CN107185497A - Wind power gear oil regeneration processing highly polar mesoporous adsorbent and preparation method thereof - Google Patents
Wind power gear oil regeneration processing highly polar mesoporous adsorbent and preparation method thereof Download PDFInfo
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- CN107185497A CN107185497A CN201710570477.7A CN201710570477A CN107185497A CN 107185497 A CN107185497 A CN 107185497A CN 201710570477 A CN201710570477 A CN 201710570477A CN 107185497 A CN107185497 A CN 107185497A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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Abstract
Wind power gear oil regeneration processing highly polar mesoporous adsorbent and preparation method thereof, the component of the adsorbent includes Si, Al, Ti and C, and Si, Al, Ti and C mol ratio are:(2~5)：(1~5)：1：(0.1~1.5)；The aperture of the adsorbent is 10~50nm, and specific surface area is 330~650m2/g；The invention also discloses the preparation method of the adsorbent；Adsorbent of the present invention is all with highly polar, it can quick, effectively remove the polarity ageing products produced in oil product by aging or additive hydrolysis, oil product acid number is reduced, improve the foam characteristic of oil product and removes greasy filth etc., so as to recover the various performance indications of oil product comprehensively；Pressure difference when wind power gear oil is pumped across regeneration filter can be greatly reduced in the mesoporous characteristic that adsorbent of the present invention has, and greatly improve again the processing safety of generating apparatus；Its preparation method simplicity, mild condition, easily operated, cost are low, are particularly suitable for large-scale production.
Description
Technical field
The invention belongs to oil for electric power regeneration treatment technical field of absorbent, and in particular at a kind of wind power gear oil regeneration
Reason highly polar mesoporous adsorbent and preparation method thereof.
Background technology
Wind power gear oil is mainly used in aerogenerator unit speed-up gearbox, is used as lubrication, the medium of radiating.Blower fan exists
In running, due to by function influences such as ambient temperature, oxygen, moisture, metal catalytic and shearing forces, oil product occur aging,
Additive decomposition and consumption is inevitable.Wind power gear oil mainly uses oil based on fully synthetic poly alpha olefin at present, adds excellent
Different extreme-pressure anti-wear antioxygen compound additive allotment is formed, and its price is 10 times of plain mineral oil or so.With wind-powered electricity generation
How the extensive use of unit, extend fluid service life, reduces the O＆M cost of Wind turbines, it has also become wind-powered electricity generation industry develops
Bottleneck.
At present, domestic each wind park takes the suggestion of equipment manufacturing to change a fresh oil per 3-5.Change fresh oil not
Only price is high, and waste oil disposal can cause many environmental problems.On the regeneration treatment of oil for electric power, presently mainly pin
To the steam turbine oil of low viscosity, fire resistant oil, transformer oil and part subsidiary engine oil, handed over more than power plant using silica gel, diatomite, ion
Change the adsorbents such as resin, activated alumina and regeneration treatment is carried out to the rotten oil product of deterioration, to extend the service life of fluid, close
It is a large amount of the characteristics of silica gel, diatomite, ion exchange resin, activated alumina and common zeolite adsorbent
Report.But for highly viscous wind power gear oil, (kinematic viscosity is 320mm240 DEG C of/s@) regeneration treatment adsorbent and its
Preparation method has not been reported, and it is primarily due to wind power gear oil, and viscosity is higher at normal temperatures, and polarity aging is produced in oil
The catabolite of thing or additive is too low to the activated centre diffusion rate of adsorbent when by adsorbent, causes to remove always
The efficiency for changing product is too low, or the pressure difference of fluid regeneration filter is excessive, equipment safety hidden danger is caused, so that can not enter
Row commercial introduction.
It is above-mentioned it is described it is mesoporous be to be provided according to international material association：Material aperture be less than 2nm for poromerics
(Microporous)；Aperture is mesopore or mesoporous material (Mesoporous) in 2-50nm；It is macropore material more than 50nm
Expect (Macroporous).
The content of the invention
To solve above-mentioned problems of the prior art, it is an object of the invention to provide a kind of wind power gear oil regeneration
Processing highly polar mesoporous adsorbent and preparation method thereof, adsorbent of the present invention is all with highly polar, can quick, effectively remove
Because of the polarity ageing products that aging or additive hydrolysis are produced in oil product, reduction oil product acid number, improve oil product foam characteristic and
Greasy filth etc. is removed, so as to recover the various performance indications of oil product comprehensively；The mesoporous characteristic that adsorbent of the present invention has can be significantly
Reduction wind power gear oil is pumped across pressure difference during regeneration filter, greatly improves again the processing safety of generating apparatus；It is prepared
Method simplicity, mild condition, easily operated, cost are low, are particularly suitable for large-scale production.
To reach above-mentioned purpose, the technical solution adopted in the present invention is：
A kind of highly polar mesoporous adsorbent of wind power gear oil regeneration processing, the component of the adsorbent includes Si, Al, Ti
And C, Si, Al, Ti and C mol ratio are:(2~5)：(1~5)：1：(0.1~1.5).
Described Si, Al, Ti and C mol ratio are 3：2.5：1：0.8.
The aperture of the adsorbent is 10~50nm, and specific surface area is 330~650m2/g。
The preparation method of the highly polar mesoporous adsorbent of wind power gear oil regeneration processing described above, including following step
Suddenly：
Step 1：It is (0.05~0.25) by weight ratio：1 organic amine and cetyl trimethylammonium bromide is configured to alkali
Property solution, regulation pH in the range of 8~12, and 50~85 DEG C stir 5 hours；
Step 2：The water soluble polymer emulsion that weight is accounted for into alkaline solution 5~17% is added to alkalescence prepared by step 1
In solution, and stir more than 3 hours；
Step 3：The carbon source that weight is accounted for into alkaline solution 0.5~2.5% is added in alkaline solution prepared by step 2, and
Stirring more than 2 hours；
Step 4：It is (2~5) by Si, Al and Ti mol ratio：(1~5)：The mixture of 1 silicon source, silicon source and titanium source,
In the case of being stirred vigorously, in the solution for being added to step 3 preparation, the addition of the mixture of silicon source, silicon source and titanium source causes
Si, Al, Ti and C mol ratio are (2~5)：(1~5)：1：(0.1~1.5), and continue stirring 8~15 hours, obtain white
Primogel product；
Step 5：The white Primogel product that step 4 is obtained is placed in 80~120 DEG C of convection ovens more than 15 hours,
Obtain white solid powder；
Step 6：The white solid powder that step 5 is obtained is washed more than 3 times with absolute ethyl alcohol, then with distillation water washing
More than 3 times, untill cleaning fluid water white transparency, obtain the former powder of white micro-porous adsorption agent；
Step 7：The former powder of white micro-porous adsorption agent that step 5 is obtained is transferred in microwave reaction kettle, in microwave radiation bar
Heated under part, the reactor pressure is 0.5~1.0MPa, 1~3 hour time, Power Control obtains strong pole in 500~1000W
Property mesoporous adsorbent.
PH regulations described in step 1 are adjusted using ammoniacal liquor or sodium hydroxide and dust technology or glacial acetic acid.
Organic amine described in step 1 is ethylenediamine, formamide, 3- Propanolamines, dipropylamine, tetraethyl ammonium hydroxide or four
Propyl group ammonium hydroxide.
Water soluble polymer emulsion described in step 2 for styrene-acrylic emulsion or acrylic emulsion or ethylene copolymerization emulsions or
Person's epoxy resin latex or one kind or its mixture in its modified emulsion, the average grain diameter of emulsion is in 50~100nm scopes
It is interior, and solid content is in the range of 45~65%, when for two kinds when, be arbitrary proportion mixing.
Carbon source described in step 3 is graphite or one kind or its mixture in CNT, and in nano powdery,
When for two kinds when, be arbitrary proportion mixing.
Silicon source described in step 4 is the one or more in sodium metasilicate, Ludox, silica gel, white carbon, when for it is a variety of when,
Mixed for arbitrary proportion.
Silicon source described in step 4 for aluminium hydroxide, meta-aluminate, aluminate, triisobutyl aluminium and diethyl aluminum chloride or
One kind in aluminum sulfate, aluminium chloride in inorganic aluminium compound.
Titanium source described in step 4 is the sulfuric acid in butyl titanate in organic titanium esters, isopropyl titanate or inorganic titanium compound
One kind in titanium, titanium chloride.
Heating can be carried out under air or oxygen atmosphere in microwave reaction kettle described in step 6.
Compared to the prior art, the invention has the advantages that：
1st, the present invention has simple synthetic method, mild condition, easily operated, cost low, is particularly suitable for scale
Metaplasia is produced；The adsorbent stability is high, wherein water soluble polymer emulsion and the carbon nanopowder end added are as to cetyl
The supplement of trimethyl amine bromide organic formwork agent, carbon nanopowder end simultaneously have catalyst effect so that reaction carry out completely and
Speed is greatly improved；The adsorbent have meso-hole structure (aperture be 10~50nm) and aperture is homogeneous, specific surface area it is big (330~
650m2/ g) the features such as；The adsorbent is handled for wind power gear oil regeneration, can effectively be removed in oil product because of aging or addition
The polarity ageing products that agent hydrolysis is produced, reduction oil product acid number, the foam characteristic for improving oil product and removal greasy filth etc., can be comprehensively extensive
The property indices of multiple oil product, the service life of effective extension oil product is significant to energy-conserving and environment-protective.
2nd, the Al elements introduced in adsorbent of the present invention, partly in order to improving metal-doped in mesoporous adsorbent
Amount, so as to improve the polarity of adsorbent, reaches quick, effective remove in oil product because the polarity of aging or additive hydrolysis generation is old
Change product, reduction oil product acid number, the foam characteristic for improving oil product and removal greasy filth etc., so as to recover the various performances of oil product comprehensively
Index；On the other hand, the Al elements of introducing can promote to combine to form caged oxide between three kinds of metals (Si, Al, Ti), preferably
The adsorbents such as conventional sial, aluminum oxide are avoided, are combined because part metals are dissolved in oil with fluid and its ageing products
Metal soap gel is formed, the problem of occurring to block oil system filter screen.
3rd, adsorbent of the present invention added in preparation process a certain amount of water soluble polymer emulsion (average grain diameter be 50~
100nm, solid content be 45~65%), be in order to obtain the Primogel containing certain proportion high molecular nano-microsphere, through overdrying
Dry and sintering step, high molecular nano-microsphere size reduction and the mesoporous hole that 10~50nm is formed after its volatilization, it is had
Pressure difference when wind power gear oil is pumped across regeneration filter can be greatly reduced in the mesoporous characteristic having, and greatly improve again generating apparatus
Processing safety.
Embodiment
The present invention is described in further detail with embodiment below.
Embodiment one：
Ethylenediamine 6g and cetyl trimethylammonium bromide 100g is taken to be dissolved in 500g distilled water respectively, with ammoniacal liquor and ice vinegar
Acid for adjusting pH value is to 8.5, and in 65 DEG C of stirred in water bath 5 hours, mixing speed was set to 800r/min, adds water-soluble styrene-acrylic emulsion
Continue to stir 4 hours after 15g and acrylic emulsion 20g, add the powder that the particle diameter prepared by CNT is 10nm or so
0.8g, continues to stir 4 hours, then by the mixture of 300g anhydrous sodium metasilicates, 250g triisobutyl aluminiums and 170g butyl titanates
It is added thereto, mixing speed is set into 1300r/min persistently stirs 10 hours, cools down at room temperature, by the white Primogel of gained
Product is placed in 95 DEG C of convection ovens and dried 15 hours, and gained white solid powder is respectively washed with absolute ethyl alcohol and distilled water respectively
Wash three times, washing lotion water white transparency.Gained white powder is transferred in microwave reaction kettle again, reactor pressure is 0.5MPa, work(
Rate control was in 800W continuous heatings 3.0 hours, and natural cooling in air obtains highly polar mesoporous adsorbent.
When the gear oil deteriorated to certain wind park carries out regeneration treatment, the highly polar mesoporous adsorbent 2wt% is added,
In 45 DEG C of water-baths after heating stirring 30min, filtered with filter paper, with before processing index after testing the oil product after processing
Contrasted, the results are shown in Table 1.
The main project Comparative result of oil product before and after certain wind park deterioration gear oil regeneration of table 1
Embodiment two：
Dipropylamine 8g, formamide 16g and cetyl trimethylammonium bromide 100g is taken to be dissolved in 500g distilled water respectively,
PH value is adjusted to 9.6 with ammoniacal liquor and glacial acetic acid, and in 55 DEG C of stirred in water bath 5 hours, mixing speed was set to 800r/min, adds water
Continue to stir 6 hours after dissolubility ethylene copolymerization emulsions 10g and acrylic emulsion 5g, adding the particle diameter prepared by CNT is
10nm or so powder 1.5g, continues to stir 3 hours, then by 160g Ludox, 190g sodium metaaluminates and 120g metatitanic acid isopropyls
The mixture of ester is added thereto, and mixing speed is set into 1500r/min persistently stirs 14 hours, cools down at room temperature, and gained is white
Color Primogel product is placed in 105 DEG C of convection ovens and dried 18 hours, and gained white solid powder is used into absolute ethyl alcohol respectively
Respectively washed with distilled water three times, washing lotion water white transparency.Gained white powder is transferred in microwave reaction kettle again, reactor pressure
For 0.8MPa, Power Control was in 500W continuous heatings 3.0 hours, and natural cooling in air obtains highly polar mesoporous adsorbent.
When the gear oil deteriorated to certain wind park carries out regeneration treatment, the highly polar mesoporous adsorbent 4wt% is added,
In 55 DEG C of water-baths after heating stirring 20min, filtered with filter paper, with before processing index after testing the oil product after processing
Contrasted, the results are shown in Table 2.
The main project Comparative result of oil product before and after certain wind park deterioration gear oil regeneration of table 2
Embodiment three：
3- Propanolamines 12g, this and ammonium hydroxide 5g and cetyl trimethylammonium bromide 90g is taken to be dissolved in 500g steamings respectively
In distilled water, pH value is adjusted to 11.5 with ammoniacal liquor and glacial acetic acid, and in 75 DEG C of stirred in water bath 5 hours, mixing speed was set to 800r/
Min, adds after water-soluble epoxy resin emulsion 12g and acrylic emulsion 7g and continues to stir 6 hours, add by CNT system
Standby particle diameter is 10nm or so powder 8.2g, continues to stir 3 hours, then by 120g white carbons, 35g sodium metasilicate, 120g bis-
Ethylmercury chloride aluminium, 8g aluminum sulfate, the mixture of 70g isopropyl titanates and 15g titanium sulfates are added thereto, and mixing speed is set to
1200r/min is persistently stirred 8 hours, is cooled down at room temperature, and the white Primogel product of gained is placed in 120 DEG C of convection ovens and done
Dry 15 hours, by gained white solid powder respectively with respectively washing three times, washing lotion water white transparency of absolute ethyl alcohol and distilled water.Again will
Gained white powder is transferred in microwave reaction kettle, and reactor pressure is 0.8MPa, and Power Control is small in 800W continuous heatings 3.0
When, natural cooling in air obtains highly polar mesoporous adsorbent.
When the gear oil deteriorated to certain wind park carries out regeneration treatment, the highly polar mesoporous adsorbent 3wt% is added,
In 65 DEG C of water-baths after heating stirring 30min, filtered with filter paper, with before processing index after testing the oil product after processing
Contrasted, the results are shown in Table 3.
The main project Comparative result of oil product before and after certain wind park deterioration gear oil regeneration of table 3
As can be seen from the above embodiments：Adsorbent of the present invention has good for the regeneration treatment of high viscosity wind power gear oil
Good additive effect, can remove the greasy filth in fluid, reduce the acid number of fluid, greatly improve the foam characteristic of fluid and wear-resistant
Performance, has reached the polarity ageing products removed in gear oil, extends the purpose of the service life of fluid.
Claims (10)
1. highly polar mesoporous adsorbent is used in a kind of wind power gear oil regeneration processing, it is characterised in that：The component bag of the adsorbent
Si, Al, Ti and C are included, Si, Al, Ti and C mol ratio are:(2~5)：(1~5)：1：(0.1~1.5)；The hole of the adsorbent
Footpath is 10~50nm, and specific surface area is 330~650m2/g。
2. highly polar mesoporous adsorbent is used in a kind of wind power gear oil regeneration processing according to claim 1, it is characterised in that：
Described Si, Al, Ti and C mol ratio are 3：2.5：1：0.8.
3. the preparation method of the highly polar mesoporous adsorbent of wind power gear oil regeneration processing described in any one of claim 1 to 2,
It is characterized in that：Comprise the following steps：
Step 1：It is (0.05~0.25) by weight ratio：It is molten that 1 organic amine and cetyl trimethylammonium bromide is configured to alkalescence
Liquid, pH is in the range of 8~12 for regulation, and is stirred 5 hours at 50~85 DEG C；
Step 2：The water soluble polymer emulsion that weight is accounted for into alkaline solution 5~17% is added to alkaline solution prepared by step 1
In, and stir more than 3 hours；
Step 3：The carbon source that weight is accounted for into alkaline solution 0.5~2.5% is added in alkaline solution prepared by step 2, and stirs 2
More than hour；
Step 4：It is (2~5) by Si, Al and Ti mol ratio：(1~5)：The mixture of 1 silicon source, silicon source and titanium source, violent
In the case of stirring, in the solution for being added to step 3 preparation, the addition of the mixture of silicon source, silicon source and titanium source cause Si,
Al, Ti and C mol ratio are (2~5)：(1~5)：1：(0.1~1.5), and continue stirring 8~15 hours, obtain white initial
Jel product；
Step 5：The white Primogel product that step 4 is obtained is placed in 80~120 DEG C of convection ovens more than 15 hours, is obtained
White solid powder；
Step 6：The white solid powder that step 5 is obtained is washed more than 3 times with absolute ethyl alcohol, then with distillation water washing 3 times
More than, untill cleaning fluid water white transparency, obtain the former powder of white micro-porous adsorption agent；
Step 7：The former powder of white micro-porous adsorption agent that step 5 is obtained is transferred in microwave reaction kettle, under the conditions of microwave radiation
Heating, the reactor pressure is 0.5~1.0MPa, and 1~3 hour time, Power Control obtains highly polar Jie in 500~1000W
Hole adsorbent.
4. preparation method according to claim 3, it is characterised in that：PH regulations described in step 1 use ammoniacal liquor or hydrogen-oxygen
Change sodium and dust technology or glacial acetic acid is adjusted；Organic amine described in step 1 is ethylenediamine, formamide, 3- Propanolamines, dipropyl
Amine, tetraethyl ammonium hydroxide or TPAOH.
5. preparation method according to claim 3, it is characterised in that：Water soluble polymer emulsion described in step 2 is benzene
Acrylic emulsion or acrylic emulsion or ethylene copolymerization emulsions or epoxy resin latex or one kind in its modified emulsion or
Its mixture, the average grain diameter of emulsion is in the range of 50~100nm, and solid content is in the range of 45~65%, when for two kinds when,
Mixed for arbitrary proportion.
6. preparation method according to claim 3, it is characterised in that：Carbon source described in step 3 is graphite or carbon nanometer
One kind or its mixture in pipe, and in nano powdery, when for two kinds when, be arbitrary proportion mixing.
7. preparation method according to claim 3, it is characterised in that：Silicon source described in step 4 is sodium metasilicate, Ludox,
One or more in silica gel, white carbon, when for it is a variety of when, be arbitrary proportion mixing.
8. preparation method according to claim 3, it is characterised in that：Silicon source described in step 4 is aluminium hydroxide, meta-aluminic acid
One kind in aluminum sulfate, aluminium chloride in salt, aluminate, triisobutyl aluminium and diethyl aluminum chloride or inorganic aluminium compound.
9. preparation method according to claim 3, it is characterised in that：Titanium source described in step 4 is metatitanic acid in organic titanium esters
One kind in titanium sulfate, titanium chloride in butyl ester, isopropyl titanate or inorganic titanium compound.
10. preparation method according to claim 3, it is characterised in that：Heated in microwave reaction kettle described in step 6 in sky
Carried out under gas or oxygen atmosphere.
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