Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of preparation method of PET strap masterbatch, and the strap masterbatch prepared has good ageing-resistant performance, can be applicable to rugged environment.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution and stir 8 minutes, after suction filtration, washing 5 times with water, be placed in baking oven and dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains is added in the aqueous solution of palmityl trimethyl ammonium chloride, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in baking oven dry 10 hours, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in baking oven dry 8 hours, obtains modification pearl white;
(4) stirring 40 minutes by adding stirrer after the drying of PET pellet, adding modified coal ash drift pearl that step (2) obtains, modification pearl white that step (3) obtains continues stirring 2 hours, obtain PET strap masterbatch.
Preferably, in step of the present invention (1), the weight ratio of fly ash float, hydrofluoric acid solution is 1:25.
Preferably, in step of the present invention (1), the concentration of hydrofluoric acid solution is 0.5mol/L.
Preferably, in step of the present invention (1), the temperature of baking oven is 140 DEG C.
Preferably, in step of the present invention (2), the massfraction of the aqueous solution of palmityl trimethyl ammonium chloride is 5%, and the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36.
Preferably, in step of the present invention (2), the temperature of baking oven is 90 DEG C.
Preferably, in step of the present invention (3), pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer.
Preferably, in step of the present invention (3), the temperature of baking oven is 80 DEG C.
Preferably, in step of the present invention (4), count by weight, PET pellet 84-88 part, modified coal ash drift pearl 8-10 part, modification pearl white 4-6 part.
Preferably, in step of the present invention (4), the stirring velocity of stirrer is 800r/min.
Compared with prior art, the present invention has following beneficial effect:
(1) fly ash float is a kind of fly ash hollow ball that can bubble through the water column, there is the structure of hollow and thin-walled, be partial vacuum in cavity, therefore thermal conduction is atomic extremely slowly, there is good heat insulating function, its heat-proof quality can be effectively improved after adding PET, greatly weaken thermal destruction to the detrimentally affect of strap masterbatch, but there is a large amount of hydroxyls on fly ash float surface, show obvious wetting ability and polarity, cause the consistency between itself and PET matrix poor, dispersiveness after adding is not good yet, thus the present invention first carries out acidification by hydrofluoric acid to it, the hydroxyl on hydrofluoric acid and its surface reacts and reduces surface polarity, thus improve dispersiveness, then surface modification is carried out by cats product palmityl trimethyl ammonium chloride, the positively charged ion that palmityl trimethyl ammonium chloride ionizes out is adsorbed in fly ash float surface by electrostatic interaction and defines organic coating, the wetting ability on its surface is become hydrophobicity, improve the consistency between itself and PET matrix, thus its heat-proof quality can be given full play to, greatly reduce thermal destruction to its detrimentally affect, the ageing-resistant performance of effective raising strap masterbatch,
(2) pearl white has very high optical index, most of refraction of light can be gone out, but it is inorganics, surface also presents wetting ability, not good with the consistency of PET matrix, therefore the present invention by PAMAM half for tree shaped polymer to having carried out modification, the two has carried out abundant complexing, organic group is introduced on pearl white surface, the wetting ability on its surface is become hydrophobicity, improve the consistency between itself and PET matrix, effectively can improve the refraction of light ability of strap masterbatch, greatly reduce photodegradation to its detrimentally affect, further raising ageing-resistant performance, rugged environment can be applicable to.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 86 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 10 parts of steps (2) obtain, modification pearl white that 4 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
Embodiment 2
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 85 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 9 parts of steps (2) obtain, modification pearl white that 6 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
Embodiment 3
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 87 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 8 parts of steps (2) obtain, modification pearl white that 5 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
Embodiment 4
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 84 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 10 parts of steps (2) obtain, modification pearl white that 6 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
Embodiment 5
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 88 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 8 parts of steps (2) obtain, modification pearl white that 4 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
Embodiment 6
A preparation method for Novel PET strap masterbatch, comprises the following steps:
(1) fly ash float is washed, add hydrofluoric acid solution that concentration is 0.5mol/L and stir 8 minutes, the weight ratio of fly ash float, hydrofluoric acid solution is 1:25,5 times are washed with water after suction filtration, be placed in temperature be 140 DEG C baking oven dry 3 hours, obtain acidifying fly ash float;
(2) the acidifying fly ash float that step (1) obtains being added massfraction is in the aqueous solution of the palmityl trimethyl ammonium chloride of 5%, the weight ratio of the aqueous solution of acidifying fly ash float and palmityl trimethyl ammonium chloride is 1:36, ultrasonic agitation left standstill 2 hours after 2 hours, the acidifying fly ash float being suspended in upper strata is poured in filtering net together with being deposited in the acidifying fly ash float of bottom and filters, filter residue washes 5 times with water, be placed in dry 10 hours of the baking oven that temperature is 90 DEG C, obtain modified coal ash drift pearl;
(3) pearl white is added to the water stirring 30 minutes obtained suspension, suspension is added PAMAM half in the aqueous solution of tree shaped polymer, pearl white and PAMAM half is 1:1 for the mol ratio of tree shaped polymer, magnetic agitation 24 hours, filter after discharging, filter residue absolute ethanol washing 5 times, is placed in dry 8 hours of the baking oven that temperature is 80 DEG C, obtains modification pearl white;
(4) count by weight, 40 minutes are stirred by adding stirrer after the drying of 86 parts of PET pellets, the stirring velocity of stirrer is 800r/min, add modified coal ash drift pearl that 9.5 parts of steps (2) obtain, modification pearl white that 4.5 parts of steps (3) obtain continues stirring 2 hours, obtain PET strap masterbatch.
After tested, the strap masterbatch that embodiment 1-6 obtains and the ageing-resistant performance of comparative example as shown in the table, the wherein Chinese patent of comparative example to be publication number be 101348601B, ageing-resistant performance test process is: determinand is placed in natural weathering, tests its every mechanical property conservation rate after 1 year:
As seen from the above table, the stretching strength retentivity of the strap masterbatch that the present invention obtains, flexural strength conservation rate, notched Izod impact strength conservation rate, all significantly better than comparative example, show good ageing-resistant performance.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.