CN105131556A - Method for preparing nano cellulose/polycarbonate composite material by virtue of sunflower straws - Google Patents
Method for preparing nano cellulose/polycarbonate composite material by virtue of sunflower straws Download PDFInfo
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- CN105131556A CN105131556A CN201510620697.7A CN201510620697A CN105131556A CN 105131556 A CN105131556 A CN 105131556A CN 201510620697 A CN201510620697 A CN 201510620697A CN 105131556 A CN105131556 A CN 105131556A
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Abstract
The invention relates to a method for preparing a nano cellulose/polycarbonate composite material by virtue of sunflower straws, and belongs to the field of a polycarbonate material, which aims at solving the problems that ordinary aliphatic-aromatic polycarbonate is poor in mechanical performance, relatively low in strength and likely to abrade and damage when being used as an engineering material. By virtue of a method for alkaline soaking and acid pickling the sunflower straws to prepare nano cellulose and for graft modifying the surface of polycarbonate particles, the mechanical strength and abrasion resistance of the polycarbonate material are improved, and environmental friendliness can be realized; the impact strength of the prepared nano cellulose/polycarbonate composite material can reach 80kJ/m<2>, and the surface hardness can reach 6H; the nano cellulose/polycarbonate composite material is prepared by virtue of the sunflower straws, so that the cost is reduced, and environmental protection is realized.
Description
Technical field
The present invention relates to a kind of method that sunflower straw prepares nano-cellulose/polycarbonate composite material, belong to polycarbonate material field.
Background technology
Polycarbonate water white transparency, heat-resisting, shock resistance, fire-retardant BI level, has good mechanical property in common use temperature.Compare close to polymethylmethacrylate with performance, the impact resistance of polycarbonate is good, and specific refractory power is high, good processability, does not need additive just to have UL94V-0 level flame retardant properties.Polycarbonate is the high molecular polymer containing carbonate group in molecular chain, and the structure according to ester group can be divided into the broad varietys such as aliphatics, aromatic series, aliphatic-aromatic.Aromatic copolycarbonate is only had to obtain suitability for industrialized production at present.Due to the singularity on polycarbonate structure, now become the general engineering plastic that in five large-engineering plastics, rate of growth is the fastest.
But because the mechanical property of aliphatics and aliphatic-aromatic polycarbonate is lower, cause wearing no resistance of polycarbonate, resistance to organic chemistry moral character, resistance to scratch is poor, and long-term exposure can be turned to be yellow in ultraviolet, and some polycarbonate devices for purposes easy to wear need effects on surface to carry out special processing, thus limit its application in engineering plastics, therefore, work out a kind of high epistasis polycarbonate material, prepare an important settling mode of aspect as existing polycarbonate material.
Summary of the invention
Technical problem to be solved by this invention: poor for current common fats race-aromatic copolycarbonate mechanical property, intensity is lower, as problem that is easy to wear during engineering materials and that damage, provide a kind of being washed by the pickling of sunflower straw alkali and prepare nano-cellulose, again by the method for nano-cellulose to polycarbonate pellets surface graft modification, improve physical strength and the wear resistance of polycarbonate material, environmental protection.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) sunflower straw gathered in and clean, after being exposed to the sun under being placed in sunlight 2 ~ 3 days, be placed on the stalk small pieces of cutting and grinding to 2 in micronizer mill ~ 3cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 20 ~ 30 DEG C, with mix and blend 15 ~ 20min under the speed of 300 ~ 500r/min, and it is filtered, filter residue is placed in the dry 30 ~ 50min of baking oven of 60 ~ 80 DEG C, obtained dry stalk filter residue;
(2) be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, add with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 30 ~ 50Hz, adjustment bath temperature is 55 ~ 60 DEG C, 1 ~ 2h is stirred to it, after it has stirred, it is filtered and dry 1 ~ 2h at being placed in 60 ~ 80 DEG C, obtained alkali leaching stalk fibre;
(3) sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 45 ~ 60min is carried out in the water-bath being placed in 45 ~ 55 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 20 ~ 30 DEG C, be placed in whizzer, by the rotating speed centrifugation 20 ~ 25min of 4000 ~ 4500r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.0 ~ 7.5 can obtain nanofiber cellulose solution,
(4) be that the polycarbonate pellets of 5 ~ 7mm puts into the vacuum vessel that volume is 1L by the size of 400 ~ 600g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1000 ~ 1200mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence;
(5) plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 30 ~ 40min;
(6) opening unit takes out the polycarbonate pellets after plasma surface grafting process, carries out flushing 3 ~ 5 times with deionized water, and is placed in and can be prepared into a kind of sunflower straw to 3 ~ 5h dry under its vacuum and prepares nano-cellulose/polycarbonate composite material.
Application method of the present invention: the nano-cellulose/polycarbonate composite material of preparation is made into polycarbonate bucket, basin, and in production, transport, to use after 3 ~ June without obvious distortion and surface scratches is less.
The present invention is compared with additive method, and Advantageous Effects is:
(1) what prepared by the present invention prepare nano-cellulose/polycarbonate composite material shock strength can reach 80 ~ 100kJ/m
2, surface hardness can reach 6 ~ 7H;
(2) be prepared by sunflower straw, cost-saving, environmental protection.
Embodiment
Sunflower straw is gathered in and cleans, after being exposed to the sun under being placed in sunlight 2 ~ 3 days, be placed on the stalk small pieces of cutting and grinding to 2 in micronizer mill ~ 3cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 20 ~ 30 DEG C, with mix and blend 15 ~ 20min under the speed of 300 ~ 500r/min, and it is filtered, filter residue is placed in the dry 30 ~ 50min of baking oven of 60 ~ 80 DEG C, obtained dry stalk filter residue, be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, add with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 30 ~ 50Hz, adjustment bath temperature is 55 ~ 60 DEG C, 1 ~ 2h is stirred to it, after it has stirred, it is filtered and dry 1 ~ 2h at being placed in 60 ~ 80 DEG C, obtained alkali leaching stalk fibre, sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 45 ~ 60min is carried out in the water-bath being placed in 45 ~ 55 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 20 ~ 30 DEG C, be placed in whizzer, by the rotating speed centrifugation 20 ~ 25min of 4000 ~ 4500r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.0 ~ 7.5 can obtain nanofiber cellulose solution, be that the polycarbonate pellets of 5 ~ 7mm puts into the vacuum vessel that volume is 1L by the size of 400 ~ 600g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1000 ~ 1200mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence, plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 30 ~ 40min, opening unit takes out the polycarbonate pellets after plasma surface grafting process, carries out flushing 3 ~ 5 times with deionized water, and is placed in and can be prepared into a kind of sunflower straw to 3 ~ 5h dry under its vacuum and prepares nano-cellulose/polycarbonate composite material.
Nano-cellulose/the polycarbonate composite material of preparation is made into polycarbonate bucket, basin, and in production, transport, to use after 3 ~ June without obvious distortion and surface scratches is less.
Example 1
Sunflower straw is gathered in and cleans, after being exposed to the sun under being placed in sunlight 2 days, to be placed in micronizer mill cutting and grinding to the stalk small pieces of 2cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 20 DEG C, with mix and blend 15min under the speed of 300r/min, and it is filtered, filter residue is placed in the dry 30min of baking oven of 60 DEG C, obtained dry stalk filter residue; Be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, adding with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 30Hz, adjustment bath temperature is 55 DEG C, stirs 1h, after it has stirred to it, it is filtered and dry 1h at being placed in 60 DEG C, obtained alkali leaching stalk fibre; Sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 45min is carried out in the water-bath being placed in 45 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 20 DEG C, be placed in whizzer, by the rotating speed centrifugation 20min of 4000r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.0 can obtain nanofiber cellulose solution; Be that the polycarbonate pellets of 5mm puts into the vacuum vessel that volume is 1L by the size of 400g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1000mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence; Plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 200kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 30min; Opening unit takes out the polycarbonate pellets after plasma surface grafting process, flushing is carried out 3 times with deionized water, and be placed in and can be prepared into a kind of sunflower straw to 3h dry under its vacuum and prepare nano-cellulose/polycarbonate composite material, prepared by the present invention prepare nano-cellulose/polycarbonate composite material shock strength can reach 80kJ/m
2, surface hardness can reach 6H; Be prepared by sunflower straw, cost-saving, environmental protection.
Example 2
Sunflower straw is gathered in and cleans, after being exposed to the sun under being placed in sunlight 2 days, to be placed in micronizer mill cutting and grinding to the stalk small pieces of 2.5cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 25 DEG C, with mix and blend 17min under the speed of 400r/min, and it is filtered, filter residue is placed in the dry 40min of baking oven of 70 DEG C, obtained dry stalk filter residue; Be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, adding with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 40Hz, adjustment bath temperature is 58 DEG C, stirs 1.5h, after it has stirred to it, it is filtered and dry 1.5h at being placed in 70 DEG C, obtained alkali leaching stalk fibre; Sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 52min is carried out in the water-bath being placed in 50 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 25 DEG C, be placed in whizzer, by the rotating speed centrifugation 23min of 4250r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.2 can obtain nanofiber cellulose solution; Be that the polycarbonate pellets of 6mm puts into the vacuum vessel that volume is 1L by the size of 500g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1100mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence; Plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 250kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 35min; Opening unit takes out the polycarbonate pellets after plasma surface grafting process, flushing is carried out 4 times with deionized water, and be placed in and can be prepared into a kind of sunflower straw to 4h dry under its vacuum and prepare nano-cellulose/polycarbonate composite material, prepared by the present invention prepare nano-cellulose/polycarbonate composite material shock strength can reach 90kJ/m
2, surface hardness can reach 6.5H; Be prepared by sunflower straw, cost-saving, environmental protection.
Example 3
Sunflower straw is gathered in and cleans, after being exposed to the sun under being placed in sunlight 3 days, to be placed in micronizer mill cutting and grinding to the stalk small pieces of 3cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 30 DEG C, with mix and blend 20min under the speed of 500r/min, and it is filtered, filter residue is placed in the dry 50min of baking oven of 80 DEG C, obtained dry stalk filter residue; Be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, adding with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 50Hz, adjustment bath temperature is 60 DEG C, stirs 2h, after it has stirred to it, it is filtered and dry 2h at being placed in 80 DEG C, obtained alkali leaching stalk fibre; Sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 60min is carried out in the water-bath being placed in 55 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 30 DEG C, be placed in whizzer, by the rotating speed centrifugation 25min of 4500r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.5 can obtain nanofiber cellulose solution; Be that the polycarbonate pellets of 7mm puts into the vacuum vessel that volume is 1L by the size of 600g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1200mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence; Plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 40min; Opening unit takes out the polycarbonate pellets after plasma surface grafting process, flushing is carried out 5 times with deionized water, and be placed in and can be prepared into a kind of sunflower straw to 5h dry under its vacuum and prepare nano-cellulose/polycarbonate composite material, prepared by the present invention prepare nano-cellulose/polycarbonate composite material shock strength can reach 100kJ/m
2, surface hardness can reach 7H; Be prepared by sunflower straw, cost-saving, environmental protection.
Claims (1)
1. sunflower straw prepares a method for nano-cellulose/polycarbonate composite material, it is characterized in that concrete preparation process is:
(1) sunflower straw gathered in and clean, after being exposed to the sun under being placed in sunlight 2 ~ 3 days, be placed on the stalk small pieces of cutting and grinding to 2 in micronizer mill ~ 3cm, and be placed in toluene and the dehydrated alcohol mixing solutions prepared of 2:1 by volume, at 20 ~ 30 DEG C, with mix and blend 15 ~ 20min under the speed of 300 ~ 500r/min, and it is filtered, filter residue is placed in the dry 30 ~ 50min of baking oven of 60 ~ 80 DEG C, obtained dry stalk filter residue;
(2) be the sodium hydroxide solution of 9% by the above-mentioned dry stalk filter residue for preparing and massfraction, 1:10 is uniformly mixed in mass ratio, make its Homogeneous phase mixing and be uniformly dispersed, add with filter residue identical in quality after it is uniformly dispersed, massfraction is the superoxol of 2%, and to its heating in water bath under rotor speed is 30 ~ 50Hz, adjustment bath temperature is 55 ~ 60 DEG C, 1 ~ 2h is stirred to it, after it has stirred, it is filtered and dry 1 ~ 2h at being placed in 60 ~ 80 DEG C, obtained alkali leaching stalk fibre;
(3) sulphuric acid soln alkali being soaked stalk fibre and 6mol/L in mass ratio 1:5 carries out mix and blend, and isothermal reaction 45 ~ 60min is carried out in the water-bath being placed in 45 ~ 55 DEG C, after its reaction terminates, add isopyknic distilled water solution with sulphuric acid soln again and stop stirring reaction, after it naturally cools to 20 ~ 30 DEG C, be placed in whizzer, by the rotating speed centrifugation 20 ~ 25min of 4000 ~ 4500r/min, get supernatant liquid and use molecular weight cut-off be 1000 ~ 2000 dialysis tubing dialyse, treat that its pH 7.0 ~ 7.5 can obtain nanofiber cellulose solution,
(4) be that the polycarbonate pellets of 5 ~ 7mm puts into the vacuum vessel that volume is 1L by the size of 400 ~ 600g, it is entered to pass into nitrogen excluding air, after air is discharged completely, again nitrogen in bottle is detached, forming vacuum pressure is-0.05MPa, under this negative pressure state, add 1000 ~ 1200mL nanofiber cellulose solution in vacuum vessel, ensure complete for polycarbonate pellets submergence;
(5) plasma radiofrequency frequency is set, open radio-frequency power supply, polycarbonate pellets and vacuum vessel is made to be in the centre at radio frequency the two poles of the earth, surface graft modification is carried out to it, after opening radio-frequency power supply, add the discharge power of 200 ~ 300kw between outer electrode when processing, in process bottle, nitrogen forms plasma body form, and the surface grafting treatment time is 30 ~ 40min;
(6) opening unit takes out the polycarbonate pellets after plasma surface grafting process, carries out flushing 3 ~ 5 times with deionized water, and is placed in and can be prepared into a kind of sunflower straw to 3 ~ 5h dry under its vacuum and prepares nano-cellulose/polycarbonate composite material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419012A (en) * | 2015-12-19 | 2016-03-23 | 华南理工大学 | Preparation method for straw-based crystalline cellulose nanocrystals and rubber composite material of straw-based crystalline cellulose nanocrystals |
| CN109233187A (en) * | 2018-09-20 | 2019-01-18 | 广州市拿火信息科技有限公司 | ABS composite material and its preparation method and application |
| CN110511749A (en) * | 2019-08-26 | 2019-11-29 | 济南大学 | A kind of preparation method of sulphur nitrogen boron codope carbon quantum dot composite material |
| WO2021029337A1 (en) * | 2019-08-09 | 2021-02-18 | 住友精化株式会社 | Graft copolymer, method for producing graft copolymer and use of same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186109A (en) * | 2007-11-13 | 2008-05-28 | 福建师范大学 | Preparation of nano fibre reinforcement composite resin with high transmittance |
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- 2015-09-27 CN CN201510620697.7A patent/CN105131556A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186109A (en) * | 2007-11-13 | 2008-05-28 | 福建师范大学 | Preparation of nano fibre reinforcement composite resin with high transmittance |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419012A (en) * | 2015-12-19 | 2016-03-23 | 华南理工大学 | Preparation method for straw-based crystalline cellulose nanocrystals and rubber composite material of straw-based crystalline cellulose nanocrystals |
| CN109233187A (en) * | 2018-09-20 | 2019-01-18 | 广州市拿火信息科技有限公司 | ABS composite material and its preparation method and application |
| WO2021029337A1 (en) * | 2019-08-09 | 2021-02-18 | 住友精化株式会社 | Graft copolymer, method for producing graft copolymer and use of same |
| CN110511749A (en) * | 2019-08-26 | 2019-11-29 | 济南大学 | A kind of preparation method of sulphur nitrogen boron codope carbon quantum dot composite material |
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Application publication date: 20151209 |