CN102513044A - Surface modification method of nanometer aluminum oxide - Google Patents

Surface modification method of nanometer aluminum oxide Download PDF

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Publication number
CN102513044A
CN102513044A CN2011104240528A CN201110424052A CN102513044A CN 102513044 A CN102513044 A CN 102513044A CN 2011104240528 A CN2011104240528 A CN 2011104240528A CN 201110424052 A CN201110424052 A CN 201110424052A CN 102513044 A CN102513044 A CN 102513044A
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aluminium oxide
nano aluminium
coupling agent
organic solvent
surface modifying
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李岩
宋美慧
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Institute of Advanced Technology of Heilongjiang Academy of Sciences
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Institute of Advanced Technology of Heilongjiang Academy of Sciences
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Abstract

The invention discloses a surface modification method of nanometer aluminum oxide, which relates to the surface treatment method of aluminum oxide and aims to solve the problem that the dispersibility of the surface-modified nanometer aluminum oxide prepared by the prior physical methods is worse or the process of the prior chemical methods is complex. The method comprises the following steps of 1, weighing nanometer aluminum oxide, organic solvent I and coupling agent; 2, transferring the dispersed nanometer aluminum oxide and organic solvent I into a round-bottom flask, adding the coupling agent, then adding hydrochloric acid, heating the materials in a water bath to reach 20 to 60 DEG C, and reflowing for 30 to 120min to obtain suspension; and 3, cooling and then filtering the suspension, centrifuging and separating the filter waste after being dipped in organic solvent II, and drying the obtained solid in a vacuum drying oven to complete the surface modification of nanometer aluminum oxide. The preparation process discloses by the invention is simple; the activation index of the obtained product is from 96 to 100 percent, so that the dispersibility and compatibility of the obtained product in organic materials are improved. The method disclosed by the invention is used for preparing surface-modified nanometer aluminum oxide.

Description

The surface modifying method of nano aluminium oxide
Technical field
The present invention relates to the surface treatment method of aluminium oxide.
Background technology
Nanometer technology fast development in recent years, nano material gains great popularity with its special physics and chemical property.The research of nano material begins from fields such as metal dust, potteries, is widely used in fields such as microelectronics, chemical industry, national defence, space flight at present.Nanometer Al 2O 3Be a kind of novel high function fine inorganic material, since the mid-80 Gleiter etc. made the nano-alumina powder end, people constantly deepened the understanding of this new high-tech material, and find its numerous characteristics.Nano aluminium oxide has high strength, high rigidity, Heat stability is good, series of characteristics such as high temperature resistant, wear-resisting and corrosion-resistant because of it; And be widely used in the modified filler of organic materials such as rubber, plastics, fiber, resin; Bring advantages of excellent stability, reinforcement property to material, and performances such as good optics and machinery.
But nanometer Al 2O 3Specific area big, the surface can be high; Be easy to produce and reunite, poor with the compatibility of plastics, rubber etc., be difficult to be dispersed in the organic matrix; Direct or too much filling often causes the mechanical properties decrease and the easy embrittlement of material easily, thereby has hindered the application prospect of nano aluminium oxide.Adopt surface modification to improve the dispersiveness of nano aluminium oxide at present, become a big focus of nano material application technology.
Nanometer Al 2O 3Surface modifying method mainly contain physics method and chemical method.Physical modification mainly adopts mechanical force to disperse and ultrasonic dispersing, and mechanical force disperses mainly to reach the purpose that particle disperses by high-speed stirred and high speed ball milling; Ultrasonic dispersing is localized hyperthermia, high pressure or strong shock wave and the microjet etc. that produce when utilizing ultrasonic cavitation, and the interaction energy between the reduction nano particle prevents nanometer Al 2O 3Reunite and make it and disperse.The nanometer water imbibition is strong, so nano particle and hydrone form hydrogen bond and crosslinked together, merely with physical method to nanometer Al 2O 3Modification is carried out on the surface, and the products therefrom dispersiveness is relatively poor, and effect is not very desirable.
Chemical method mainly is meant selects for use suitable dispersant to disperse to cooperate and the protection of newborn particle when carrying out mechanical force disperses.Adding the bigger decentralized medium of some polarity during dispersion can increase wetting power, reduces the free energy of liquid-solid interface, improves the decentralization of nano particle; Dispersant can also change the electrical property of powder surface simultaneously, increases the reunion again that electrostatic repulsion reduces dispersed particle; The other macromolecule dispersing agent can also increase sterically hindered effect through increasing the polymer substance adsorbent layer thickness, to reach the purpose that suppresses particle agglomeration.But prepare the chemical method complex process of surface-modified nano aluminium oxide at present, cost is higher.
Summary of the invention
The present invention will solve the problem of the dispersed relatively poor or existing chemical method complex process of surface-modified nano aluminium oxide of existing physical method preparation, and a kind of surface modifying method of nano aluminium oxide is provided.
The surface modifying method of nano aluminium oxide is to carry out according to the following steps: one, take by weighing 100 parts of nano aluminium oxides, 100~10000 parts of organic solvent I, 1~15 part of coupling agent by ratio of weight and the number of copies; Two, the nano aluminium oxide and the organic solvent I that step 1 are taken by weighing join in the container, transfer in the round-bottomed flask behind ultrasonic dispersion 10~80min, under the condition of magnetic agitation; In round-bottomed flask, add the coupling agent that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 1~5mol/L again, the pH value of mixed liquor is 3~5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 20~60 ℃; Backflow 30~120min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding organic solvent II is embathed filter residue in centrifuge tube again, behind centrifugal 15~30min, topple over the liquid that centrifugal spectators; The gained solid is dried 12~48h in 50~70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.
The invention has the beneficial effects as follows: 1, used in process of production organic solvent, can utilize again after the recovery, not only reduced production cost, also make full use of resource, reduce discharging, help environmental protection; 2, preparation technology of the present invention is simple, and reaction condition is gentle, and energy consumption is low, is fit to industrial mass production; 3, the modified Nano aluminium oxide that obtains of the present invention, activation index is 96%~100%, is difficult for reuniting; Increased substantially it at macromolecular material; Especially dispersiveness in the elastomeric material and compatibility can be prepared high nano powder content, finely dispersed composite, have so both given full play to inorganic nanoparticles and macromolecular material advantage separately; Can also realize the optimal design of functional material, thereby have a wide range of applications in field of nanocomposite materials.
The specific embodiment
The specific embodiment one: the surface modifying method of the nano aluminium oxide of this embodiment is to carry out according to the following steps: one, take by weighing 100 parts of nano aluminium oxides, 100~10000 parts of organic solvent I, 1~15 part of coupling agent by ratio of weight and the number of copies; Two, the nano aluminium oxide and the organic solvent I that step 1 are taken by weighing join in the container, transfer in the round-bottomed flask behind ultrasonic dispersion 10~80min, under the condition of magnetic agitation; In round-bottomed flask, add the coupling agent that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 1~5mol/L again, the pH value of mixed liquor is 3~5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 20~60 ℃; Backflow 30~120min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding organic solvent II was embathed filter residue in centrifuge tube again, centrifugal 15~30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 12~48h in 50~70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.
Organic solvent I and organic solvent II used in this embodiment can recyclings.
Ultrasonic power is 30~50kHz in the step 1, and the rotating speed of magnetic agitation is 100~250r/min in the step 2, and centrifuge speed is 1000~5000r/min in the step 3, and the vacuum in the vacuum drying chamber is 1Pa.
The beneficial effect of this embodiment is: 1, used in process of production organic solvent, can utilize again after the recovery, and not only reduced production cost, also make full use of resource, reduce discharging, help environmental protection; 2, this embodiment preparation technology is simple, and reaction condition is gentle, and energy consumption is low, is fit to industrial mass production; 3, the modified Nano aluminium oxide that obtains of this embodiment, activation index is 96%~100%, is difficult for reuniting; Increased substantially it at macromolecular material; Especially dispersiveness in the elastomeric material and compatibility can be prepared high nano powder content, finely dispersed composite, have so both given full play to inorganic nanoparticles and macromolecular material advantage separately; Can also realize the optimal design of functional material, thereby have a wide range of applications in field of nanocomposite materials.
The specific embodiment two: this embodiment with the difference of the specific embodiment one is: nano aluminium oxide is that particle diameter is the powder of 20~80nm in the step 1.Other is identical with the specific embodiment one.
The specific embodiment three: this embodiment with the specific embodiment one or two difference is: the organic solvent I in the step 1 is aromatic hydrocarbon, alcohol, ether, ester, ketone, acid amides, aliphatic hydrocarbon or alicyclic.Other is identical with the specific embodiment one or two.
The specific embodiment four: this embodiment with the specific embodiment one or two difference is: the organic solvent I in the step 1 is propyl alcohol or absolute ethyl alcohol.Other is identical with the specific embodiment one or two.
The specific embodiment five: this embodiment and the specific embodiment one or one of four difference are: the coupling agent in the step 1 is titanate coupling agent NTC401, a kind of among titanate coupling agent CT136 and the titanate coupling agent JSC or wherein several kinds.Other is identical with one of the specific embodiment one or four.
The specific embodiment six: this embodiment with one of the specific embodiment one or fives' difference is: take by weighing 1000~8000 parts of organic solvent I in the step 1,2~12 parts coupling agent.Other is identical with one of the specific embodiment one or five.
The specific embodiment seven: this embodiment with one of the specific embodiment one or sixs' difference is: water bath heating temperature is 30~50 ℃ in the step 2, and 50~100min refluxes.Other is identical with one of the specific embodiment one or six.
The specific embodiment eight: this embodiment with one of the specific embodiment one or sevens' difference is: the organic solvent II in the step 3 is aromatic hydrocarbon, alcohol, ether, ester, ketone, acid amides, aliphatic hydrocarbon or alicyclic.Other is identical with one of the specific embodiment one or seven.
The specific embodiment nine: this embodiment and the specific embodiment one or one of seven difference are that the organic solvent II in the step 3 is propyl alcohol or absolute ethyl alcohol.Other is identical with one of the specific embodiment one or seven.
The specific embodiment ten: this embodiment with one of the specific embodiment one or nines' difference is: the gained solid is dried 24~36h in the step 3 in 55~65 ℃ of vacuum drying chambers.Other is identical with one of the specific embodiment one or nine.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment 1
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 20nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 2000 parts of isopropyl alcohols, 15 parts of titanate coupling agent CT136; Two, the nano aluminium oxide and the isopropyl alcohol that step 1 are taken by weighing join in the container, are under the ultrasonic power of 40kHZ at power, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min; At rotating speed is under the magnetic agitation condition of 150r/min, in round-bottomed flask, adds the titanate coupling agent CT136 that takes by weighing in the step 1, adds the hydrochloric acid solution that concentration is 3mol/L again; The pH value of mixed liquor is 3.5 to the round-bottomed flask; The round-bottomed flask water-bath is heated to 50 ℃, and backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 24h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.
Estimate the dispersiveness of the nano aluminium oxide of surface modification through detecting activation index, present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
The assay method of activation index: taking by weighing quality is W 1The alumina samples of surface modification, add and fill in the beaker of distilled water, fully stir and leave standstill more than the 1h, will fall to the feed separation of beaker bottom then, (W weighs after the drying 2).With former state quality (W 1) deduct its sedimentation part quality (W 2), can obtain the quality (W of floating part in the sample 1-W 2).Through formula 1, calculate activation index R.
R=(W 1-W 2)/W 1 (1)
Embodiment 2
What present embodiment and embodiment 1 were different is, water bath heating temperature is 40 ℃ in the step 2, and reflux time is 90min.Other is identical with embodiment 1.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 3
What present embodiment and embodiment 1 were different is, water bath heating temperature is 30 ℃ in the step 2, and reflux time is 120min.Other is identical with embodiment 1.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 4
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 60nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 5000 parts of absolute ethyl alcohols, 15 parts of titanate coupling agent JSC; Two, the nano aluminium oxide and the absolute ethyl alcohol that step 1 are taken by weighing join in the container, are under the ultrasonic power of 40kHZ at power, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min; At rotating speed is under the magnetic agitation condition of 250r/min, in round-bottomed flask, adds the titanate coupling agent JSC that takes by weighing in the step 1, adds the hydrochloric acid solution that concentration is 2mol/L again; The pH value of mixed liquor is 3 to the round-bottomed flask; The round-bottomed flask water-bath is heated to 60 ℃, and backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding propyl alcohol embathed filter residue in centrifuge tube again, centrifugal 25min toppled over the liquid that in the centrifuge tube; The gained solid is dried 36h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 5
What present embodiment and embodiment 4 were different is that reflux time is 90min in the step 2.Other is identical with embodiment 4.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 6
What present embodiment and embodiment 4 were different is that reflux time is 120min in the step 2.Other is identical with embodiment 4.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 7
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 80nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 5000 parts of absolute ethyl alcohols, 15 parts of titanate coupling agent NTC401; Two, the nano aluminium oxide and the absolute ethyl alcohol that step 1 are taken by weighing join in the container, are under the ultrasonic power of 30kHZ at power, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min; At rotating speed is under the magnetic agitation condition of 100r/min, in round-bottomed flask, adds the titanate coupling agent NTC401 that takes by weighing in the step 1, adds the hydrochloric acid solution that concentration is 5mol/L again; The pH value of mixed liquor is 5 to the round-bottomed flask; The round-bottomed flask water-bath is heated to 45 ℃, and backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 36h in 60 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 96%.
Embodiment 8
What present embodiment and embodiment 7 were different is that reflux time is 90min in the step 2.Other is identical with embodiment 7.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 96%.
Embodiment 9
What present embodiment and embodiment 7 were different is that reflux time is 120min in the step 2.Other is identical with embodiment 7.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 96%.
Embodiment 10
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 20nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 10000 parts of isopropyl alcohols, 7.5 parts of titanate coupling agent CT136 and 7.5 parts of titanate coupling agent JSC; Two, the nano aluminium oxide and the isopropyl alcohol that step 1 are taken by weighing join in the container; At power is under the ultrasonic power of 40kHZ, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min, and be under the magnetic agitation condition of 150r/min at rotating speed; In round-bottomed flask, add titanate coupling agent CT136 and the titanate coupling agent JSC that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 5mol/L again, the pH value of mixed liquor is 3.5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 50 ℃; Backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 24h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 11
What present embodiment and embodiment 10 were different is that reflux time is 90min in the step 2.Other is identical with embodiment 10.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 12
What present embodiment and embodiment 10 were different is that reflux time is 90min in the step 2.Other is identical with embodiment 10.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 100%.
Embodiment 13
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 20nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 10000 parts of absolute ethyl alcohols, 7.5 parts of titanate coupling agent NTC401 and 7.5 parts of titanate coupling agent JSC; Two, the nano aluminium oxide and the absolute ethyl alcohol that step 1 are taken by weighing join in the container; At power is under the ultrasonic power of 40kHZ, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min, and be under the magnetic agitation condition of 180r/min at rotating speed; In round-bottomed flask, add titanate coupling agent NTC401 and the titanate coupling agent JSC that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 1mol/L again, the pH value of mixed liquor is 3.5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 50 ℃; Backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 24h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 98%.
Embodiment 14
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 20nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 10000 parts of absolute ethyl alcohols, 7.5 parts of titanate coupling agent NTC401 and 7.5 parts of titanate coupling agent CT136; Two, the nano aluminium oxide and the absolute ethyl alcohol that step 1 are taken by weighing join in the container; At power is under the ultrasonic power of 40kHZ, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min, and be under the magnetic agitation condition of 180r/min at rotating speed; In round-bottomed flask, add titanate coupling agent NTC401 and the titanate coupling agent CT136 that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 1mol/L again, the pH value of mixed liquor is 3.5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 50 ℃; Backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 24h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 97.5%.
Embodiment 15
The surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide are to carry out according to the following steps: the aluminium oxide that is 20nm that, takes by weighing 100 parts of particle diameters by ratio of weight and the number of copies, 10000 parts of absolute ethyl alcohols, 5 parts of titanate coupling agent NTC401,5 parts of titanate coupling agent JSC and 5 parts of titanate coupling agent CT136; Two, the nano aluminium oxide and the absolute ethyl alcohol that step 1 are taken by weighing join in the container; At power is under the ultrasonic power of 40kHZ, transfer in the round-bottomed flask behind the ultrasonic dispersion 50min, and be under the magnetic agitation condition of 200r/min at rotating speed; In round-bottomed flask, add titanate coupling agent NTC401, titanate coupling agent JSC and the titanate coupling agent CT136 that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 5mol/L again, the pH value of mixed liquor is 3.5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 50 ℃; Backflow 30min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding absolute ethyl alcohol embathed filter residue in centrifuge tube again, centrifugal 30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 24h in 70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.Present embodiment technology is simple, and the activation index of the nano aluminium oxide of the surface modification of gained is 96.5%.

Claims (10)

1. the surface modifying method of nano aluminium oxide, the surface modifying method that it is characterized in that nano aluminium oxide is to carry out according to the following steps: one, take by weighing 100 parts of nano aluminium oxides, 100~10000 parts of organic solvent I, 1~15 part of coupling agent by ratio of weight and the number of copies; Two, the nano aluminium oxide and the organic solvent I that step 1 are taken by weighing join in the container, transfer in the round-bottomed flask behind ultrasonic dispersion 10~80min, under the condition of magnetic agitation; In round-bottomed flask, add the coupling agent that takes by weighing in the step 1; Add the hydrochloric acid solution that concentration is 1~5mol/L again, the pH value of mixed liquor is 3~5 to the round-bottomed flask, and the round-bottomed flask water-bath is heated to 20~60 ℃; Backflow 30~120min obtains suspension; Three, the suspension that step 2 is obtained filters after being cooled to room temperature; The filter residue that obtains is transferred in the centrifuge tube; After the adding organic solvent II was embathed filter residue in centrifuge tube, centrifugal 15~30min toppled over the liquid that in the centrifuge tube; The gained solid is dried 12~48h in 50~70 ℃ of vacuum drying chambers, accomplish the surface modification of nano aluminium oxide.
2. the surface modifying method of nano aluminium oxide according to claim 1 is characterized in that nano aluminium oxide is that particle diameter is the powder of 20~80nm in the step 1.
3. the surface modifying method of nano aluminium oxide according to claim 2 is characterized in that the organic solvent I in the step 1 is aromatic hydrocarbon, alcohol, ether, ester, ketone, acid amides, aliphatic hydrocarbon or alicyclic.
4. the surface modifying method of nano aluminium oxide according to claim 2 is characterized in that the organic solvent I in the step 1 is propyl alcohol or absolute ethyl alcohol.
5. according to the surface modifying method of any described nano aluminium oxide of claim among the claim 1-4; It is characterized in that the coupling agent in the step 1 is titanate coupling agent NTC401, a kind of among titanate coupling agent CT136 and the titanate coupling agent JSC or wherein several kinds.
6. the surface modifying method of nano aluminium oxide according to claim 5 is characterized in that taking by weighing in the step 1 1000~8000 parts of organic solvent I, 2~12 parts coupling agent.
7. the surface modifying method of nano aluminium oxide according to claim 6 is characterized in that water bath heating temperature is 30~50 ℃ in the step 2, and 50~100min refluxes.
8. the surface modifying method of nano aluminium oxide according to claim 7 is characterized in that the organic solvent II in the step 3 is aromatic hydrocarbon, alcohol, ether, ester, ketone, acid amides, aliphatic hydrocarbon or alicyclic.
9. the surface modifying method of nano aluminium oxide according to claim 7 is characterized in that the organic solvent II in the step 3 is propyl alcohol or absolute ethyl alcohol.
10. according to the surface modifying method of any described nano aluminium oxide of claim in the claim 1,6,7,8 or 9, it is characterized in that the gained solid is dried 24~36h in the step 3 in 55~65 ℃ of vacuum drying chambers.
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CN103572507A (en) * 2012-07-24 2014-02-12 上海纳米技术及应用国家工程研究中心有限公司 Preparation method for antibiosis ultraviolet prevention silk fibroin nanofiber membrane
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CN106335116A (en) * 2016-08-27 2017-01-18 安徽省阜南志峰工艺品有限公司 Anti-ultraviolet and anti-aging treatment agent and preparing method thereof
CN108097200A (en) * 2016-11-25 2018-06-01 中国石油化工股份有限公司 A kind of method for preparing modified aluminas
CN108097200B (en) * 2016-11-25 2020-08-11 中国石油化工股份有限公司 Method for preparing modified alumina
CN109608230A (en) * 2018-12-28 2019-04-12 东南大学 A kind of modified nano-alumina material and its preparation method and application for promoting concrete corrosion-resistant performance
CN112961725A (en) * 2021-02-21 2021-06-15 上海中器实业有限公司 Environment-friendly lubricating oil additive and preparation method thereof
CN115477319A (en) * 2022-09-16 2022-12-16 无锡成旸科技股份有限公司 Anti-agglomeration composite powder and preparation method thereof

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Application publication date: 20120627