CN106421798A - Preparation method of layered composite nanomaterial M-LDHs@SiO2 microspheres - Google Patents

Preparation method of layered composite nanomaterial M-LDHs@SiO2 microspheres Download PDF

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CN106421798A
CN106421798A CN201610873935.XA CN201610873935A CN106421798A CN 106421798 A CN106421798 A CN 106421798A CN 201610873935 A CN201610873935 A CN 201610873935A CN 106421798 A CN106421798 A CN 106421798A
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ldhs
microballoon
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王辉
张峰
赵立芳
卫粉艳
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Baoji University of Arts and Sciences
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
    • A61K31/19—Carboxylic acids, e.g. valproic acid
    • A61K31/192—Carboxylic acids, e.g. valproic acid having aromatic groups, e.g. sulindac, 2-aryl-propionic acids, ethacrynic acid 
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/24—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing atoms other than carbon, hydrogen, oxygen, halogen, nitrogen or sulfur, e.g. cyclomethicone or phospholipids

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Abstract

The invention discloses a preparation method of layered composite nanomaterial M-LDHs@SiO2 microspheres. The method comprises steps as follows: step 1, M(OH)2 is prepared with a precipitation method and dried at the normal temperature, and an M(OH)2 initial raw material is obtained; step 2, a large number of the M(OH)2 initial raw materials in step 1 and benzoic acid are weighed, a large amount of deionized water is added, the three materials are evenly mixed and react in microwaves, and M-LDHs are prepared; step 3, SiO2 microspheres are synthesized; step 4, the M-LDHs@SiO2 microspheres are synthesized. The composite microsphere particle M-LDHs@SiO2 microspheres are prepared from nano SiO2 microspheres with advantages of smooth surface, uniform particle size, good dispersity and the like and with characteristics of large specific surface area and quantum size effect of nano particles, the problems that existing nano drug-loading materials are poor in targeting, low in drug loading capacity and poor in slow release effect are solved, and the method is simple and has good use value.

Description

A kind of lamellar composite nano material M-LDHs@Si02The preparation method of microballoon
Technical field
The invention belongs to sustained release composite nano-microsphere technical field is and in particular to a kind of lamellar composite nano material M- LDHs@Si02The preparation method of microballoon.
Background technology
With the fast development of economic society, a large amount of waste water that various industry, agricultural and daily routines produce, waste gas, useless Slag makes environment increasingly deteriorate, and these environmental problems bring serious threat to the existence of the mankind and health, for example, cause to dislike Property tumour, diabetes, the incidence of disease of cardio-cerebrovascular diseases greatly improve.For the treatment of these diseases, traditional administration side , there is the shortcomings of administration number of times is many, and bioavilability is low, poor selectivity, toxic and side effect is big in formula.Therefore, medicine how is made more to pacify Entirely, more effectively, solve the poor selectivity of medicine, be the huge difficult problem that scientific research personnel faces the problems such as toxic and side effect is big.
Nano medication Transmission system has the characteristic of slow release and targeting, can deliver to medicine according to the change of pathology Diseased region, plays the greatest treatment efficacy of medicine, simultaneously Drug controlled release speed so that blood concentration stable safe range it Interior, thus reducing what medicine caused toxicity to human body, therefore show wide application prospect in field of pharmaceutical preparations. At present, layered double hydroxide (LDHs) conduct of the features such as have that security performance is high, cheap, be easy to surface modification The new nanometer medicine-carried system carrier material of one class, shows good security, biocompatibility and biodegradability, can Improve medicine stability and curative effect, mitigate bad reaction, be beneficial to realize slow controlled release drug administration, have a extensive future.But due to it The problems such as targeting is strong, drugloading rate is little, slow release effect is good, especially has well to specific cells system in cell multiplex system Targeted delivery inefficiency, also there is a problem of certain in the application.
Content of the invention
It is an object of the invention to provide a kind of lamellar composite nano material M-LDHs@Si02The preparation method of microballoon, solves The problem that existing nano drug-carrying material targeting is strong, drugloading rate is little, slow release effect is not good.
A kind of present invention lamellar composite nano material M-LDHs@Si02The preparation method of microballoon, the technical scheme being adopted Comprise the following steps：
Step 1, prepares M (OH) by the precipitation method2, and air drying process is carried out to it, obtain M (OH)2Initial feed；
Step 2, weighs the M (OH) of some steps 12Initial feed and benzoic acid, put in container, add some deionizations Water, is reacted after three is mixed in microwave, produces M-LDHs；
Step 3, synthesizes SiO2Microballoon；
Step 4, weighs the SiO in the M-LDHs and step 3 in some steps 22Microballoon, puts in container, and adds Ionized water, ethanol, carry out synthetic reaction after four are mixed in microwave, obtain product M-LDHs@Si02Microballoon.
The present invention is further characterized in that,
M(OH)2Solid, M-LDHs and M-LDHs@Si02M in microballoon is any one in transition metal Zn or Ni.
Concretely comprising the following steps in step 2：
Step 2.1, according to material amount than for 1：1 measures M (OH)2Initial feed and benzoic acid, put in container, simultaneously Add deionized water 15～20ml, three is mixed；
Step 2.2, the material that step 2.1 is processed carries out synthetic reaction 30～50min in microwave, obtains reactant liquor；
Step 2.3, the reactant liquor of step 2.2. is carried out suction filtration, is precipitated thing, and sediment is carried out at normal temperatures 5 ～6 deionized water washings；
Step 2.4, the sediment after step 2.3 is processed carries out room temperature to 50 DEG C of drying 20～24h, obtains M-LDHs.
Step 3 be specially：
Step 3.1, according to volume ratio 1.6：1.5：1 measures deionized water, ammoniacal liquor and ethanol and is mixedly configured into solution A；
Step 3.2, is 5 according to volume ratio：1 measures ethanol and tetraethyl orthosilicate and is mixedly configured into B solution；
Step 3.3, the B solution that step 3.2 is obtained is slowly added dropwise the solution A in the step 3.1 to stirring, is mixed Close solution；
Step 3.4, the mixed solution in step 3.3 is sealed reaction 22～26h at normal temperatures, obtains reactant liquor；
Step 3.5, the reactant liquor in step 3.4 is centrifuged, is precipitated thing, carries out deionization to sediment Water washing 3～5 times, air drying, obtain SiO2Microballoon.
The concretely comprising the following steps of step 4：
Step 4.1, weighing mass ratio is 1：1 M-LDHs and SiO2Microballoon, the volume of deionized water is 7.5～15ml, The volume of ethanol is 7.5～15ml, puts in container and mixes；
Step 4.2, the material after step 4.1 is processed carries out synthetic reaction 40～60min in microwave, reacted Liquid；
Step 4.3, the reactant liquor of step 4.2 is carried out suction filtration, is precipitated thing, and sediment is carried out at normal temperatures 5 ～6 deionized water washings；
Step 4.4, the sediment of step 4.3 is carried out drying at room temperature 20～24h, obtains product M-LDHs@Si02Microballoon.
In step 2.2 carrying out synthetic reaction in microwave and put into condition it is：Temperature is 60～100 DEG C, microwave power 400 ～600W.
In step 4.2 carrying out synthetic reaction in microwave and put into condition it is：Temperature is 60～100 DEG C, microwave power 500 ～800W.
The invention has the beneficial effects as follows：A kind of present invention lamellar composite nano material M-LDHs@Si02The preparation side of microballoon Method is passed through using the Nano-meter SiO_2 with smooth surface, particle diameter unification, favorable dispersibility2Microballoon, and have nanometer concurrently Particle specific surface area is big, quantum size effect feature, prepares complex microsphere particle M-LDHs@Si02Microballoon, solves existing receiving The problem that rice medicine carrying material targeting is not strong, drugloading rate is little, slow release effect is not good, method is simple, has good use value.
Brief description
Fig. 1 is the SEM figure of Ni-LDHs in the embodiment of the present invention 2；
Fig. 2 is Ni-LDHs@Si0 in the embodiment of the present invention 22The SEM figure of microballoon；
Fig. 3 is Ni-LDHs and Ni-LDHs@Si0 in the embodiment of the present invention 22The slow release effect figure to brufen for the microballoon；
Fig. 4 is the SEM figure of Zn-LDHs in the embodiment of the present invention 3；
Fig. 5 is Zn-LDHs@Si0 in the embodiment of the present invention 32The SEM figure of microballoon；
Fig. 6 is Zn-LDHs and Zn-LDHs@Si0 in the embodiment of the present invention 32The slow release effect figure to brufen for the microballoon.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of present invention lamellar composite nano material M-LDHs@Si02The preparation method of microballoon, comprises the following steps：
Step 1, prepares M (OH) by the precipitation method2, and air drying process is carried out to it, obtain M (OH)2Initial feed；
Step 2, weighs the M (OH) of some steps 12Initial feed and benzoic acid, put in container, add some deionizations Water, is reacted after three is mixed in microwave, produces M-LDHs；
Step 3, synthesizes SiO2Microballoon；
Step 4, weighs the SiO in the M-LDHs and step 3 in some steps 22Microballoon, puts in container, and adds Ionized water, ethanol, carry out synthetic reaction after four are mixed in microwave, obtain product M-LDHs@Si02Microballoon.
M(OH)2Solid, M-LDHs and M-LDHs@Si02M in microballoon is any one in transition metal Zn or Ni.
Concretely comprising the following steps in step 2：
Step 2.1, according to material amount than for 1：1 measures M (OH)2Initial feed and benzoic acid, put in container, simultaneously Add deionized water 15～20ml, three is mixed；
Step 2.2, the material that step 2.1 is processed carries out synthetic reaction 30～50min in microwave, obtains reactant liquor；
Step 2.3, the reactant liquor of step 2.2. is carried out suction filtration, is precipitated thing, and sediment is carried out at normal temperatures 5 ～6 deionized water washings；
Step 2.4, the sediment after step 2.3 is processed carries out room temperature to 50 DEG C of drying 20～24h, obtains M-LDHs.
The concretely comprising the following steps of step 3：
Step 3.1, according to volume ratio 1.6：1.5：1 measures deionized water, ammoniacal liquor and ethanol and is mixedly configured into solution A；
Step 3.2, is 5 according to volume ratio：1 measures ethanol and tetraethyl orthosilicate and is mixedly configured into B solution；
Step 3.3, the B solution that step 3.2 is obtained is slowly added dropwise the solution A in the step 3.1 to stirring, is mixed Close solution；
Step 3.4, the mixed solution in step 3.3 is sealed reaction 22～26h at normal temperatures, obtains reactant liquor；
Step 3.5, the reactant liquor in step 3.4 is centrifuged, is precipitated thing, carries out deionization to sediment Water washing 3～5 times, air drying, obtain SiO2Microballoon.
The concretely comprising the following steps of step 4：
Step 4.1, weighing mass ratio is 1：1 M-LDHs and SiO2Microballoon, the volume of deionized water is 7.5～15ml, The volume of ethanol is 7.5～15ml, puts in container and mixes；
Step 4.2, the material after step 4.1 is processed carries out synthetic reaction 40～60min in microwave, reacted Liquid；
Step 4.3, the reactant liquor of step 4.2 is carried out suction filtration, is precipitated thing, and sediment is carried out at normal temperatures 5 ～6 deionized water washings；
Step 4.4, the sediment of step 4.3 is carried out drying at room temperature 20～24h, obtains product M-LDHs@Si02Microballoon.
In step 2.2 carrying out synthetic reaction in microwave and put into condition it is：Temperature is 60～100 DEG C, microwave power 400 ～600W.
In step 4.2 carrying out synthetic reaction in microwave and put into condition it is：Temperature is 60～100 DEG C, microwave power 500 ～800W.
Embodiment 1
The preparation of a.Ni-LDHs material
Nickel nitrate solution 200ml, 0.8mol.L-1 sodium hydroxide solution 200mL of configuration 0.5mol.L-1 is raw material, Under room temperature, sodium hydroxide solution is slowly added in nickel nitrate solution, is stirred continuously and so that it is mixed, after question response is complete, Suction filtration after standing 7h, sediment is washed with deionized 4 times, drying at room temperature 22h, obtains the Ni (OH) of green at room temperature2 Initial feed.
According to material amount than for 1：1 Ni (OH) measuring green2Initial feed and benzoic acid, put in container, simultaneously Add deionized water 15ml, three is mixed, be 60 DEG C in temperature, carry out Hydrothermal Synthesiss under the conditions of microwave power 400w anti- Answer 30min, suction filtration, and sediment is carried out at normal temperatures 6 deionized water washings, then drying at room temperature 22h, obtain Ni- LDHs.
b.Si02The preparation of microballoon
Measure ethanol solution 20.0mL, ammoniacal liquor 30.0mL and deionized water 31.5mL respectively, be solution A after mixing；Measure Ethanol solution 50.0mL, tetraethyl orthosilicate 11.0mL are B solution after being thoroughly mixed；B solution is slowly added dropwise to by magnetic agitation In the solution A of device stirring, the 24h of sealing reaction at normal temperatures, obtain reactant liquor, reactant liquor is centrifuged, be precipitated Thing, carries out deionized water and washs 3 times to sediment, and air drying obtains SiO2Microballoon.
C. carry out Ni-LDHs@Si02The preparation of microballoon
Si0 by 0.100gNi-LDHs and 0.100g2Microballoon with and 10.0mL deionized water, 10.0mL ethanol in three necks Mix in flask, at 100 DEG C, under the conditions of microwave power 500w, synthetic reaction 40min suction filtration, is precipitated thing, and will sink Starch carries out 5 deionized water washings at normal temperatures；Sediment is carried out drying at room temperature 20h, obtains product Ni-LDHs@Si02 Microballoon.
Embodiment 2
The preparation of a.Ni-LDHs material
Nickel nitrate solution 100ml, 0.8mol.L-1 sodium hydroxide solution 100mL of configuration 0.5mol.L-1 is raw material, Under room temperature, sodium hydroxide solution is slowly added in nickel nitrate solution, is stirred continuously and so that it is mixed, after question response is complete, Suction filtration after standing 5h, sediment is washed with deionized 6 times, drying at room temperature 20h, obtains the Ni (OH) of green at room temperature2 Initial feed.
According to material amount than for 1：1 Ni (OH) measuring green2Initial feed and benzoic acid, put in container, simultaneously Add deionized water 18ml, three is mixed, be 100 DEG C in temperature, under the conditions of microwave power 600w, carry out Hydrothermal Synthesiss Reaction 50min, suction filtration, and sediment is carried out at normal temperatures 6 deionized water washings, then drying at room temperature 20h, obtain Ni- LDHs, as shown in Figure 1.
b.Si02The preparation of microballoon
Measure ethanol solution 20.0mL, ammoniacal liquor 30.0mL and deionized water 31.5mL respectively, be solution A after mixing；Measure Ethanol solution 50.0mL, tetraethyl orthosilicate 11.0mL are B solution after being thoroughly mixed；B solution is slowly added dropwise to by magnetic agitation In the solution A of device stirring, the 24h of sealing reaction at normal temperatures, obtain reactant liquor, reactant liquor is centrifuged, be precipitated Thing, carries out deionized water and washs 4 times to sediment, and air drying obtains SiO2Microballoon.
C. carry out Ni-LDHs@Si02The preparation of microballoon
Si0 by 0.100gNi-LDHs and 0.100g2Microballoon with and 15.0mL deionized water, 15.0mL ethanol in three necks Mix in flask, at 60 DEG C, under the conditions of microwave power 800w, synthetic reaction 50min suction filtration, is precipitated thing, and will precipitate Thing carries out 6 deionized water washings at normal temperatures；Sediment is carried out drying at room temperature 22h, obtains product Ni-LDHs@Si02Micro- Ball, as shown in Figure 2.
d.Ni-LDHs、Ni-LDHs@Si02The slow releasing function to medicine ibuprofen raw material medicine solution (IBU) for the microballoon
Medicine ibuprofen raw material medicine solution (IBU) is processed：First brufen active compound is dissolved in sodium hydroxide solution, brufen The ratio of the amount of the material of active compound and sodium hydroxide solution is 1：In 1, it is filtered to remove insoluble matter, filtrate is standby.
Take 1gNi-LDHs@Si02Microballoon and 10ml brufen raw material medicine solution (IBU), mix and are placed in container, stir Mix 2h, under temperature 60 C, place 24h, filter, be washed with deionized precipitation, be then dried at normal temperatures, you can obtain Ni- LDHs/IBU@Si02Sample；Take 1g Ni-LDHs and brufen raw material medicine solution, mix and be placed in container, stir 2h, Place 24h under temperature 60 C, filter, be washed with deionized precipitation, be then dried at normal temperatures, prepare Ni-LDHs/IBU sample Product.
Respectively by Ni-LDHs/IBU@SiO2Sample and Ni-LDHs/IBU sample are added to pH for 7.4 under the conditions of 37 DEG C Phosphate buffer solution in (mass/volume than for 0.2g/500mL), stirring；Every 20 minutes, take 4mL suspension, and supplement Enter 4mL phosphate buffer, filter, and (at 264nm) measures its absorbance on ultraviolet-visible spectrophotometer, its result is such as Shown in Fig. 3.
Embodiment 3
The preparation of a.Zn-LDHs material
The zinc nitrate solution 100ml of configuration 0.5mol.L-1,0.8mol.L-1 sodium hydroxide solution 100mL are raw material, Under room temperature, sodium hydroxide solution is slowly added in zinc nitrate solution, is stirred continuously and so that it is mixed, after question response is complete, Suction filtration after standing 3h, sediment is washed with deionized 5 times, and 24h is dried at 50 DEG C, obtain the Zn of white at room temperature (OH)2Initial feed.
According to material amount than for 1：1 Zn (OH) measuring white2Initial feed and benzoic acid, put in container, simultaneously Add deionized water 20ml, three mixed, be 90 DEG C in temperature, carry out under the conditions of microwave power 500w reacting 40min, Suction filtration, and sediment is carried out at room temperature 6 deionized water washings, then 50 DEG C are dried 24h, obtain Zn-LDHs, such as Fig. 4 Shown.
b.Si02The preparation of microballoon
Measure ethanol solution 20.0mL, ammoniacal liquor 30.0mL and deionized water 31.5mL respectively, be solution A after mixing；Measure Ethanol solution 50.0mL, tetraethyl orthosilicate 11.0mL are B solution after being thoroughly mixed；B solution is slowly added dropwise to by magnetic agitation In the solution A of device stirring, the 26h of sealing reaction at normal temperatures, obtain reactant liquor, reactant liquor is centrifuged, be precipitated Thing, carries out deionized water and washs 5 times to sediment, and air drying obtains SiO2Microballoon.
C. carry out Zn-LDHs@Si02The preparation of microballoon
Si0 by 0.08gZn-LDHs and 0.08g2Microballoon and 7.5mL deionized water, 7.5mL ethanol are in three-neck flask Mix, at 90 DEG C, carry out synthetic reaction 60min, suction filtration respectively under the conditions of microwave power 600w, be precipitated thing, and will Sediment carries out 6 deionized water washings at normal temperatures；Sediment is carried out drying at room temperature 24h, obtains product Zn-LDHs@ Si02Microballoon, as shown in Figure 5.
d.Zn-LDHs、Zn-LDHs@Si02The slow releasing function to medicine ibuprofen raw material medicine solution (IBU) for the microballoon
Medicine ibuprofen raw material medicine solution (IBU) is processed：First brufen active compound is dissolved in sodium hydroxide solution, brufen The ratio of the amount of the material of active compound and sodium hydroxide solution is 1：In 1, it is filtered to remove insoluble matter, filtrate is standby.
Take 1g Zn-LDHs@Si02Microballoon and 10ml brufen raw material medicine solution (IBU), mix and are placed in container, Stirring 2h, places 24h under temperature 60 C, filters, is washed with deionized precipitation, is then dried at normal temperatures, you can obtain Zn-LDHs/IBU@Si02Sample；Take 1gZn-LDHs and brufen raw material medicine solution, mix and be placed in container, stir 2h, Place 24h under temperature 60 C, filter, be washed with deionized precipitation, be then dried at normal temperatures, prepare Zn-LDHs/IBU Sample.
Respectively by Zn-LDHs/IBU@SiO2Sample and Zn-LDHs/IBU sample are added to pH for 7.4 under the conditions of 37 DEG C Phosphate buffer solution in (mass/volume than for 0.2g/500mL), stirring；Every 20 minutes, take 4mL suspension, and supplement Enter 4mL phosphate buffer, filter, and (at 264nm) measures its absorbance on ultraviolet-visible spectrophotometer, its result is such as Shown in Fig. 6.
From Fig. 1～Fig. 6, the M-LDHs of stratiform is equably wrapped in SiO2On microballoon, overall pattern is complete, with routine M-LDHs compares, M-LDHs@SiO2Microballoon has loose porous pattern, can adsorb medicine；M-LDHs/IBU absorbance is big, Brufen in solution is many, and slow releasing function is poor, M-LDHs/IBU@SiO2Absorbance is little, and the brufen in solution is few, slow releasing function Good, medicament slow release is acted on good, solve that existing nano drug-carrying material targeting is strong, drugloading rate is little, slow release effect is not good Problem.

Claims (7)

1. a kind of lamellar composite nano material M-LDHs@Si02The preparation method of microballoon is it is characterised in that comprise the following steps：
Step 1, prepares M (OH) by the precipitation method2, and air drying process is carried out to it, obtain M (OH)2Initial feed；
Step 2, weighs the M (OH) of some steps 12Initial feed and benzoic acid, put in container, add some deionized waters, will Three is reacted after mixing in microwave, produces M-LDHs；
Step 3, synthesizes SiO2Microballoon；
Step 4, weighs the SiO in the M-LDHs and step 3 in some steps 22Microballoon, puts in container, and adds deionization Water, ethanol, carry out synthetic reaction after four are mixed in microwave, obtain product M-LDHs@Si02Microballoon.
2. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 12The preparation method of microballoon, its feature It is, described M (OH)2Solid, M-LDHs and M-LDHs@Si02M in microballoon is arbitrary in transition metal Zn or Ni Kind.
3. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 12The preparation method of microballoon, its feature It is, concretely comprising the following steps in described step 2：
Step 2.1, according to material amount than for 1：1 measures M (OH)2Initial feed and benzoic acid, put in container, are simultaneously introduced Deionized water 15～20ml, three is mixed；
Step 2.2, the material that step 2.1 is processed carries out synthetic reaction 30～50min in microwave, obtains reactant liquor；
Step 2.3, the reactant liquor of step 2.2. is carried out suction filtration, is precipitated thing, and sediment is carried out at normal temperatures 5～6 Secondary deionized water washing；
Step 2.4, the sediment after step 2.3 is processed carries out room temperature to 50 DEG C of drying 20～24h, obtains M-LDHs.
4. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 12The preparation method of microballoon, its feature It is, being specially of described step 3：
Step 3.1, according to volume ratio 1.6：1.5：1 measures deionized water, ammoniacal liquor and ethanol and is mixedly configured into solution A；
Step 3.2, is 5 according to volume ratio：1 measures ethanol and tetraethyl orthosilicate and is mixedly configured into B solution；
Step 3.3, the B solution that step 3.2 is obtained is slowly added dropwise the solution A in the step 3.1 to stirring, obtains mixing molten Liquid；
Step 3.4, the mixed solution in step 3.3 is sealed reaction 22～26h at normal temperatures, obtains reactant liquor；
Step 3.5, the reactant liquor in step 3.4 is centrifuged, is precipitated thing, carries out deionization washing to sediment Wash 3～5 times, air drying, obtain SiO2Microballoon.
5. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 12The preparation method of microballoon, its feature It is, the concretely comprising the following steps of described step 4：
Step 4.1, weighing mass ratio is 1：1 M-LDHs and SiO2Microballoon, the volume of deionized water is 7.5～15ml, ethanol Volume is 7.5～15ml, puts in container and mixes；
Step 4.2, the material after step 4.1 is processed carries out synthetic reaction 40～60min in microwave, obtain reactant liquor；
Step 4.3, the reactant liquor of step 4.2 is carried out suction filtration, is precipitated thing, and sediment is carried out 5～6 times at normal temperatures Deionized water is washed；
Step 4.4, the sediment of step 4.3 is carried out drying at room temperature 20～24h, obtains product M-LDHs@Si02Microballoon.
6. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 32The preparation method of microballoon, its feature It is, in described step 2.2 carrying out synthetic reaction in microwave and put into condition be：Temperature is 60～100 DEG C, microwave power 400～600W.
7. a kind of lamellar composite nano material M-LDHs@Si0 according to claim 52The preparation method of microballoon, its feature It is, in described step 4.2 carrying out synthetic reaction in microwave and put into condition be：Temperature is 60～100 DEG C, microwave power 500～800W.
CN201610873935.XA 2016-09-30 2016-09-30 Preparation method of layered composite nanomaterial M-LDHs@SiO2 microspheres Pending CN106421798A (en)

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CN110255977A (en) * 2019-06-24 2019-09-20 中国路桥工程有限责任公司 High-grade asphalt mixture and preparation method thereof

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