CN108410543A - A kind of fire-retardant preparation of greases method of concave convex rod soil matrix - Google Patents
A kind of fire-retardant preparation of greases method of concave convex rod soil matrix Download PDFInfo
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- CN108410543A CN108410543A CN201810353129.9A CN201810353129A CN108410543A CN 108410543 A CN108410543 A CN 108410543A CN 201810353129 A CN201810353129 A CN 201810353129A CN 108410543 A CN108410543 A CN 108410543A
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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
- 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
- C10M169/04—Mixtures of base-materials and additives
- C10M169/042—Mixtures of base-materials and additives the additives being compounds of unknown or incompletely defined constitution only
-
- 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
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
-
- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/02—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds
- C10M2219/021—Sulfur-containing compounds obtained by sulfurisation with sulfur or sulfur-containing compounds used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
-
- 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
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- 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
- C10N2030/56—Boundary lubrication or thin film lubrication
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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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 fire-retardant preparation of greases methods of concave convex rod soil matrix, belong to lubricating grease preparing technical field.Containing attapulgite modified in lubricating grease produced by the present invention, the present invention is generated castor oil fermentation using mould microorganism rancid, castor-oil plant oil decomposition is generated into a large amount of free property ester groups and carboxyl organic matter using microorganism, the chelation of carboxyl organic matter so that the part metals element in attapulgite's surface lattice is chelated absorption simultaneously, promote the formation of wear surface oxide skin(coating), so that wearer surface forms oxide reconditioning layer, reduce wear extent, lubricating grease will be made in attapulgite modified incorporation base oil in the present invention, wherein attapulgite also have passed through organic siloxane modified, and its product decomposed can also largely absorb pernicious gas and smog caused by high molecular polymer burning while fire-retardant, smog is eliminated while not to make burning stop quickly, with splendid flame retardant effect, it has a extensive future.
Description
Technical field
The invention discloses a kind of fire-retardant preparation of greases methods of concave convex rod soil matrix, belong to lubricating grease technology of preparing neck
Domain.
Background technology
Lubricating grease is a kind of grease-like semisolid of stiff, for the friction part of machinery, plays lubrication and sealing function.
For metal surface, filling gap and anti-rust action are played.Mainly by mineral oil（Or synthetic lubricant fluid）It is modulated with thickening agent.
Many positions on automobile and engineering machinery all use lubricating grease as lubriation material, i.e., the butter that we often say.
It can be divided into two class of soap grease and non-soap base fat according to thickening agent.The thickening agent of soap grease often uses lithium, sodium, calcium, aluminium, zinc
Equal metallic soaps, also use the metallic soaps such as potassium, barium, lead, manganese.Thickening agent graphite, carbon black, the asbestos of non-soap base fat also have synthesis
（Such as polyureas base, bentonite）, two kinds of general-purpose grease and special grease can be divided into according to purposes, the former is used for common mechanical zero
Part, the latter is for tractor, railway locomotive, ship machinery, oil drilling machine, valve etc..Primary quality measure is dropping point, needle
In-degree, ash content and moisture etc..Index for evaluating lubricating grease colloidal stability is bleeding test, rolling bearing performance experiment
Deng.Tumbler test is the test method for testing the lower consistency change of rolling effect.Fluidity test is to evaluate lubricating grease at low temperature
The test method of aid pumpability.Anti-water drenching experiment is to evaluate the test method for the resistivity that lubricating grease goes out water wash.Glue
Body stability is that lubricating grease keeps colloid-stabilised in storage and use, the performance that liquid dormant oil is not precipitated from fat.Machinery peace
Qualitative is to indicate that lubricating grease resists the performance of consistency change under the conditions of machine work.Ball bearing torsional moment test is evaluation lubrication
A kind of test method of fat cryogenic property.Lubricating grease is that thickening agent is scattered in a kind of stabilization formed in fluid lubricant
Solid or semisolid product, wherein the additive and filler for being intended to improve certain characteristic of lubricating grease can be added.Lubricating grease is normal
It can be attached to vertical surface under temperature not to be lost in, and there can be other lubricants in unlimited or poor sealing friction part work
Irreplaceable holds a little.In general, the lubricating grease compatibility of identical soap base is preferable.Organic clay base and other bases not phase
Hold.
The rapid development of the modern industry, the requirement to lubricating grease is higher and higher, and the lubricating grease of high-quality multiple-effect is its development
Direction.Lubricating grease is as a kind of inflammable substance, and component 90% is mineral oil, it is easy to which spontaneous combustion is not only electrically set in underground
Received shipment, which turns bad, can cause big fire, and mechanical equipment operating is bad, and the friction overheat for breaking down and generating localized sustained generates foot
Enough warm-natured degree of combustion higher than oil equally can also cause fire, poor fire.Therefore, a kind of fire-retardant lubrication of concave convex rod soil matrix is invented
Fat has positive effect to lubricating grease preparing technical field.
Invention content
Present invention mainly solves the technical issues of, for lubricating grease as a kind of inflammable substance, component 90% is mine
Object oil, it is easy to which spontaneous combustion, in underground, not only electrical equipment operating is bad can cause big fire, and mechanical equipment operating is bad, and event occurs
The friction overheat for hindering and generating localized sustained is generated sufficiently higher than the oily warm-natured degree of combustion, equally can also cause fire, poor fire
Defect, provide a kind of fire-retardant preparation of greases method of concave convex rod soil matrix.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of fire-retardant preparation of greases method of concave convex rod soil matrix, it is characterised in that specifically preparation process is：
（1）Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 3~5 times successively, and the attapulgite after flushing is put into
Baking oven, drying to constant weight at 105~110 DEG C, then the attapulgite after drying is fitted into ball grinder mistake after 1~2h of ball milling
200 mesh sieve, and collect sieving powder and obtain pretreatment attapulgite powder；
（2）It is fitted into fermentation tank after above-mentioned attapulgite powder and castor oil are mixed, first fermentation tank opening is put into greenhouse,
Mouldy processing 3~5 days are stood, mouldy object is obtained；
（3）With sealed fermenter after the mouldy 15~20min of object of stirring rod stirring, it is sealed by fermentation, is separated by filtration after fermentation
To fermentation filter residue, it is fitted into three-necked flask after fermentation filter residue and dimethyl silicone polymer and water are mixed, at 60~70 DEG C,
It is stirred to react 30~40min, is separated by filtration to obtain filter cake, it is as attapulgite modified, it is spare；
（4）It is 1 in mass ratio that pork liver is put into the sodium chloride solution for being 0.75% with mass fraction after being crushed in tissue pulverizer:5
It is mixed to get mixture, is transferred in fermentation tank after mixture and methane liquid are mixed by equal mass ratioes, heat-preservation fermentation, fermentation ends
After be separated by filtration to obtain ferment filtrate；
（5）By N, it is fitted into three-necked flask after N '-penylene bismaleimide and soybean oil and the mixing of above-mentioned ferment filtrate,
130~150 DEG C are heated to, discharges after 2~3h of insulated and stirred reaction and obtains modified base oil；
（6）It is fitted into reaction kettle and is stirred after spare attapulgite modified and modified base oil is mixed, in the mistake of stirring
Absolute ethyl alcohol is added in journey, continues 20~30min of stirring, high-pressure homogenizer is transferred to after stirring, with the pressure of 20~30MPa
Homogenizing 1~2h of processing, deaerates to get the fire-retardant lubricating grease of concave convex rod soil matrix.
Step（2）Described in attapulgite powder and castor oil mass ratio be 1:2, the temperature in greenhouse is 25~35
DEG C, relative air humidity is 60~70%.
Step（3）Described in the temperature of sealing and fermenting be 35~40 DEG C, time of sealing and fermenting is 15~20 days, fermentation
The mass ratio of filter residue and dimethyl silicone polymer and water is 8:1:5.
Step（4）Described in the temperature of heat-preservation fermentation be 35~40 DEG C, time of heat-preservation fermentation is 12~15 days.
Step（5）Described in N, the quality of N '-penylene bismaleimide and soybean oil and ferment filtrate mixing
Than being 1:30:5.
Step（6）Described in the mass ratio of attapulgite modified and modified base oil be 2:1, the addition of absolute ethyl alcohol
It is the 10% of modified basic oil quality.
The beneficial effects of the invention are as follows：
（1）The present invention by ball milling after attapulgite ethyl alcohol and water washing, obtains attapulgite powder first, then by concave convex rod
It is mouldy in the environment of high temperature and humidity after native powder and castor oil mixing, it recycles mould to be sealed by fermentation later, obtains fermentation filter
Slag, continue to be obtained with organic siloxane modified fermentation filter residue it is attapulgite modified, then the present invention using pork liver as raw material, utilize natural pond
Gas-liquid ferments to obtain the ferment filtrate rich in elements such as nitrogen, sulphur, phosphorus, then soybean oil and vulcanizing agent and ferment filtrate is jointly anti-
It answers, the carbon-carbon double bond in soybean oil is opened to and introduced extreme pressure element sulphur, it is final that modified base oil is made, it finally will modified basis
Oily and attapulgite modified compounding is finally made the fire-retardant lubricating grease of concave convex rod soil matrix, contains in lubricating grease produced by the present invention and change
Property attapulgite, during modification, the present invention using mould microorganism by castor oil fermentation generate it is rancid, utilize microorganism
Castor-oil plant oil decomposition is generated into a large amount of free property ester groups and carboxyl organic matter, and by these ester groups under the self-crosslinking of microorganism
Attapulgite's surface is introduced, the introducing of wherein ester group greatly reduces the surface energy of attapulgite, makes it in base oil
Dispersibility is got higher, simultaneously because the similar intermiscibility of ester group and base oil, also makes the phase of modified attapulgite and base oil
Capacitive is improved, and can play the doping performance of attapulgite to greatest extent, while the chelation of carboxyl organic matter makes
Part metals element in attapulgite's surface lattice is chelated absorption, leave its original lattice position into after rancid
In carboxyl organic phase, to generate hole on attapulgite's surface lattice, the generation in these holes makes the oxygen of attapulgite
Change activity to be improved, during final lubricating grease use obtained so that the attapulgite with nano-scale layers chain structure
It can promote the formation of wear surface oxide skin(coating) so that wearer surface by the mechanically and chemically effect in friction process
Formation oxide reconditioning layer, reduction wear extent, and surface of the elements such as nitrogen, sulphur, phosphorus after lubricating grease coating in base oil
A stratification polarization layer protective film can be formed, the wear extent of base material can be also reduced, there is splendid lubrication to drop mill effect；
（2）Lubricating grease will be made in attapulgite modified incorporation base oil in the present invention, and wherein attapulgite also have passed through organosilicon
It is siloxane modified, and organosiloxane and rich zeopan clay mineral attapulgite itself are imitated with good at charcoal suppression cigarette
Fruit, lubricating grease burn occur when, organic matrix therein generates transitional charcoal in low temperature thermal decomposition, and organosiloxane with
The silica that rich zeopan attapulgite generates forms unbodied silicon protective layer on system surface, and and transitional
Between charcoal formed Si-O-C keys and-Si-C- keys protection layer of charcoal, isolation basis material and imflammable gas exchange and with it is outer
The heat on boundary is transmitted, and to reach flame retardant effect, and attapulgite modified can decompose when burning is heated absorbs comburant
Surface heat, while releasing the oxygen on large quantity of moisture dilution combustion things surface, decompose generation activated alumina be attached to it is flammable
Object surface further prevents the progress of burning, and is not only generated in the process without any harmful substance entirely fire-retardant,
And its decompose product can also largely be absorbed while fire-retardant high molecular polymer burning caused by pernicious gas and
Smog constantly absorbs imperfect combustion fusing residue, smog is eliminated while to make burning stop quickly, has splendid
Flame retardant effect, have a extensive future.
Specific implementation mode
Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 3~5 times successively, and the attapulgite after flushing is put into
Baking oven, drying to constant weight at 105~110 DEG C, then the attapulgite after drying is fitted into ball grinder mistake after 1~2h of ball milling
200 mesh sieve, and collect sieving powder and obtain pretreatment attapulgite powder；In mass ratio by above-mentioned attapulgite powder and castor oil
It is 1:Is fitted into fermentation tank after 2 mixing, it is 25~35 DEG C that fermentation tank opening, which is first put into temperature, relative air humidity for 60~
In 70% greenhouse, mouldy processing 3~5 days are stood, mouldy object is obtained；Hair is sealed after stirring mouldy 15~20min of object with stirring rod
Fermentation tank is sealed by fermentation 15~20 days at 35~40 DEG C, is separated by filtration to obtain fermentation filter residue after fermentation, will fermentation filter residue and
Dimethyl silicone polymer and water are 8 in mass ratio:1:It is fitted into three-necked flask after 5 mixing, at 60~70 DEG C, is stirred to react
30~40min is separated by filtration to obtain filter cake, as attapulgite modified, spare；Pork liver is put into after being crushed in tissue pulverizer
The sodium chloride solution for being 0.75% with mass fraction is 1 in mass ratio:5 are mixed to get mixture, mixture and methane liquid are pressed etc.
It is transferred in fermentation tank after mass ratio mixing, heat-preservation fermentation 12~15 days at 35~40 DEG C are separated by filtration to obtain after fermentation
Ferment filtrate；It is 1 in mass ratio:30:5 is mixed by N, N '-penylene bismaleimide and soybean oil and above-mentioned ferment filtrate
It is fitted into three-necked flask after conjunction, is heated to 130~150 DEG C, discharges after 2~3h of insulated and stirred reaction and obtain modified basis
Oil；It is 2 in mass ratio by spare attapulgite modified and modified base oil:It is fitted into reaction kettle and is stirred after 1 mixing,
The absolute ethyl alcohol of modified basic oil quality 10% is added during stirring, continues 20~30min of stirring, is transferred to after stirring
High-pressure homogenizer handles 1~2h with the pressure equalization of 20~30MPa, deaerates to get the fire-retardant lubricating grease of concave convex rod soil matrix.
Example 1
Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 3 times successively, and the attapulgite after flushing is put into baking oven,
Drying to constant weight at 105 DEG C, then the attapulgite after drying is fitted into ball grinder after ball milling 1h and crosses 200 mesh sieve, collects sieving
Powder obtains pretreatment attapulgite powder；It is 1 in mass ratio by above-mentioned attapulgite powder and castor oil:It is packed into after 2 mixing
In fermentation tank, it is 25 DEG C that fermentation tank opening, which is first put into temperature, in the greenhouse that relative air humidity is 60%, stands mouldy processing 3
It, obtains mouldy object；With sealed fermenter after the mouldy object 15min of stirring rod stirring, it is sealed by fermentation 15 days at 35 DEG C, fermentation knot
It is separated by filtration to obtain fermentation filter residue after beam, is 8 in mass ratio by fermentation filter residue and dimethyl silicone polymer and water:1:5 mixing
It is fitted into three-necked flask afterwards, at 60 DEG C, is stirred to react 30min, be separated by filtration to obtain filter cake, it is as attapulgite modified, it is standby
With；It is 1 in mass ratio that pork liver is put into the sodium chloride solution for being 0.75% with mass fraction after being crushed in tissue pulverizer:5 mixing
Mixture is obtained, is transferred in fermentation tank after mixture and methane liquid are mixed by equal mass ratioes, the heat-preservation fermentation 12 days at 35 DEG C,
It is separated by filtration to obtain ferment filtrate after fermentation；It is 1 in mass ratio:30:5 by N, N '-penylene bismaleimide and big
It is fitted into three-necked flask after soya-bean oil and the mixing of above-mentioned ferment filtrate, is heated to 130 DEG C, discharges after insulated and stirred reaction 2h
Obtain modified base oil；It is 2 in mass ratio by spare attapulgite modified and modified base oil:It is packed into reaction kettle after 1 mixing
In be stirred, the absolute ethyl alcohol of modified basic oil quality 10% is added during stirring, continues to stir 20min, stirring knot
It is transferred to high-pressure homogenizer after beam, 1h is handled with the pressure equalization of 20MPa, is deaerated to get the fire-retardant lubricating grease of concave convex rod soil matrix.
Example 2
Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 4 times successively, and the attapulgite after flushing is put into baking oven,
Drying to constant weight at 107 DEG C, then the attapulgite after drying is fitted into ball grinder after ball milling 1.5h and crosses 200 mesh sieve, collected
Sieve powder obtains pretreatment attapulgite powder；It is 1 in mass ratio by above-mentioned attapulgite powder and castor oil:It is filled after 2 mixing
Enter in fermentation tank, it is 30 DEG C that fermentation tank opening, which is first put into temperature, in the greenhouse that relative air humidity is 65%, stands mouldy place
Reason 4 days, obtains mouldy object；With sealed fermenter after the mouldy object 17min of stirring rod stirring, it is sealed by fermentation 17 days, sends out at 37 DEG C
It is separated by filtration to obtain fermentation filter residue after ferment, is 8 in mass ratio by fermentation filter residue and dimethyl silicone polymer and water:1:5
It is fitted into three-necked flask after mixing, at 65 DEG C, is stirred to react 35min, be separated by filtration to obtain filter cake, as modified attapulgite
Soil, it is spare；It is 1 in mass ratio that pork liver is put into the sodium chloride solution for being 0.75% with mass fraction after being crushed in tissue pulverizer:
5 are mixed to get mixture, are transferred in fermentation tank after mixture and methane liquid are mixed by equal mass ratioes, the heat-preservation fermentation at 37 DEG C
It 14 days, is separated by filtration to obtain ferment filtrate after fermentation；It is 1 in mass ratio:30:5 by N, N '-penylene bismaleimide
It is fitted into three-necked flask with after soybean oil and the mixing of above-mentioned ferment filtrate, is heated to 140 DEG C, insulated and stirred reacts 2.5h
Discharging obtains modified base oil afterwards；It is 2 in mass ratio by spare attapulgite modified and modified base oil:It is packed into after 1 mixing
It is stirred in reaction kettle, the absolute ethyl alcohol of modified basic oil quality 10% is added during stirring, continues to stir 25min,
It is transferred to high-pressure homogenizer after stirring, 1.5h is handled with the pressure equalization of 25MPa, is deaerated to get the fire-retardant profit of concave convex rod soil matrix
Consistent lubricant.
Example 3
Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 5 times successively, and the attapulgite after flushing is put into baking oven,
Drying to constant weight at 110 DEG C, then the attapulgite after drying is fitted into ball grinder after ball milling 2h and crosses 200 mesh sieve, collects sieving
Powder obtains pretreatment attapulgite powder；It is 1 in mass ratio by above-mentioned attapulgite powder and castor oil:It is packed into after 2 mixing
In fermentation tank, it is 35 DEG C that fermentation tank opening, which is first put into temperature, in the greenhouse that relative air humidity is 70%, stands mouldy processing 5
It, obtains mouldy object；With sealed fermenter after the mouldy object 20min of stirring rod stirring, it is sealed by fermentation 20 days at 40 DEG C, fermentation knot
It is separated by filtration to obtain fermentation filter residue after beam, is 8 in mass ratio by fermentation filter residue and dimethyl silicone polymer and water:1:5 mixing
It is fitted into three-necked flask afterwards, at 70 DEG C, is stirred to react 40min, be separated by filtration to obtain filter cake, it is as attapulgite modified, it is standby
With；It is 1 in mass ratio that pork liver is put into the sodium chloride solution for being 0.75% with mass fraction after being crushed in tissue pulverizer:5 mixing
Mixture is obtained, is transferred in fermentation tank after mixture and methane liquid are mixed by equal mass ratioes, the heat-preservation fermentation 15 days at 40 DEG C,
It is separated by filtration to obtain ferment filtrate after fermentation；It is 1 in mass ratio:30:5 by N, N '-penylene bismaleimide and big
It is fitted into three-necked flask after soya-bean oil and the mixing of above-mentioned ferment filtrate, is heated to 150 DEG C, discharges after insulated and stirred reaction 3h
Obtain modified base oil；It is 2 in mass ratio by spare attapulgite modified and modified base oil:It is packed into reaction kettle after 1 mixing
In be stirred, the absolute ethyl alcohol of modified basic oil quality 10% is added during stirring, continues to stir 30min, stirring knot
It is transferred to high-pressure homogenizer after beam, 2h is handled with the pressure equalization of 30MPa, is deaerated to get the fire-retardant lubricating grease of concave convex rod soil matrix.
Comparative example
With the fire-retardant lubricating grease of concave convex rod soil matrix of Shanghai company production as a comparison case to concave convex rod soil matrix produced by the present invention
The fire-retardant lubricating grease of concave convex rod soil matrix in fire-retardant lubricating grease and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Dropping point test is detected by the standard of GB/T 3498；
600 DEG C of hot plate combustion tests：The iron plate of 150 × 10mm of Φ is heated to 600 DEG C on electric furnace, using electric thermo-couple temperature
Meter control temperature ± 5 DEG C, keep 5min, with dropping in lubricating grease sample:On hot plate, observes its burning, do not burn, repeat two
Secondary equifinality is final judging result；
Abrasion loss test is detected by 3960 standards of GB/T；
PVvalue testing is detected by 3960 standards of GB/T；
Flame retardant rating test is by flame retardant rating by HB, and incremental standard is detected step by step to V-0 by V-2, V-1.
1 PERFORMANCE OF GREASES measurement result of table
According to the fire-retardant lubricating grease good flame resistance of the concave convex rod soil matrix produced by the present invention of data among the above, 600 DEG C of hot plate burnings
Non-ignitable after experiment, flame retardant rating reaches 0 grade, has broad application prospects.
Claims (6)
1. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix, it is characterised in that specifically preparation process is：
（1）Weigh attapulgite uses absolute ethyl alcohol and deionized water to rinse 3~5 times successively, and the attapulgite after flushing is put into
Baking oven, drying to constant weight at 105~110 DEG C, then the attapulgite after drying is fitted into ball grinder mistake after 1~2h of ball milling
200 mesh sieve, and collect sieving powder and obtain pretreatment attapulgite powder；
（2）It is fitted into fermentation tank after above-mentioned attapulgite powder and castor oil are mixed, first fermentation tank opening is put into greenhouse,
Mouldy processing 3~5 days are stood, mouldy object is obtained；
（3）With sealed fermenter after the mouldy 15~20min of object of stirring rod stirring, it is sealed by fermentation, is separated by filtration after fermentation
To fermentation filter residue, it is fitted into three-necked flask after fermentation filter residue and dimethyl silicone polymer and water are mixed, at 60~70 DEG C,
It is stirred to react 30~40min, is separated by filtration to obtain filter cake, it is as attapulgite modified, it is spare；
（4）It is 1 in mass ratio that pork liver is put into the sodium chloride solution for being 0.75% with mass fraction after being crushed in tissue pulverizer:5
It is mixed to get mixture, is transferred in fermentation tank after mixture and methane liquid are mixed by equal mass ratioes, heat-preservation fermentation, fermentation ends
After be separated by filtration to obtain ferment filtrate；
（5）By N, it is fitted into three-necked flask after N '-penylene bismaleimide and soybean oil and the mixing of above-mentioned ferment filtrate,
130~150 DEG C are heated to, discharges after 2~3h of insulated and stirred reaction and obtains modified base oil；
（6）It is fitted into reaction kettle and is stirred after spare attapulgite modified and modified base oil is mixed, in the mistake of stirring
Absolute ethyl alcohol is added in journey, continues 20~30min of stirring, high-pressure homogenizer is transferred to after stirring, with the pressure of 20~30MPa
Homogenizing 1~2h of processing, deaerates to get the fire-retardant lubricating grease of concave convex rod soil matrix.
2. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix according to claim 1, it is characterised in that：Step
（2）Described in attapulgite powder and castor oil mass ratio be 1:2, the temperature in greenhouse is 25~35 DEG C, and air is opposite
Humidity is 60~70%.
3. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix according to claim 1, it is characterised in that：Step
（3）Described in the temperature of sealing and fermenting be 35~40 DEG C, time of sealing and fermenting is 15~20 days, and ferment filter residue and poly- diformazan
The mass ratio of radical siloxane and water is 8:1:5.
4. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix according to claim 1, it is characterised in that：Step
（4）Described in the temperature of heat-preservation fermentation be 35~40 DEG C, time of heat-preservation fermentation is 12~15 days.
5. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix according to claim 1, it is characterised in that：Step
（5）Described in N, the mass ratio of N '-penylene bismaleimide and soybean oil and ferment filtrate mixing is 1:30:5.
6. a kind of fire-retardant preparation of greases method of concave convex rod soil matrix according to claim 1, it is characterised in that：Step
（6）Described in the mass ratio of attapulgite modified and modified base oil be 2:1, the addition of absolute ethyl alcohol is modified base oil
The 10% of quality.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940037A (en) * | 2005-09-28 | 2007-04-04 | 中国石油化工股份有限公司 | Thermal roll-oil composition of dispersing oily clay wear-resistant anti-skid agent |
| CN102533417A (en) * | 2011-12-02 | 2012-07-04 | 华北电力大学 | Method for preparing nano-attapulgite lubricating grease |
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2018
- 2018-04-19 CN CN201810353129.9A patent/CN108410543A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940037A (en) * | 2005-09-28 | 2007-04-04 | 中国石油化工股份有限公司 | Thermal roll-oil composition of dispersing oily clay wear-resistant anti-skid agent |
| CN102533417A (en) * | 2011-12-02 | 2012-07-04 | 华北电力大学 | Method for preparing nano-attapulgite lubricating grease |
Non-Patent Citations (3)
| Title |
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| 凹凸棒在阻燃材料方向的研究应用进展，孙慧茹等: "凹凸棒在阻燃材料方向的研究应用进展", 《化工管理》 * |
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Application publication date: 20180817 |