CN106319972B - Organic silicon emulsion and preparation method thereof of the filtrate containing modified carbon nano-tube - Google Patents
Organic silicon emulsion and preparation method thereof of the filtrate containing modified carbon nano-tube Download PDFInfo
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Abstract
The invention proposes a kind of organic silicon emulsion and preparation method thereof of filtrate containing modified carbon nano-tube.The organic silicon emulsion containing modified carbon nano-tube, including following component, carbon nano tube dispersion liquid, silicone oil, organosiloxane, silane coupling agent, emulsifier, stabilizer and water.The present invention passes through the use to modified carbon nano-tube, and keep it fully dispersed in organic silicon emulsion, prepare a kind of organic silicon emulsion of the filtrate containing modified carbon nano-tube, by the excellent properties of carbon nanotube and the special nature of organic silicon emulsion, filter material surface effect can be improved, reach soft, smooth, waterproof refuses oily effect, and filtrate chemical-resistance, strainability are improved, while improving the high temperature resistance and antioxygenic property of filtrate to a certain extent.
Description
Technical field
The present invention relates to a kind of filtrate post-finishing agents, more particularly to a kind of organic silicon emulsion containing modified carbon nano-tube
Preparation method.Belong to auxiliary chemicals technical field.
Background technique
With the improvement of living standards, requirement of the common people to environmental quality is constantly improving；Government also pollutes for control
Total amount reduces pollution level and does effort, and the environmental regulation and discharge standard of formulation are increasingly strict.This facilitate operations simultaneously can
It leans on, is flexible and convenient to use, the development and progress of high dust collection efficiency sack cleaner.And the critical material of sack cleaner is filter
Material, chemical-resistance, high-temperature behavior, deashing property, the cleaning cycle for extending filtrate and the service life for improving filtrate are scientific researches
The direction of personnel's unremitting effort, while also determining the validity and economic feasibility of filtering.
Carbon nanotube is found in doctor lijima by Japanese NEC Corporation in 1991, is the typical case of monodimension nanometer material
It represents.By domestic and international years of researches, carbon nanotube possesses excellent conduction, mechanics, thermal stability, either intensity also
It is that toughness is all much better than any fiber, not only with the peculiar person's character of carbon materials, but also it is heat-resisting and corrosion-resistant with ceramic material
Property, it is considered to be following " super fiber " is had great expectations in the various aspects such as electricity field and catalyst carrier by people, and
The hot spot material of enhancing composite property at present.
Organic silicon emulsion is widely used in fields such as weaving, leathers as fabric finishing agent, fabric can be made to have
The features such as smooth, soft, good hand feeling, waterproof are wrinkle resistant, wear-resisting, heat-resisting.But it is directed to the organic silicon emulsion of filtrate, is especially deposited
The good organic silicon emulsion of storage stability is rarely reported.
Summary of the invention
The purpose of the present invention is by effective addition to carbon nanotube, prepare a kind of organic silicon emulsion and its preparation side
Method reaches soft, smooth to improve filter material surface effect, and waterproof refuses oily effect, and improve filtrate chemical-resistance,
Strainability, while the high temperature resistance and antioxygenic property of filtrate are improved to a certain extent.
To achieve the above object, solution of the invention is:
A kind of organic silicon emulsion of the filtrate containing modified carbon nano-tube comprising the ingredient of following quality proportioning:
The carbon nano tube dispersion liquid includes the ingredient of following quality proportioning:
0.1-2.0 parts of modified carbon nano-tube,
10.0 parts of organic solvent,
0.05-1.0 parts of surfactant.
The silicone oil is one of vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil or two kinds or two kinds
Above mixture.
The vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil dynamic viscosity are 25~5000mPas.
The vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil dynamic viscosity are 500~3000mPas.
The siloxanyl monomers are octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes
One of or two kinds or two or more of mixture.
The silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, methacryloxypropyl three
Methoxy silane, methacrylic acid methoxyl group propyl trimethoxy silicane, γ aminopropyltriethoxy silane, vinyl three
One of Ethoxysilane or two kinds or two or more of mixture.
The emulsifier is allyl polyethenoxy ether, ethoxylated dodecyl alcohol, castor oil polyoxyethylene ether, isomery ten
One of alcohol polyoxyethylene ether, isomery undecyl alcohol polyoxyethylene ether, isomerous tridecanol polyoxyethylene ether or two kinds or two kinds
Above mixture.
The stabilizer be one of polyvinyl alcohol, polyvinylpyrrolidone, Phenoxyethanol, carboxymethyl cellulose,
Or two kinds or two or more of mixture.
The modified carbon nano-tube is at least containing SWCNTs a kind of in the functional groups such as carboxyl, amino, hydroxyl or sulfydryl
One of (single-walled carbon nanotube), DWCNTs (double-walled carbon nano-tube) and MWCNTs (multi-walled carbon nanotube) or two kinds or two
Kind or more mixture.
The organic solvent is one of isopropanol, dichloro-benzenes, N-Methyl pyrrolidone or two kinds or two or more
Mixture.
The surfactant one of logical, neopelex, lauryl sodium sulfate or two for Qula
Kind or two or more mixtures.
The preparation method of organic silicon emulsion of the filtrate containing modified carbon nano-tube comprising following steps:
(1) preparation of carbon nano tube dispersion liquid；
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 50-65 DEG C of water-bath, mixing speed
300-500r/min is slowly added to silicone oil, is kept stirring 8-24h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, siloxanyl monomers, cream is added into mixed liquor
Agent, the stabilizer of half, water under low whipping speed 200-600r/min, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 200-600r/min, stirs 20min,
Obtain the organic silicon emulsion containing modified carbon nano-tube.
The preparation of carbon nano tube dispersion liquid in the step 1: for surfactant to be added to the beaker for being placed with organic solvent
In, the heating stirring 15-30min in 50-65 DEG C of water-bath dissolves surfactant sufficiently in organic solvent, takes out and burns
Cup, cooled to room temperature；It is slowly stirred and is gradually added into modified carbon nano-tube, makes the carbon nanotube complete wetting being added；So
Ultrasonic disperse afterwards, frequency 20-40KHz, processing time are 15-20min, take out and stand, and are further continued for after blibbing elimination
Ultrasonic disperse, supersonic frequency are set as 60-100KHz, and the processing time is 5-10min, further takes out standing, eliminate to blibbing
After be further continued for ultrasonic disperse, reciprocal 3 times, i.e., total ultrasonic time 60-90min；Dispersion liquid is placed in centrifuge, revolving speed 2000-
Obtained supernatant liquid is crossed 300-500 mesh filter cloth by 3000r/min, time 10min, obtains stand-by carbon nanotube dispersion
Liquid.
After adopting the above scheme, the present invention is by the use to modified carbon nano-tube, and fills it in organic silicon emulsion
Dispersion, prepares a kind of organic silicon emulsion of the filtrate containing modified carbon nano-tube.It can be effectively improved filter material surface effect, reached
To soft, smooth, waterproof refuses oily effect, and improves filtrate chemical-resistance, strainability, while to a certain extent
Improve the high temperature resistance and antioxygenic property of filtrate.
Specific embodiment
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to
Cross the conventional products of commercially available acquisition.
Present invention discloses a kind of organic silicon emulsion of filtrate containing modified carbon nano-tube comprising following quality proportioning
Ingredient:
The carbon nano tube dispersion liquid includes the ingredient of following quality proportioning:
0.1-2.0 parts of modified carbon nano-tube,
10.0 parts of organic solvent,
0.05-1.0 parts of surfactant.
The silicone oil is one of vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil or two kinds or two kinds
Above mixture.The vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil dynamic viscosity are 25~5000mPa
s.It is preferred that 500~3000mPas.For the working condition of filtrate complexity, phenyl silicone oil thermal stability is good, to UV stable,
Radiation resistance can improve filtrate oxidative resistance and high temperature resistance to a certain extent；Vinyl silicone oil, hydroxy silicon oil, amido silicon oil
It can be reacted with active group on modified carbon nano-tube, form covalently key connection, be grafted in carbon nanotube, performance is more stable.
The vinyl-terminated silicone fluid of the vinyl silicone oil preferred vinyl content 0.8mol%；The preferred phenyl of phenyl silicone oil contains
Measure the phenyl silicone oil of 25mol%；The hydroxy silicon oil of the preferred hydroxy radical content 8%wt. of hydroxy silicon oil；The preferred ammonia value of amido silicon oil is
The amido silicon oil of 0.6mmol/g.
The siloxanyl monomers are octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes
One of or two kinds or two or more of mixture.
The silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, methacryloxypropyl three
Methoxy silane, methacrylic acid methoxyl group propyl trimethoxy silicane, γ aminopropyltriethoxy silane, vinyl three
One of Ethoxysilane or two kinds or two or more of mixture.
The emulsifier is allyl polyethenoxy ether, ethoxylated dodecyl alcohol, castor oil polyoxyethylene ether, isomery ten
One of alcohol polyoxyethylene ether, isomery undecyl alcohol polyoxyethylene ether, isomerous tridecanol polyoxyethylene ether or two kinds or two kinds
Above mixture, preferably allyl polyethenoxy ether.
The allyl polyethenoxy ether, molecular weight 600-5000, preferred molecular weight are the allyl of 800-1500
Polyoxyethylene ether.
The stabilizer be one of polyvinyl alcohol, polyvinylpyrrolidone, Phenoxyethanol, carboxymethyl cellulose,
Or two kinds or two or more of mixture.Selected stabilizer is soluble in the aqueous phase, and increases system viscosity, increases latex inter-particle collisions
While resistance, in emulsion polymerization systems, it can be adsorbed on emulsion particle surface and form certain thickness hydrated sheath, hinder emulsifier phase
Mutually collision occurs to gather simultaneously；Phenoxyethanol may also function as the effect of preservative.
The modified carbon nano-tube is at least containing SWCNTs a kind of in the functional groups such as carboxyl, amino, hydroxyl or sulfydryl
One of (single-walled carbon nanotube), DWCNTs (double-walled carbon nano-tube) and MWCNTs (multi-walled carbon nanotube) or two kinds or two
Kind or more mixture.
The organic solvent is one of isopropanol, dichloro-benzenes, N-Methyl pyrrolidone or two kinds or two or more
Mixture.It is preferred that N-Methyl pyrrolidone.The organic solvent of selection is good with emulsion system conformability, avoids emulsion polymerization process
Middle dispersion liquid is unstable to be caused to polymerize the problems such as uneven.
The surfactant one of logical, neopelex, lauryl sodium sulfate or two for Qula
Kind or two or more mixtures.
The preparation method of organic silicon emulsion of the filtrate containing modified carbon nano-tube, it is characterized in that including the following steps:
(1) preparation of carbon nano tube dispersion liquid；
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 50-65 DEG C of water-bath, mixing speed
300-500r/min is slowly added to silicone oil, is kept stirring 8-24h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, siloxanyl monomers, cream is added into mixed liquor
Agent, the stabilizer of half, water under low whipping speed 200-600r/min, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 200-600r/min, stirs 20min,
Obtain the organic silicon emulsion containing modified carbon nano-tube.
Surfactant addition is placed in the beaker of organic solvent, in 50- by the preparation of the carbon nano tube dispersion liquid
Heating stirring 15-30min in 65 DEG C of water-baths, dissolves surfactant sufficiently in organic solvent, takes out beaker, naturally cold
But to room temperature；It is slowly stirred and is gradually added into modified carbon nano-tube, makes the carbon nanotube complete wetting being added；Then ultrasound point
It dissipating, frequency 20-40KHz, the processing time is 15-20min, takes out and stands, it is further continued for ultrasonic disperse after blibbing elimination,
Supersonic frequency is set as 60-100KHz, and the processing time is 5-10min, further takes out standing, is further continued for surpassing after blibbing elimination
Sound dispersion, reciprocal 3 times, i.e., total ultrasonic time 60-90min；Dispersion liquid is placed in centrifuge, revolving speed 2000-3000r/min, when
Between be 10min, obtained supernatant liquid is crossed into 300-500 mesh filter cloth, obtains stand-by carbon nano tube dispersion liquid.Heating appropriate
It can accelerate the dissolution of surfactant in organic solvent, but unsuitable high temperature easily causes solution muddy；Dispersion liquid ultrasonic procedure
Will appear fever, bubble phenomenon, in order to prevent persistently bubble and heating caused by dispersion liquid it is unstable, therefore sonication stage be arranged
Stand step.
The present invention is to increase stability of emulsion, is not added with inorganic salts or metal soap catalyst, but relies on surface living
The catalytic activity of property agent, plays the role of catalytic emulsion polymerization reaction, lotion prepare be added dropwise in whipping process a small amount of acetic acid or
When pH is 4-6, lotion preparation process can shorten system.
Embodiment 1:
Organic silicon emulsion of the present embodiment containing modified carbon nano-tube includes the ingredient of following quality proportioning,
Wherein carbon nano tube dispersion liquid, the ingredient including following quality proportioning,
0.1 part of multi-walled carbon nanotube of hydroxyl, amino,
10.0 parts of N-Methyl pyrrolidone,
0.05 part of neopelex.
Preparation method includes the following steps:
(1) neopelex the preparation of carbon nano tube dispersion liquid: is added to the burning for being placed with N-Methyl pyrrolidone
In cup, the heating stirring 15min in 65 DEG C of water-baths takes out beaker, cooled to room temperature；It is slowly stirred and is gradually added into and change
Property carbon nanotube, make be added carbon nanotube complete wetting；Then ultrasonic disperse, frequency 20KHz, processing time are 20min,
It takes out and stands, ultrasonic disperse is further continued for after blibbing elimination, supersonic frequency is set as 100KHz, and the processing time is 5min,
Standing is further taken out, is further continued for ultrasonic disperse after blibbing elimination, reciprocal 3 times, i.e., total ultrasonic time 75min；By dispersion liquid
It is placed in centrifuge, obtained supernatant liquid is crossed 300 mesh filter clothes, obtains stand-by carbon by revolving speed 3000r/min, time 10min
Nanotube dispersion liquid.
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 65 DEG C of water-baths, mixing speed
500r/min is slowly added to silicone oil, is kept stirring 8h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, ten diformazan basic rings six is added into mixed liquor
Siloxanes, allyl polyethenoxy ether, the polyvinylpyrrolidone of half and Phenoxyethanol, water, low whipping speed 600r/
Under min, 60min is stirred；
(4) silane coupling agent and remaining polyvinylpyrrolidone and Phenoxyethanol, low whipping speed 600r/ are added
Under min, 20min is stirred, the organic silicon emulsion containing modified carbon nano-tube is obtained.
Obtained lotion is uniformly applied on polyphenyl thioether filter material dust-collecting face, by 8 groups of different temperatures of stentering forming furnace
Baking oven, obtain coating filter material, oven temperature setting is respectively 150 DEG C of (from an area to 8th area), 165 DEG C, 180 DEG C, 180 DEG C,
195 DEG C, 195 DEG C, 200 DEG C, 200 DEG C.
Performance test: according to JB/T 11261-2012, filtrate traditional performance is tested；According to ISO5470-1YG522N, adopt
Filtrate wear-resisting property is tested with disc type fabric abrasion machine；According to GB/T4745-1997, tested using YG813 type degree of getting wet instrument
Filtrate waterproofing grade；According to AATCC 118:1997, the grease proofing grade of filtrate is tested；According to GB/T 6719-2009, filtered using VDI
Expect that experimental rig tests media filtration performance；Resistance to oxidation test is will not apply 1 filtrate sample of lotion PPS filtrate sample and embodiment
Product are cut into 5cm*200mm, immerse 20%HNO3In solution, 85 DEG C of heating are for 24 hours.Filtrate ultimate strength, comparison are measured after drying
Untreated samples simultaneously calculate strength retention.Test result is as follows shown in table.
Table 1
Embodiment 2
Organic silicon emulsion of the present embodiment containing modified carbon nano-tube includes the ingredient of following quality proportioning,
Wherein carbon nano tube dispersion liquid, the ingredient including following quality proportioning,
Preparation method includes the following steps:
(1) logical be added of Qula the preparation of carbon nano tube dispersion liquid: is placed with dichloro-benzenes and N-Methyl pyrrolidone mixed liquor
Beaker in, the heating stirring 25min in 60 DEG C of water-baths, take out beaker, cooled to room temperature；It is slowly stirred and gradually adds
Enter modified carbon nano-tube, makes the carbon nanotube complete wetting being added；Then ultrasonic disperse, frequency 25KHz, processing the time be
20min takes out and stands, and is further continued for ultrasonic disperse after blibbing elimination, and supersonic frequency is set as 60KHz, and the processing time is
10min further takes out standing, is further continued for ultrasonic disperse after blibbing elimination, and reciprocal 3 times, i.e., total ultrasonic time 90min；It will
Dispersion liquid is placed in centrifuge, and obtained supernatant liquid is crossed 300 mesh filter clothes by revolving speed 2000r/min, time 10min, obtain to
Carbon nano tube dispersion liquid.
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 60 DEG C of water-baths, mixing speed
300r/min, is slowly added to silicone oil, is kept stirring later for 24 hours；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, five silicon of decamethyl ring is added into mixed liquor
Oxygen alkane, emulsifier, the stabilizer of half, water under low whipping speed 400r/min, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 600r/min, stirs 20min, obtain
Organic silicon emulsion containing modified carbon nano-tube.
Obtained lotion is uniformly applied on glass fiber filter material dust-collecting face, by the baking of 8 groups of different temperatures of stentering forming furnace
Case, obtains coating filter material, and oven temperature setting is respectively 120 DEG C of (from an area to 8th area), and 120 DEG C, 160 DEG C, 160 DEG C, 160
DEG C, 200 DEG C, 200 DEG C, 225 DEG C.
Performance test: according to JB/T 11261-2012, filtrate traditional performance is tested；According to ISO5470-1YG522N, adopt
Filtrate wear-resisting property is tested with disc type fabric abrasion machine；According to GB/T4745-1997, tested using YG813 type degree of getting wet instrument
Filtrate waterproofing grade；According to AATCC 118:1997, the grease proofing grade of filtrate is tested；According to GB/T 6719-2009, filtered using VDI
Expect that experimental rig tests media filtration performance；Folding resistance test is will not apply 2 filtrate of lotion glass fiber filter material sample and embodiment
Sample is cut into 5cm*300mm batten, bends 150,000 times under 180 degree bending angle, compares untreated samples and calculates strength
Conservation rate.Test result is as follows shown in table.
Table 2
Embodiment 3
Organic silicon emulsion of the present embodiment containing modified carbon nano-tube includes the ingredient of following quality proportioning,
Wherein carbon nano tube dispersion liquid, the ingredient including following quality proportioning,
Preparation method includes the following steps:
(1) neopelex and lauryl sodium sulfate addition the preparation of carbon nano tube dispersion liquid: are placed with N-
In the beaker of methyl pyrrolidone, the heating stirring 30min in 50 DEG C of water-baths takes out beaker, cooled to room temperature；Slowly
Modified carbon nano-tube is stirred and be gradually added into, the carbon nanotube complete wetting being added is made；Then ultrasonic disperse, frequency 40KHz,
The processing time is 15min, takes out and stands, and is further continued for ultrasonic disperse after blibbing elimination, and supersonic frequency is set as 60KHz,
The processing time is 10min, further takes out standings, is further continued for ultrasonic disperse after blibbing elimination, reciprocal 3 times, i.e., when total ultrasonic
Between 75min；Dispersion liquid is placed in centrifuge, obtained supernatant liquid is crossed 300 mesh by revolving speed 2000r/min, time 10min
Filter cloth obtains stand-by carbon nano tube dispersion liquid.
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 50 DEG C of water-baths, mixing speed
300r/min is slowly added to silicone oil, is kept stirring 12h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, four silicon of prestox ring is added into mixed liquor
Six siloxanes of oxygen alkane and ten diformazan basic rings, allyl polyethenoxy ether, the stabilizer of half, water, low whipping speed 300r/min
Under, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 600r/min, stirs 20min, obtain
Organic silicon emulsion containing modified carbon nano-tube.
Obtained lotion is uniformly applied on aramid fiber filtrate dust-collecting face, by the baking of 8 groups of different temperatures of stentering forming furnace
Case, obtains coating filter material, and oven temperature setting is respectively 120 DEG C of (from an area to 8th area), and 145 DEG C, 160 DEG C, 160 DEG C, 175
DEG C, 190 DEG C, 200 DEG C, 200 DEG C.
Performance test: according to JB/T 11261-2012, filtrate traditional performance is tested；According to ISO5470-1YG522N, adopt
Filtrate wear-resisting property is tested with disc type fabric abrasion machine；According to GB/T4745-1997, tested using YG813 type degree of getting wet instrument
Filtrate waterproofing grade；According to AATCC 118:1997, the grease proofing grade of filtrate is tested；Acid proof test is will not apply the filter of lotion aramid fiber
Material sample and 3 filtrate sample of embodiment are cut into 5cm*200mm, immerse 40%H2SO4In solution, 85 DEG C are heated for 24 hours, after drying
Filtrate ultimate strength is measured, untreated samples are compared and calculates strength retention；Alkaline-resisting test is will not apply the filter of lotion aramid fiber
Material sample and 3 filtrate sample of embodiment are cut into 5cm*200mm, immerse in 10%NaOH solution, and 85 DEG C are heated for 24 hours, after drying
Filtrate ultimate strength is measured, untreated samples are compared and calculates strength retention；Heat-resisting quantity is will not apply the filter of lotion aramid fiber
Material sample and 3 filtrate sample of embodiment are cut into 5cm*200mm size, are placed in baking oven, and 300 DEG C of heating for 24 hours, are surveyed after cooling
Filtrate ultimate strength is measured, untreated samples are compared and calculates strength retention；According to GB/T 6719-2009, using VDI filtrate
Experimental rig tests media filtration performance.Test result is as follows shown in table.
Table 3
Embodiment 4
Organic silicon emulsion of the present embodiment containing modified carbon nano-tube includes the ingredient of following quality proportioning,
Wherein carbon nano tube dispersion liquid, the ingredient including following quality proportioning,
1.5 parts of multi-walled carbon nanotube containing carboxyl and sulfydryl,
10.0 parts of N-Methyl pyrrolidone,
0.5 part of neopelex.
Preparation method includes the following steps:
(1) neopelex the preparation of carbon nano tube dispersion liquid: is added to the burning for being placed with N-Methyl pyrrolidone
In cup, the heating stirring 20min in 65 DEG C of water-baths dissolves neopelex sufficiently in organic solvent, takes out
Beaker, cooled to room temperature；It is slowly stirred and is gradually added into modified carbon nano-tube, makes the carbon nanotube complete wetting being added；
Then ultrasonic disperse, frequency 40KHz, processing time are 15min, take out and stand, and are further continued for ultrasound after blibbing elimination
Dispersion, supersonic frequency are set as 100KHz, and the processing time is 5min, further take out standing, are further continued for surpassing after blibbing elimination
Sound dispersion, reciprocal 3 times, i.e., total ultrasonic time 60min；Dispersion liquid is placed in centrifuge, revolving speed 3000r/min, the time is
Obtained supernatant liquid is crossed 500 mesh filter clothes, obtains stand-by carbon nano tube dispersion liquid by 10min.
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 65 DEG C of water-baths, mixing speed
500r/min is slowly added to silicone oil, is kept stirring 8h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, ten diformazan basic rings six is added into mixed liquor
Siloxanes, emulsifier, the stabilizer of half, water under low whipping speed 200r/min, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 600r/min, stirs 20min, obtain
Organic silicon emulsion containing modified carbon nano-tube.
Obtained lotion is uniformly applied on polyimides filtrate dust-collecting face, by 8 groups of different temperatures of stentering forming furnace
Baking oven, obtain coating filter material, oven temperature setting is respectively 150 DEG C of (from an area to 8th area), 150 DEG C, 150 DEG C, 180 DEG C,
180 DEG C, 200 DEG C, 200 DEG C, 220 DEG C.
Performance test: according to JB/T 11261-2012, filtrate traditional performance is tested；According to ISO5470-1YG522N, adopt
Filtrate wear-resisting property is tested with disc type fabric abrasion machine；According to GB/T4745-1997, tested using YG813 type degree of getting wet instrument
Filtrate waterproofing grade；According to AATCC 118:1997, the grease proofing grade of filtrate is tested；According to GB/T 6719-2009, filtered using VDI
Expect that experimental rig tests media filtration performance；Acid proof test is will not apply 4 filtrate sample of lotion PI filtrate sample and embodiment
It is cut into 5cm*200mm, immerses 60%H2SO4In solution, 85 DEG C of heating for 24 hours, measure filtrate ultimate strength, comparison is not after drying
Processing sample simultaneously calculates strength retention；Alkaline-resisting test is will not apply lotion PI filtrate sample and 4 filtrate sample of embodiment sanction
It is cut into 5cm*200mm, is immersed in 0.5%NaOH solution, 85 DEG C of heating for 24 hours, measure filtrate ultimate strength after drying, comparison is not located
Reason sample simultaneously calculates strength retention；Heat-resisting quantity is will not apply lotion PI filtrate sample and the cutting of 4 filtrate sample of embodiment
It at 5cm*200mm size, is placed in baking oven, 320 DEG C of heating for 24 hours, measure filtrate ultimate strength after cooling, compare untreated sample
Product simultaneously calculate strength retention.Test result is as follows shown in table.
Table 4
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
The case where make changes, modifications, substitutions and variations to the above described embodiments and all belong to the scope of protection of the present invention.
Claims (8)
1. a kind of organic silicon emulsion of filtrate containing modified carbon nano-tube, which is characterized in that the ingredient including following quality proportioning:
10.15-13.0 parts of carbon nano tube dispersion liquid,
8.0-10.0 parts of silicone oil,
22.0-35.0 parts of siloxanyl monomers,
1.0-3.0 parts of silane coupling agent,
1.5-5.0 parts of emulsifier,
1.0 parts of stabilizer,
45.0-55.0 parts of distilled water；
The silicone oil is one of vinyl silicone oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil or two or more mixing
Object；
The siloxanyl monomers are octamethylcy-clotetrasiloxane, in decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes
One kind or two or more mixtures；
The silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane, methacryloxypropyl trimethoxy
Base silane, methacrylic acid methoxyl group propyl trimethoxy silicane, γ aminopropyltriethoxy silane, three ethoxy of vinyl
One of base silane or two or more mixtures；Include the following steps:
(1) preparation of carbon nano tube dispersion liquid: surfactant addition is placed in the beaker of organic solvent, in 50-65 DEG C of water
Heating stirring 15-30min in bath dissolves surfactant sufficiently in organic solvent, takes out beaker, naturally cools to room
Temperature；It is slowly stirred and is gradually added into modified carbon nano-tube, makes the modified carbon nano-tube complete wetting being added；Then ultrasonic disperse,
Frequency is 20-40KHz, and the processing time is 15-20min, takes out and stands, and is further continued for ultrasonic disperse after blibbing elimination, surpasses
Acoustic frequency is set as 60-100KHz, and the processing time is 5-10min, further takes out standing, is further continued for ultrasound after blibbing elimination
Dispersion, reciprocal 3 times, i.e., total ultrasonic time 60-90min；Dispersion liquid is placed in centrifuge, revolving speed 2000-3000r/min, time
For 10min, obtained supernatant liquid is crossed into 300-500 mesh filter cloth, obtains stand-by carbon nano tube dispersion liquid；The carbon modified is received
Mitron is at least containing single-walled carbon nanotube a kind of in carboxyl, amino, hydroxyl or mercapto functional group, double-walled carbon nano-tube and more
One of wall carbon nano tube or two or more mixtures；
(2) carbon nano tube dispersion liquid is placed in three-necked flask, the heating stirring in 50-65 DEG C of water-bath, mixing speed 300-
500r/min is slowly added to silicone oil, is kept stirring 8-24h later；
(3) mixed liquor taking-up in three-necked flask is placed in Simple stirrer, siloxanyl monomers, emulsification is added into mixed liquor
Agent, the stabilizer of half, distilled water under low whipping speed 200-600r/min, stir 60min；
(4) it adds silane coupling agent and remaining stabilizer, under low whipping speed 200-600r/min, stirs 20min, obtain
Organic silicon emulsion containing modified carbon nano-tube.
2. organic silicon emulsion of the filtrate as described in claim 1 containing modified carbon nano-tube, which is characterized in that the carbon nanometer
Pipe dispersion liquid includes the ingredient of following quality proportioning:
0.1-2.0 parts of modified carbon nano-tube,
10.0 parts of organic solvent,
0.05-1.0 parts of surfactant.
3. organic silicon emulsion of the filtrate as described in claim 1 containing modified carbon nano-tube, which is characterized in that vinyl silicon
Oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil dynamic viscosity are 25 ~ 5000mPas.
4. organic silicon emulsion of the filtrate as claimed in claim 3 containing modified carbon nano-tube, which is characterized in that vinyl silicon
Oil, phenyl silicone oil, hydroxy silicon oil, amido silicon oil dynamic viscosity are 500 ~ 3000mPas.
5. organic silicon emulsion of the filtrate as described in claim 1 containing modified carbon nano-tube, which is characterized in that the emulsifier
For allyl polyethenoxy ether, ethoxylated dodecyl alcohol, castor oil polyoxyethylene ether, heterogeneous ten alcohol polyoxyethylene ether, isomery
One of undecyl alcohol polyoxyethylene ether, isomerous tridecanol polyoxyethylene ether or two or more mixtures.
6. organic silicon emulsion of the filtrate as described in claim 1 containing modified carbon nano-tube, which is characterized in that the stabilizer
For one of polyvinyl alcohol, polyvinylpyrrolidone, Phenoxyethanol, carboxymethyl cellulose or two or more mixtures.
7. organic silicon emulsion of the filtrate as claimed in claim 2 containing modified carbon nano-tube, which is characterized in that described organic molten
Agent is one of isopropanol, dichloro-benzenes, N-Methyl pyrrolidone or two or more mixtures.
8. organic silicon emulsion of the filtrate as claimed in claim 2 containing modified carbon nano-tube, which is characterized in that the surface is living
Property agent be that Qula is logical, one of neopelex, lauryl sodium sulfate or two or more mixtures.
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