of isocyanic ester and the oil solution of organic amine are mixed, fully stir, organic amine and isocyanic ester are reacted, controlled temperature is elevated to 100-150 ℃, preferred 110-145 ℃, for reacting fully, preferably constant temperature stirred 10-30 minute, add cold oil (mineral oil or poly ﹠ Alpha ,-olefin oil) then, on three-roll grinder, grind to form fat.

Said organic amine is the mixture of aliphatic amide and aromatic amine, and the mol ratio of the two is 0.25-4: 1, and preferred 0.5-3: 1.Wherein the carbon number of aliphatic amide is 10-20, preferred 12-18, for example, amino dodecane, tetradecy lamine, cetylamine, stearylamine; The aromatic amine carbon number is 6-8, can be aniline, the perhaps aniline that replaces of alkyl or halogen, for example para-totuidine, Ortho Toluidine, meta-aminotoluene, to ethylaniline, adjacent ethylbenzene amine, an ethylbenzene amine; P-Chlorobenzoic acid amide, m-chloro aniline, dichlorphenamide bulk powder, bromaniline etc.Said isocyanic ester can be the vulcabond of 7-13 carbon, for example MDI (4,4 '-vulcabond ditane), TDI (2,4 toluene diisocyanate, 2,6-tolylene diisocyanate, or their mixture).Organic amine and isocyanic ester react according to 1: 0.5 mol ratio in theory, but for organic amine is reacted completely, the consumption of isocyanic ester can be 1.02-1.05 times of isocyanic ester calculated amount.

Said base oil is that 100 ℃ of viscosity are 4-40cSt, mineral oil or the poly ﹠ Alpha ,-olefin oil of preferred 8-20cSt.

Said cold oil is the part of base oil, and consumption is the 5%-35% of base oil total mass, preferred 8%-30%.

Adopt the urea-base grease of the inventive method preparation to have stable vibration values, at short notice (10-20 second) just can detect and obtain vibration values data accurately, avoided urea-base grease vibration values instability with the prior art preparation, (60-120 second even longer time) just can detect the problem of accurate data to need the long period, be used for the time that bearing vibration value detects in the Production of bearing process thereby shortened, the production efficiency that improves bearing is had tangible help.

Embodiment

Example 1

Earlier stearylamine (64.4g) and para-totuidine (25.6g) are joined (100 ℃ of viscosity 16.1cSt) in the 373g poly ﹠ Alpha ,-olefin oil, be heated to 60 ℃, organic amine is melted fully; In the 373g poly ﹠ Alpha ,-olefin oil, add MDI (59.9g) again, be heated to MDI simultaneously and melt; Then MDI-oil is joined in organic amine-oil, fully stir, make organic amine and isocyanic ester complete reaction,, stir and constant temperature 30min when temperature is elevated to 110 ℃; At last, add the 373g poly ﹠ Alpha ,-olefin oil, the lubricating grease in the still is cooled off rapidly as cold oil.The urea-base grease of making grinds three times and becomes fat on three-roll grinder.

Example 2

Earlier amino dodecane (8.9g) and m-chloro aniline (6.1g) are joined (100 ℃ of viscosity 11cSt) in the 212.5g mineral oil, be heated to 60 ℃, organic amine is melted fully; In 212.5g mineral oil, add MDI (12.2g) again, be heated to MDI simultaneously and melt; Then MDI-oil is joined in organic amine-oil, fully stir, make organic amine and isocyanic ester complete reaction, make temperature remain on 120 ℃ then, stir constant temperature 30min; At last, add 30g mineral oil, the lubricating grease in the still is cooled off rapidly as cold oil.The urea-base grease of making grinds three times and becomes fat on three-roll grinder.

Example 3

Earlier stearylamine (12.4g) and adjacent ethylbenzene amine (16.7g) are joined (100 ℃ of viscosity 8.0cSt) in the 202.5g poly ﹠ Alpha ,-olefin oil, be heated to 60 ℃, organic amine is melted fully; In the 202.5g poly ﹠ Alpha ,-olefin oil, add TDI (16.3g) again, be heated to TDI simultaneously and melt; Then TDI-oil is joined in organic amine-oil, fully stir, make organic amine and isocyanic ester complete reaction,, stir constant temperature 30min when temperature is elevated to 140 ℃; At last, add the 50g poly ﹠ Alpha ,-olefin oil, the lubricating grease in the still is cooled off rapidly as cold oil.The urea-base grease of making grinds three times and becomes fat on three-roll grinder.

Comparative Examples 1

Method according to the JP3243696 patent disclosure, the MDI (29.9g) that will be dissolved in the poly ﹠ Alpha ,-olefin oil of 186g (100 ℃ of viscosity 16.1cSt) adds in the stearylamine (64.4g) of the poly ﹠ Alpha ,-olefin oil that is dissolved in 186g (100 ℃ of viscosity 16.1cSt), under fully stirring, temperature is raised to 170 ℃, place cool to room temperature then, make A fat, the MDI (30g) that gets the alkene oil that is dissolved in 186g (100 ℃ of viscosity 16.1cSt) again joins in the para-totuidine (25.6g) of the poly ﹠ Alpha ,-olefin oil that is dissolved in 186g (100 ℃ of viscosity 16.1cSt), under fully stirring, temperature is raised to 170 ℃, place cool to room temperature then, make B fat.Get A fat 80g and B fat 20g then and mix, on three-roll grinder, grind one-tenth fat then three times.

Comparative Examples 2

According to the method for JP2077494 patent disclosure, earlier stearylamine (64.4g) and para-totuidine (25.6g) are joined (100 ℃ of viscosity 16.1cSt) in the 500g poly ﹠ Alpha ,-olefin oil, be heated to 60 ℃, organic amine is melted fully; In the 519g poly ﹠ Alpha ,-olefin oil, add MDI (59.9g) again, be heated to MDI simultaneously and melt; Then MDI-oil is joined in organic amine-oil, fully stir, make organic amine and isocyanic ester complete reaction, this moment, temperature can be elevated to 100～120 ℃, carried out for reacting fully, and continued to raise the temperature to 180 ℃, again constant temperature 30min under agitation; At last, naturally cool to room temperature.The urea-base grease of making grinds three times and becomes fat on three-roll grinder.

Comparative Examples 3

Earlier stearylamine (64.4g) and para-totuidine (25.6g) are joined (100 ℃ of viscosity 16.1cSt) in the 559.5g poly ﹠ Alpha ,-olefin oil, be heated to 60 ℃, organic amine is melted fully; In the 559.5g poly ﹠ Alpha ,-olefin oil, add MDI (59.9g) again, be heated to MDI simultaneously and melt; Then MDI-oil is joined in organic amine-oil, fully stir, make organic amine and isocyanic ester complete reaction, this moment, temperature can be elevated to 130 ℃, for reacting fully, stirred constant temperature 30min under this temperature; At last, naturally cool to room temperature.The urea-base grease of making grinds three times and becomes fat on three-roll grinder.

The test method of embodiment and Comparative Examples and analytical data see Table 1 and table 2 respectively.

Table 1 test method

Method name	Side's religious name	Test conditions
			Cone penetration	????GB/T269	Room temperature is worked 60 times
Dropping point	????GB/T3498
			Vibration values	????JB/T5313-91	????1800r/min，50N

Table 2 analytical results

Sample	Example 1	Example 2	Example 3	Comparative Examples 1	Comparative Examples 2	Comparative Examples 3
							Aliphatic amide	Stearylamine	Amino dodecane	Stearylamine	Stearylamine	Stearylamine	Stearylamine
Aromatic amine	Para-totuidine	P-Chlorobenzoic acid amide	Adjacent ethylbenzene amine	Para-totuidine	Para-totuidine	Para-totuidine
							Isocyanic ester	MDI	??MDI	??TDI	??MDI	??MDI	??MDI
Base oil types viscosity, cSt	PAO 16.1	??MIN ??11	??PAO ??8.0	??PAO ??16.1	??PAO ??16.1	??PAO ??16.1
							Refining temperature, ℃	110	??120	??140	??180	??100	??130
Add cold oil, g	373	??75	??30	??/	??/	??0
							The viscosifying agent consumption, %	10	??9	??9	??10	??10	??10
Cone penetration, 0.1mm	260	??270	??265	??290	??318	??285
							Dropping point, ℃	＞280	??＞280	??＞280	??280	??＞280	??＞280
Vibration values (high frequency), μ m/s steady time, second	17 15	??18 ??20	??24 ??18	??26-19 ??60	??30-20 ??＞120	??30-20 ??＞120

Claims (9)

1. the preparation method of a low-noise urea-base grease, comprise: with organic amine and isocyanic ester and base oil is mixed and reaction, after treating that temperature of charge is elevated to 100-150 ℃, adding cold oil cools off material rapidly, grind to form fat, wherein organic amine is the mixture of aliphatic amide and aromatic amine, and the two mol ratio is 0.25-4: 1.

2. in accordance with the method for claim 1, it is characterized in that the control temperature of charge is elevated to 110-145 ℃, and constant temperature stirred 10-30 minute.

3. in accordance with the method for claim 1, it is characterized in that organic amine is that carbon number is that aliphatic amide and the carbon number of 10-20 is the mixture of the aromatic amine of 6-8, the two mol ratio is 0.5-3: 1.

4. according to claim 1 or 3 described methods, it is characterized in that aliphatic amide is selected from one or more the mixture in amino dodecane, tetradecy lamine, cetylamine, the stearylamine.

5. according to claim 1 or 3 described methods, it is characterized in that aromatic amine is selected from para-totuidine, Ortho Toluidine, meta-aminotoluene, to one or more the mixture in ethylaniline, adjacent ethylbenzene amine, an ethylbenzene amine, p-Chlorobenzoic acid amide, m-chloro aniline, dichlorphenamide bulk powder, the bromaniline.

6. in accordance with the method for claim 1, it is characterized in that said isocyanic ester is that carbon number is the vulcabond of 7-13.

7. in accordance with the method for claim 6, it is characterized in that isocyanic ester is 4,4 '-vulcabond ditane, 2,4 toluene diisocyanate, 2,6-tolylene diisocyanate or their mixture.

8. in accordance with the method for claim 1, it is characterized in that said base oil is mineral oil or the poly ﹠ Alpha ,-olefin oil that 100 ℃ of viscosity are 4-40cSt.

9. in accordance with the method for claim 1, it is characterized in that said cold oil consumption is the 5%-35% of base oil total amount.