CN103342893A - Preparation method of uniformly dispersed nano-particle/polymer composite material - Google Patents
Preparation method of uniformly dispersed nano-particle/polymer composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a uniformly dispersed nano-particle/polymer composite material, which relates to the field of nano-particle/polymer copolymerization and blending and aims to solve the problems that nano-particles in the existing nano-particle/polymer composite material are serious in agglomeration and the characteristics of the nano-particles can not be exerted. The preparation method comprises the following steps of: 1, preparing sol; 2, preparing nano-particles; 3, preparing a nano-particle/polymer mixed solution; and 4, preparing the nano-particle/polymer composite material. The preparation method of the uniformly dispersed nano-particle/polymer composite material provides a new copolymerization method of nano-particles/polymers, the preparation process and required equipment are simple, low in cost and easy to implement, the nano-particles in the prepared nano-particle/polymer composite material are uniformly dispersed, the self-agglomeration phenomenon of the nano-particles is overcome, and a uniformly dispersed composite material is obtained, so that the preparation method can be applied to the field of nano-particle/polymer copolymerization and blending.
Description
Technical field
The present invention relates to nanoparticle/polymer composites copolymerizing and blending field.
Background technology
Along with the fast development of material industry, various matrix materials emerge in an endless stream, and polymer materials is the field because its good processability has a wide range of applications, as common polyethylene, polypropylene, polyimide etc.In order to improve its application performance, need in polymer materials, add various inorganic particulates, strengthen its corona-resistance property as adding aluminum oxide in to polyethylene, add dielectric ceramic in the polyimide and strengthen its specific inductivity.The inorganic particulate of nanoscale as bigger specific surface area, is widely used as adding particle because of its natural characteristics; But because its granularity is little, the surface energy height, agglomeration is serious when adding polymeric matrix to, can not bring into play its nano-meter characteristic well; Good nanoparticle dispersiveness in polymeric matrix is the precondition of nanoparticle/polymer composites preparation.
Summary of the invention
The present invention seeks in order to solve in existing nanoparticle/polymer composites the nanoparticle agglomeration seriously, and then can not bring into play the problem of nanoparticle characteristic, and a kind of preparation method of even dispersing nanometer particle/polymer composites is provided.
The evenly preparation method of dispersing nanometer particle/polymer composites, realization according to the following steps:
One, in ethylene glycol monomethyl ether, add nitrocalcite and cupric nitrate, under 40 ℃～60 ℃, behind stir speed (S.S.) stirring 20min～40min with 300r/min～500r/min, be cooled to 20 ℃～30 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind stir speed (S.S.) stirring 40min～80min with 300r/min～500r/min, leave standstill 20h～28h, get colloidal sol; Wherein, the ratio of the volume of described ethylene glycol monomethyl ether and the amount of substance of nitrocalcite be (3.65L～8.65L): 1mol, the mol ratio of cupric nitrate and nitrocalcite is (2～4): 1, the mol ratio of tetrabutyl titanate and nitrocalcite is (3.5～4.5): 1;
Two, gained colloidal sol in the step 1 is lighted, get powder, after powder ground 1h～2h with mortar, put into retort furnace, speed with 4 ℃/min～8 ℃/min, be warming up to 250 ℃～350 ℃, insulation 5h～7h, be cooled to room temperature, obtain solid, then with the rotating speed ball milling 3～5h of solid with 500r/min～700r/min, particle diameter＜50nm, obtain nanoparticle, again with nanoparticle and hydrophilic anion surfactant ball milling mixing 1h, place 100 ℃～140 ℃ oven dry 20h～28h down then; Wherein, the mass ratio of described hydrophilic anion surfactant and nano particle is (1～5): 100;
Three, in N,N-DIMETHYLACETAMIDE, add 4, the 4'-diaminodiphenyl oxide, the dissolving back adds the nanoparticle after the oven dry in the step 2, obtaining mixture, is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～900r/min in ultrasonic frequency then, adds pyromellitic acid anhydride, obtain nanoparticle/mixed with polymers solution, specifically finish according to the following steps:
A, pyromellitic dianhydride equivalent is divided into 10 parts, mixture is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～600r/min in frequency, adds 6 parts of pyromellitic dianhydrides successively, and add pitch time is 4min～6min at every turn; B, take off Vltrasonic device, under 0～5 ℃ environment, strengthen stirring velocity to 600r/min～900r/min, add remaining 4 parts of pyromellitic dianhydrides successively, be 9min～11min pitch time, all adds the back and continue to stir 1h, obtains nanoparticle/mixed with polymers solution; Wherein, the mass ratio of gained nanoparticle is (10mL～50mL): 1g in the volume of N,N-DIMETHYLACETAMIDE and the step 2, described 4, the mass ratio of gained nanoparticle is (0.60～3.25) in 4'-diaminodiphenyl oxide and the step 2: 1, and the mass ratio of gained nanoparticle is (0.64～3.58) in the pyromellitic dianhydride of adding and the step 2: 1;
Four, get gained nanoparticle/mixed with polymers solution in the step 3, be applied on glass, in air, leave standstill 10min～20min, put into the microwave vacuum drying case then, vacuumize and be 100Pa～160Pa, 70 ℃～90 ℃ oven dry 20min～40min down carry out the hyperthermic treatment of staged microwave again under normal pressure, 120～330 ℃, obtain nanoparticle/polymer composites, namely finish the preparation method of even dispersing nanometer particle/polymer composites.
A kind of preparation method of even dispersing nanometer particle/polymer composites among the present invention, a kind of method of new copolymerization is provided for nanoparticle/polymer composites, preparation technology and required equipment are simple, with low cost, implement easily, nanoparticle is uniformly dispersed in preparation gained nanoparticle/polymer composites, overcome nanoparticle from agglomeration, obtain finely dispersed matrix material, can be applied to nanoparticle/polymkeric substance copolymerizing and blending field.
Description of drawings
Fig. 1 is the sem photograph of gained nanoparticle/polymer composites section among the embodiment.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of the even dispersing nanometer particle/polymer composites of present embodiment, realize according to the following steps:
One, in ethylene glycol monomethyl ether, add nitrocalcite and cupric nitrate, under 40 ℃～60 ℃, behind stir speed (S.S.) stirring 20min～40min with 300r/min～500r/min, be cooled to 20 ℃～30 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind stir speed (S.S.) stirring 40min～80min with 300r/min～500r/min, leave standstill 20h～28h, get colloidal sol; Wherein, the ratio of the volume of described ethylene glycol monomethyl ether and the amount of substance of nitrocalcite be (3.65L～8.65L): 1mol, the mol ratio of cupric nitrate and nitrocalcite is (2～4): 1, the mol ratio of tetrabutyl titanate and nitrocalcite is (3.5～4.5): 1;
Two, gained colloidal sol in the step 1 is lighted, get powder, after powder ground 1h～2h with mortar, put into retort furnace, speed with 4 ℃/min～8 ℃/min, be warming up to 250 ℃～350 ℃, insulation 5h～7h, be cooled to room temperature, obtain solid, then with the rotating speed ball milling 3～5h of solid with 500r/min～700r/min, particle diameter＜50nm, obtain nanoparticle, again with nanoparticle and hydrophilic anion surfactant ball milling mixing 1h, place 100 ℃～140 ℃ oven dry 20h～28h down then; Wherein, the mass ratio of described hydrophilic anion surfactant and nano particle is (1～5): 100;
Three, in N,N-DIMETHYLACETAMIDE, add 4, the 4'-diaminodiphenyl oxide, the dissolving back adds the nanoparticle after the oven dry in the step 2, obtaining mixture, is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～900r/min in ultrasonic frequency then, adds pyromellitic acid anhydride, obtain nanoparticle/mixed with polymers solution, specifically finish according to the following steps:
A, pyromellitic dianhydride equivalent is divided into 10 parts, mixture is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～600r/min in frequency, adds 6 parts of pyromellitic dianhydrides successively, and add pitch time is 4min～6min at every turn; B, take off Vltrasonic device, under 0～5 ℃ environment, strengthen stirring velocity to 600r/min～900r/min, add remaining 4 parts of pyromellitic dianhydrides successively, be 9min～11min pitch time, all adds the back and continue to stir 1h, obtains nanoparticle/mixed with polymers solution; Wherein, the mass ratio of gained nanoparticle is (10mL～50mL): 1g in the volume of N,N-DIMETHYLACETAMIDE and the step 2, described 4, the mass ratio of gained nanoparticle is (0.60～3.25) in 4'-diaminodiphenyl oxide and the step 2: 1, and the mass ratio of gained nanoparticle is (0.64～3.58) in the pyromellitic dianhydride of adding and the step 2: 1;
Four, get gained nanoparticle/mixed with polymers solution in the step 3, be applied on glass, in air, leave standstill 10min～20min, put into the microwave vacuum drying case then, vacuumize and be 100Pa～160Pa, 70 ℃～90 ℃ oven dry 20min～40min down carry out the hyperthermic treatment of staged microwave again under normal pressure, 120～330 ℃, obtain nanoparticle/polymer composites, namely finish the preparation method of even dispersing nanometer particle/polymer composites.
Embodiment two: the difference of present embodiment and embodiment one is: the ratio of the volume of the ethylene glycol monomethyl ether in the described step 1 and the amount of substance of nitrocalcite is 6.67L:1mol, the mol ratio of cupric nitrate and nitrocalcite is 3:1, and the mol ratio of tetrabutyl titanate and nitrocalcite is 4:1.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or twos' difference is: in the described step 1 under 50 ℃, behind the stir speed (S.S.) stirring 30min with 400r/min, be cooled to 25 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind the stir speed (S.S.) stirring 50min with 400r/min, leave standstill 24h.Other step and parameter are identical with embodiment one or two.
Embodiment four: the difference of one of present embodiment and embodiment one to three is: after in the described step 2 powder being ground 1.5h with mortar, put into retort furnace, speed with 6 ℃/min, be warming up to 300 ℃, insulation 6h, be cooled to room temperature, obtain solid, then with the rotating speed ball milling 4h of solid with 600r/min.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: the difference of one of present embodiment and embodiment one to four is: the hydrophilic anion surfactant is Sodium dodecylbenzene sulfonate in the described step 2.Other step and parameter are identical with one of embodiment one to four.
Embodiment six: the difference of one of present embodiment and embodiment one to five is: the mass ratio of gained nanoparticle is 31.7mL:1g in the volume of the N,N-DIMETHYLACETAMIDE in the described step 3 and the step 2, described 4, the mass ratio of gained nanoparticle is 1.90:1 in 4'-diaminodiphenyl oxide and the step 2, and the mass ratio of gained nanoparticle is 2.09:1 in the pyromellitic acid anhydride of adding and the step 2.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: the difference of one of present embodiment and embodiment one to six is: 0～5 ℃ environment in the described step 3 is to adopt mixture of ice and water.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: the difference of one of present embodiment and embodiment one to seven is: be 5min adding pitch time of 6 parts of pyromellitic dianhydrides in the described step 3; Are 10min adding pitch times of remaining 4 parts of pyromellitic dianhydrides.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: the difference of one of present embodiment and embodiment one to eight is: leave standstill 15min in the described step 4 in air, put into the microwave vacuum drying case then, vacuumize and be 130Pa, 80 ℃ of oven dry 30min down.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: the difference of one of present embodiment and embodiment one to nine is: carry out the hyperthermic treatment of staged microwave in the described step 4 under normal pressure, 120 ℃～330 ℃: at 120 ℃ of constant temperature 30min, continue heating then, at 165 ℃ of constant temperature 30min, at 235 ℃ of constant temperature 30min, at 260 ℃ of constant temperature 1h, at 285 ℃ of constant temperature 1h, at 330 ℃ of constant temperature 1h.Other step and parameter are identical with one of embodiment one to nine.
Embodiment:
Adopt following verification experimental verification effect of the present invention:
The evenly preparation method of dispersing nanometer particle/polymer composites, realization according to the following steps:
One, in ethylene glycol monomethyl ether, adds nitrocalcite and cupric nitrate, under 50 ℃, behind the stir speed (S.S.) stirring 30min with 400r/min, be cooled to 25 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind the stir speed (S.S.) stirring 60min with 400r/min, leave standstill 24h, get colloidal sol; Wherein, the ratio of the volume of described ethylene glycol monomethyl ether and the amount of substance of nitrocalcite is 6.67L:1mol, and the mol ratio of cupric nitrate and nitrocalcite is 3:1, and the mol ratio of tetrabutyl titanate and nitrocalcite is 4:1;
Two, gained colloidal sol in the step 1 is lighted, is got powder, powder is ground 1.5h with mortar after, put into retort furnace, with the speed of 5 ℃/min, be warming up to 300 ℃, insulation 6h, be cooled to room temperature, obtain solid, then with the rotating speed ball milling 4h of solid with 600r/min, particle diameter＜50nm, obtain nanoparticle, again with nanoparticle and Sodium dodecylbenzene sulfonate ball milling mixing 1h, the nanoparticle after will handling is afterwards dried 20h～28h down at 100 ℃～140 ℃; Wherein, the mass ratio of described Sodium dodecylbenzene sulfonate and nano particle is 2:100.
Three, in N,N-DIMETHYLACETAMIDE, add 4, the 4'-diaminodiphenyl oxide, the dissolving back adds the nanoparticle of drying in the step 2, obtaining mixture, is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～900r/min in ultrasonic frequency then, adds pyromellitic acid anhydride, obtain nanoparticle/mixed with polymers solution, specifically finish according to the following steps:
A, pyromellitic dianhydride equivalent is divided into 10 parts, mixture is that 60kHz, stir speed (S.S.) are under the condition of 500r/min in frequency, adds 6 parts of pyromellitic dianhydrides successively, and add pitch time is 5min at every turn; B, take off Vltrasonic device, under 0 ℃ environment, strengthen stirring velocity to 700r/min, add remaining 4 parts of pyromellitic dianhydrides successively, be 10min pitch time, all adds the back and continue to stir 1h, obtains nanoparticle/mixed with polymers solution; Wherein, the mass ratio of gained nanoparticle is 31.7mL:1g in the volume of N,N-DIMETHYLACETAMIDE and the step 2, described 4, the mass ratio of gained nanoparticle is 1.90:1 in 4'-diaminodiphenyl oxide and the step 2, and the mass ratio of gained nanoparticle is 2.09:1 in the pyromellitic acid anhydride of adding and the step 2;
Four, get gained nanoparticle/mixed with polymers solution in the step 3, be applied on glass, in air, leave standstill 15min, put into the microwave vacuum baking oven then, vacuumize and be 130Pa, dry 30min down for 80 ℃, again at normal pressure, be heated to 120 ℃ of constant temperature 30min, continue heating then, at 165 ℃ of constant temperature 30min, at 235 ℃ of constant temperature 30min, at 260 ℃ of constant temperature 1h, at 285 ℃ of constant temperature 1h, at 330 ℃ of constant temperature 1h, obtain nanoparticle/polymer composites, namely finish the preparation method of even dispersing nanometer particle/polymer composites.
The massfraction of the nanoparticle in the present embodiment in gained nanoparticle/polymer composites is 20%.
To gained nanoparticle/polymer composites brittle failure in liquid nitrogen in the present embodiment, with scanning electron microscopic observation mixture section, as shown in Figure 1.Fig. 1 is the sectional drawing of the scanning electron microscope of nanoparticle massfraction 20% matrix material, as can be seen from the figure nanoparticle is less than 50nm, and in polymeric matrix, be uniformly dispersed, nanoparticle is as growing on polymeric matrix, anionic show promoting agent can with the fine combination of nanoparticle, nanoparticle after the guaranteed processing of wetting ability can be scattered in the polar solvent well, illustrate the present invention can overcome nanoparticle from agglomeration, obtain finely dispersed matrix material.
Claims (10)
1. the preparation method of an even dispersing nanometer particle/polymer composites is characterized in that it realizes according to the following steps:
One, in ethylene glycol monomethyl ether, add nitrocalcite and cupric nitrate, under 40 ℃～60 ℃, behind stir speed (S.S.) stirring 20min～40min with 300r/min～500r/min, be cooled to 20 ℃～30 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind stir speed (S.S.) stirring 40min～80min with 300r/min～500r/min, leave standstill 20h～28h, get colloidal sol; Wherein, the ratio of the volume of described ethylene glycol monomethyl ether and the amount of substance of nitrocalcite be (3.65L～8.65L): 1mol, the mol ratio of cupric nitrate and nitrocalcite is (2～4): 1, the mol ratio of tetrabutyl titanate and nitrocalcite is (3.5～4.5): 1;
Two, gained colloidal sol in the step 1 is lighted, get powder, after powder ground 1h～2h with mortar, put into retort furnace, speed with 4 ℃/min～8 ℃/min, be warming up to 250 ℃～350 ℃, insulation 5h～7h, be cooled to room temperature, obtain solid, then with the rotating speed ball milling 3～5h of solid with 500r/min～700r/min, particle diameter＜50nm, obtain nanoparticle, again with nanoparticle and hydrophilic anion surfactant ball milling mixing 1h, place 100 ℃～140 ℃ oven dry 20h～28h down then; Wherein, the mass ratio of described hydrophilic anion surfactant and nano particle is (1～5): 100;
Three, in N,N-DIMETHYLACETAMIDE, add 4, the 4'-diaminodiphenyl oxide, the dissolving back adds the nanoparticle after the oven dry in the step 2, obtaining mixture, is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～900r/min in ultrasonic frequency then, adds pyromellitic acid anhydride, obtain nanoparticle/mixed with polymers solution, specifically finish according to the following steps:
A, pyromellitic dianhydride equivalent is divided into 10 parts, mixture is that 50kHz～70kHz, stir speed (S.S.) are under the condition of 400r/min～600r/min in frequency, adds 6 parts of pyromellitic dianhydrides successively, and add pitch time is 4min～6min at every turn; B, take off Vltrasonic device, under 0～5 ℃ environment, strengthen stirring velocity to 600r/min～900r/min, add remaining 4 parts of pyromellitic dianhydrides successively, be 9min～11min pitch time, all adds the back and continue to stir 1h, obtains nanoparticle/mixed with polymers solution; Wherein, the mass ratio of gained nanoparticle is (10mL～50mL): 1g in the volume of N,N-DIMETHYLACETAMIDE and the step 2, described 4, the mass ratio of gained nanoparticle is (0.60～3.25) in 4'-diaminodiphenyl oxide and the step 2: 1, and the mass ratio of gained nanoparticle is (0.64～3.58) in the pyromellitic dianhydride of adding and the step 2: 1;
Four, get gained nanoparticle/mixed with polymers solution in the step 3, be applied on glass, in air, leave standstill 10min～20min, put into the microwave vacuum drying case then, vacuumize and be 100Pa～160Pa, 70 ℃～90 ℃ oven dry 20min～40min down carry out the hyperthermic treatment of staged microwave again under normal pressure, 120～330 ℃, obtain nanoparticle/polymer composites, namely finish the preparation method of even dispersing nanometer particle/polymer composites.
2. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 1, the ratio that it is characterized in that the amount of substance of the volume of the ethylene glycol monomethyl ether in the step 1 and nitrocalcite is 6.67L:1mol, the mol ratio of cupric nitrate and nitrocalcite is 3:1, and the mol ratio of tetrabutyl titanate and nitrocalcite is 4:1.
3. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 1 and 2, it is characterized in that in the step 1 under 50 ℃, behind the stir speed (S.S.) stirring 30min with 400r/min, be cooled to 25 ℃, obtain mixing solutions, in mixing solutions, add tetrabutyl titanate, behind the stir speed (S.S.) stirring 50min with 400r/min, leave standstill 24h.
4. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 3, after it is characterized in that in the step 2 powder ground 1.5h with mortar, put into retort furnace, speed with 6 ℃/min, be warming up to 300 ℃, insulation 6h is cooled to room temperature, obtain solid, then with the rotating speed ball milling 4h of solid with 600r/min.
5. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 4 is characterized in that the hydrophilic anion surfactant is Sodium dodecylbenzene sulfonate in the step 2.
6. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 5, the mass ratio that it is characterized in that gained nanoparticle in the volume of the N,N-DIMETHYLACETAMIDE in the step 3 and the step 2 is 31.7mL:1g, described 4, the mass ratio of gained nanoparticle is 1.90:1 in 4'-diaminodiphenyl oxide and the step 2, and the mass ratio of gained nanoparticle is 2.09:1 in the pyromellitic acid anhydride of adding and the step 2.
7. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 6 is characterized in that 0～5 ℃ environment in the step 3 is to adopt mixture of ice and water.
8. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 7 is characterized in that be 5min adding pitch time of 6 parts of pyromellitic dianhydrides in the step 3; Are 10min adding pitch times of remaining 4 parts of pyromellitic dianhydrides.
9. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 8 is characterized in that leaving standstill 15min in the step 4 in air, puts into the microwave vacuum drying case then, vacuumizes to be 130Pa, dries 30min down for 80 ℃.
10. the preparation method of a kind of even dispersing nanometer particle/polymer composites according to claim 9, it is characterized in that in the step 4 under normal pressure, 120 ℃～330 ℃, carrying out the hyperthermic treatment of staged microwave: at 120 ℃ of constant temperature 30min, continue heating then, at 165 ℃ of constant temperature 30min, at 235 ℃ of constant temperature 30min, at 260 ℃ of constant temperature 1h, at 285 ℃ of constant temperature 1h, at 330 ℃ of constant temperature 1h.
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| CN103788459A (en) * | 2014-02-19 | 2014-05-14 | 哈尔滨理工大学 | Preparation method of nanometer bismuth hydroxide/polyethylene flame-retardant composite material |
| CN104945713A (en) * | 2015-06-23 | 2015-09-30 | 哈尔滨理工大学 | Preparing method for nanometer bismuth oxide and aluminum hydroxide/polyethylene flame-retardant composite material |
| CN109422838A (en) * | 2017-08-30 | 2019-03-05 | 天津大学 | The method of evenly dispersed nanoparticle in the polymer |
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| CN102924920A (en) * | 2012-11-23 | 2013-02-13 | 哈尔滨理工大学 | Amorphous calcium-copper-titanium-oxygen ceramic/polyimide composite film and preparation method thereof |
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| CN102924920A (en) * | 2012-11-23 | 2013-02-13 | 哈尔滨理工大学 | Amorphous calcium-copper-titanium-oxygen ceramic/polyimide composite film and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788459A (en) * | 2014-02-19 | 2014-05-14 | 哈尔滨理工大学 | Preparation method of nanometer bismuth hydroxide/polyethylene flame-retardant composite material |
| CN103788459B (en) * | 2014-02-19 | 2016-01-20 | 哈尔滨理工大学 | The preparation method of nanometer hydrogen-oxygen oxygen bismuth/polyethylene fire retardant composite material |
| CN104945713A (en) * | 2015-06-23 | 2015-09-30 | 哈尔滨理工大学 | Preparing method for nanometer bismuth oxide and aluminum hydroxide/polyethylene flame-retardant composite material |
| CN109422838A (en) * | 2017-08-30 | 2019-03-05 | 天津大学 | The method of evenly dispersed nanoparticle in the polymer |
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Application publication date: 20131009 |