CN108083259A - The preparation method of carbon quantum dot - Google Patents

The preparation method of carbon quantum dot Download PDF

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CN108083259A
CN108083259A CN201810028705.2A CN201810028705A CN108083259A CN 108083259 A CN108083259 A CN 108083259A CN 201810028705 A CN201810028705 A CN 201810028705A CN 108083259 A CN108083259 A CN 108083259A
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raw material
quantum dot
carbon quantum
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skin
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史书亭
史书杰
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The preparation method of carbon quantum dot, it belongs to nano luminescent material preparing technical field.The present invention is 1 according to parts by weight:(1~100):(0.5~100) one or more kinds of mixtures in agriculture and forestry organic waste material and rubbish from cooking and veterinary antibiotics, grain, flowers, Chinese herbal medicine are weighed as raw material, by load weighted raw material, crush, sieve after after mixing, organic acid or highly basic or weak base are added in into treated mixed liquor.Supersound process, hydro-thermal process, centrifugal treating obtain solution after centrifugation and are fitted into bag filter, are placed in dialysis treatment in the beaker equipped with distilled water, obtain carbon quantum dot.For the yield of carbon quantum dot of the present invention 50~90%, the carbon quantum dot size of preparation is 1~2nm, and compared with existing carbon quantum dot preparation method, preparation process is simple, raw material is readily available, environmentally friendly.

Description

The preparation method of carbon quantum dot
Technical field
The invention belongs to nano luminescent material preparing technical fields, and in particular to a kind of preparation method of carbon quantum dot.
Background technology
Carbon nano-particles have very big surface area, so scientists think this nano-particle phase always for a long time Than macroscopical carbon, there are very peculiar chemical and physical features.Scientist extracts carbon nano-particles, and proves these particles After surface covers a kind of special polymer, very bright light can be sent under light illumination, is like small photosphere. Scientists think that this luminescence generated by light phenomenon may be caused by can storing energy due to the cavity on carbon quantum dot surface.And The luminous mechanism of metal quantum point is then somewhat different.
For metal quantum point, carbon quantum dot is nontoxic, small to the harm of environment, and cost is also less expensive.It is made by it Into sensor can be used for detect the biochemical war agents such as explosive and anthrax.Clemson University doctor of Chemistry Sun Ya is put down: " carbon is not semiconductor, and the carbon nano-particles that shine still all are very interesting in terms of application angle either from point of theory. It represents a new platform of luminescent nanoparticle research." especially with respect to it biology and medicine in application.Quantum Point is usually what is extracted from the mixture of lead, cadmium and silicon, but these materials are generally toxic, also harmful to environment. So scientists start to extract quantum dot in some benign compounds.Carbon quantum dot exists as a kind of green non-poisonous material The fields such as photocatalysis, sensor, bio-imaging, pharmaceutical synthesis, genophore are widely used.Prepare the side of carbon quantum dot Method has:Arc discharge method, laser ablation method, electrochemical process and hydro-thermal method etc..The common raw material for preparing carbon quantum dot is mostly to purify Product, such as citric acid, carbohydrate, polymer.
The content of the invention
It is an object of the present invention to provide a kind of preparation methods of carbon quantum dot, and this method yield is high, simple production process.
The invention is realized by the following technical scheme:
A kind of preparation method of carbon quantum dot, includes the following steps:
Step 1, raw material prepare:Weigh raw material A either raw material B or raw material C or weighing raw material A, raw material B or weighing Raw material A, raw material B, raw material C, the raw material A are agriculture and forestry organic waste material, and the raw material B is rubbish from cooking, and the raw material C is One or more kinds of mixtures in veterinary antibiotics, grain, flowers, Chinese herbal medicine, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added Enter the tap water of certain mass, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the mixed liquor and the graphite are added in step 3 treated mixed liquor Mass ratio be 30:0.1~10, be then ultrasonically treated, sonification power be 100~1000W, ultrasonic time 5~ 300min, the mixture after supersound process, for use;
Step 5, hydro-thermal process:The mixture that step 4 is obtained carries out hydro-thermal reaction or microwave hydrothermal reaction, control reaction 20~180 DEG C, 1~300h of reaction time of temperature, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, the liquid after centrifugation is collected, treats With;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water Middle dialysis treatment, obtains carbon quantum dot.
The preparation method of carbon quantum dot of the present invention, the mass ratio of raw material A and raw material B described in step 1 is 1:1 ~100 or the mass ratio of the raw material A and raw material B and raw material C be 1:(1~100):(0.5~100);
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, straw straw One or more kinds of mixtures in stalk, cotton stalk, various flower straws and its leaf and seed, described in step 1 Rubbish from cooking be one or more kinds of mixtures in carbohydrate or Fruit Peel, the Fruit Peel is shaddock Skin, banana skin, orange peel, mangosteen skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin, passion fruit skin, pachyrhizus One or more kinds of mixtures in skin, purple potato skin, potato peel, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, fresh ginger Melon, purple sweet potato, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot, Chinese yam, wild cabbage, broccoli, cucumber, balsam pear, sponge gourd, wild vegetables In one or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, Portugal Grape, honey dew melon, muskmelon, the one or more in "Hami" melon, dragon fruit, banana, mangosteen, passion fruit, persimmon, blueberry, jujube Mixture, grain is rice, light flour, maize flour, black soya bean face, soy noodle, mung bean face, rde bean face, in red bean face One or more, flowers are a kind of or more in Chinese rose flower, rose flower, sweet osmanthus, white orchid, Jasmine, chrysanthemum flower Kind mixture, Chinese herbal medicine for folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii, wilsonii, pueraria lobata, Chinese prickly ash, fennel fruit Perfume, Moringa, Radix Glycyrrhizae, Fructus Forsythiae, gleditsia sinensis, aloe, reed root, caulis bambusae in taenian, Radix Isatidis, dandelion, plantain seed, honeysuckle, black tea, white tea, One or more kinds of mixtures in green tea, jasmine tea, Radix Salviae Miltiorrhizae, ginseng, ganoderma lucidum, ginkgo leaf.
The preparation method of carbon quantum dot of the present invention carries out powder in raw material pre-treatment in step 2 using pulverizer Broken, the raw material after crushing is crossed 20~100 mesh sieves and is sieved, by the raw material handled well according to mass ratio be 1:10~200 add in Tap water or distilled water.
The preparation method of carbon quantum dot of the present invention, the organic acid in step 3 is citric acid, acetic acid, malic acid or One kind in tartaric acid, highly basic are one kind in sodium hydroxide or potassium hydroxide, ammonium hydroxide, urea, and weak base is sodium carbonate or carbonic acid One kind in hydrogen sodium, the pH for adjusting solution are 2~10.
The preparation method of carbon quantum dot of the present invention, the quality of mixed liquor and the graphite described in step 4 Than for 30:1.
The preparation method of carbon quantum dot of the present invention, in the microwave hydrothermal reaction in step 5 microwave power for 100~ 1000W, 10~300min of microwave time.
The preparation method of carbon quantum dot of the present invention, the fluid density after centrifuging in step 6 are 1.02~1.10g/ cm3
The preparation method of carbon quantum dot of the present invention, bag filter molecular cut off is 500~3000Da in step 7.
The preparation method of carbon quantum dot of the present invention, selected material can release carbon in preparation process It is reacted into solvent, using hydro-thermal method, the carbon being dissolved in solvent is synthesized into carbon quantum dot.
The preparation method of carbon quantum dot of the present invention, compared with existing carbon quantum dot preparation method, preparation process letter Single, raw material is readily available, environmentally friendly.
The preparation method of carbon quantum dot of the present invention, the yield of carbon quantum dot is 50~90%.
The preparation method of carbon quantum dot of the present invention, the carbon quantum dot size of preparation is 1~2nm.
Description of the drawings
Fig. 1 is the high-resolution transmission of carbon quantum dot prepared by the preparation method of one carbon quantum dot of specific embodiment method Electron microscopic picture;
Fig. 2 is the high-resolution transmission of carbon quantum dot prepared by the preparation method of two carbon quantum dot of specific embodiment method Electron microscope.
Specific embodiment
Specific embodiment one:
A kind of preparation method of carbon quantum dot, includes the following steps:
Step 1, raw material prepare:Weigh raw material A, raw material B, raw material C, the raw material A be agriculture and forestry organic waste material, the original Material B is rubbish from cooking, and the raw material C is one or more kinds of mixing in veterinary antibiotics, grain, flowers, Chinese herbal medicine Object, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added Enter the tap water of certain mass, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the mixed liquor and the graphite are added in step 3 treated mixed liquor Mass ratio be 30:1, it is then ultrasonically treated, sonification power 1000W, ultrasonic time 60min, after supersound process Mixture, for use;
Step 5, hydro-thermal process:The mixture progress microwave hydrothermal reaction that step 4 is obtained, 180 DEG C of controlling reaction temperature, Reaction time 2h, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, the liquid after centrifugation is collected, treats With;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water Middle dialysis treatment, obtains carbon quantum dot.
The preparation method of carbon quantum dot described in present embodiment, the raw material A described in step 1 is with raw material B and raw material C's Mass ratio is 1:1:0.5;
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, straw straw One or more kinds of mixtures in stalk, cotton stalk, various flower straws and its leaf and seed, described in step 1 Rubbish from cooking be one or more kinds of mixtures in carbohydrate or Fruit Peel, the Fruit Peel is shaddock Skin, banana skin, orange peel, mangosteen skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin, passion fruit skin, pachyrhizus One or more kinds of mixtures in skin, purple potato skin, potato peel, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, fresh ginger Melon, purple sweet potato, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot, Chinese yam, wild cabbage, broccoli, cucumber, balsam pear, sponge gourd, wild vegetables In one or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, Portugal Grape, honey dew melon, muskmelon, the one or more in "Hami" melon, dragon fruit, banana, mangosteen, passion fruit, persimmon, blueberry, jujube Mixture, grain is rice, light flour, maize flour, black soya bean face, soy noodle, mung bean face, rde bean face, in red bean face One or more, flowers are a kind of or more in Chinese rose flower, rose flower, sweet osmanthus, white orchid, Jasmine, chrysanthemum flower Kind mixture, Chinese herbal medicine for folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii, wilsonii, pueraria lobata, Chinese prickly ash, fennel fruit Perfume, Moringa, Radix Glycyrrhizae, Fructus Forsythiae, gleditsia sinensis, aloe, reed root, caulis bambusae in taenian, Radix Isatidis, dandelion, plantain seed, honeysuckle, black tea, white tea, One or more kinds of mixtures in green tea, jasmine tea, Radix Salviae Miltiorrhizae, ginseng, ganoderma lucidum, ginkgo leaf.
The preparation method of carbon quantum dot described in present embodiment, in the raw material pre-treatment in step 2 using pulverizer into Row crushes, and the raw material after crushing crosses 100 mesh sieves and sieved, and according to mass ratio is 1 by the raw material handled well:10 add in originally Water.
The preparation method of carbon quantum dot described in present embodiment, the organic acid in step 3 is citric acid, acetic acid, apple One kind in acid or tartaric acid, the pH for adjusting solution are 3.
The preparation method of carbon quantum dot described in present embodiment, the fluid density after centrifuging in step 6 are 1.05g/ cm3
The preparation method of carbon quantum dot described in present embodiment, bag filter molecular cut off is 3000Da in step 7.
The preparation method of carbon quantum dot described in present embodiment, the carbon quantum dot of preparation as shown in Figure 1, from Fig. 1 , it can be seen that the carbon quantum dot size prepared is 1~2nm, and carbon quantum dot is a large amount of existing.
The preparation method of carbon quantum dot described in present embodiment, the yield of carbon quantum dot is 82.33%.
Specific embodiment two:
A kind of preparation method of carbon quantum dot, includes the following steps:
Step 1, raw material prepare:Weigh raw material A, raw material B, raw material C, the raw material A be agriculture and forestry organic waste material, the original Material B is rubbish from cooking, and the raw material C is one or more kinds of mixing in veterinary antibiotics, grain, flowers, Chinese herbal medicine Object, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added Enter the tap water of certain mass, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the mixed liquor and the graphite are added in step 3 treated mixed liquor Mass ratio be 30:2, it is then ultrasonically treated, sonification power 800W, ultrasonic time 20-100min, is ultrasonically treated Mixture afterwards, for use;
Step 5, hydro-thermal process:The mixture progress microwave hydrothermal reaction that step 4 is obtained, 150 DEG C of controlling reaction temperature, Reaction time 3h, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, the liquid after centrifugation is collected, treats With;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water Middle dialysis treatment, obtains carbon quantum dot.
The preparation method of carbon quantum dot described in present embodiment, the raw material A described in step 1 is with raw material B and raw material C's Mass ratio is 1:2:3;
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, straw straw One or more kinds of mixtures in stalk, cotton stalk, various flower straws and its leaf and seed, described in step 1 Rubbish from cooking be one or more kinds of mixtures in carbohydrate or Fruit Peel, the Fruit Peel is shaddock Skin, banana skin, orange peel, mangosteen skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin, passion fruit skin, pachyrhizus One or more kinds of mixtures in skin, purple potato skin, potato peel, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, fresh ginger Melon, purple sweet potato, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot, Chinese yam, wild cabbage, broccoli, cucumber, balsam pear, sponge gourd, wild vegetables In one or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, Portugal Grape, honey dew melon, muskmelon, the one or more in "Hami" melon, dragon fruit, banana, mangosteen, passion fruit, persimmon, blueberry, jujube Mixture, grain is rice, light flour, maize flour, black soya bean face, soy noodle, mung bean face, rde bean face, in red bean face One or more, flowers are a kind of or more in Chinese rose flower, rose flower, sweet osmanthus, white orchid, Jasmine, chrysanthemum flower Kind mixture, Chinese herbal medicine for folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii, wilsonii, pueraria lobata, Chinese prickly ash, fennel fruit Perfume, Moringa, Radix Glycyrrhizae, Fructus Forsythiae, gleditsia sinensis, aloe, reed root, caulis bambusae in taenian, Radix Isatidis, dandelion, plantain seed, honeysuckle, black tea, white tea, One or more kinds of mixtures in green tea, jasmine tea, Radix Salviae Miltiorrhizae, ginseng, ganoderma lucidum, ginkgo leaf.
The preparation method of carbon quantum dot described in present embodiment, in the raw material pre-treatment in step 2 using pulverizer into Row crushes, and the raw material after crushing crosses 100 mesh sieves and sieved, and according to mass ratio is 1 by the raw material handled well:200 add in originally Water or distilled water.
The preparation method of carbon quantum dot described in present embodiment, the weak base in step 3 is in sodium carbonate or sodium acid carbonate One kind, adjust solution pH be 8.
The preparation method of carbon quantum dot described in present embodiment, the fluid density after centrifuging in step 6 are 1.10g/ cm3
The preparation method of carbon quantum dot described in present embodiment, bag filter molecular cut off is 2000Da in step 7.
The preparation method of carbon quantum dot described in present embodiment, the carbon quantum dot of preparation as shown in Figure 2, from Fig. 2 , it can be seen that the carbon quantum dot size prepared is 1~2nm, and carbon quantum dot is a large amount of existing.
The preparation method of carbon quantum dot described in present embodiment, the yield of carbon quantum dot is 89.97%.
Specific embodiment three:
A kind of preparation method of carbon quantum dot, includes the following steps:
Step 1, raw material prepare:Weigh raw material A, raw material B, raw material C, the raw material A be agriculture and forestry organic waste material, the original Material B is rubbish from cooking, and the raw material C is one or more kinds of mixing in veterinary antibiotics, grain, flowers, Chinese herbal medicine Object, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added Enter the tap water of certain mass, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the mixed liquor and the graphite are added in step 3 treated mixed liquor Mass ratio be 30:0.1, it is then ultrasonically treated, sonification power 100W, ultrasonic time 300min, is ultrasonically treated Mixture afterwards, for use;
Step 5, hydro-thermal process:The mixture that step 4 is obtained carries out hydro-thermal reaction, 60 DEG C of controlling reaction temperature, reaction Time 300h, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, the liquid after centrifugation is collected, treats With;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water Middle dialysis treatment, obtains carbon quantum dot.
The preparation method of carbon quantum dot described in present embodiment, the raw material A described in step 1 is with raw material B and raw material C's Mass ratio is 1:10:10;
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, straw straw One or more kinds of mixtures in stalk, cotton stalk, various flower straws and its leaf and seed, described in step 1 Rubbish from cooking be one or more kinds of mixtures in carbohydrate or Fruit Peel, the Fruit Peel is shaddock Skin, banana skin, orange peel, mangosteen skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin, passion fruit skin, pachyrhizus One or more kinds of mixtures in skin, purple potato skin, potato peel, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, fresh ginger Melon, purple sweet potato, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot, Chinese yam, wild cabbage, broccoli, cucumber, balsam pear, sponge gourd, wild vegetables In one or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, Portugal Grape, honey dew melon, muskmelon, the one or more in "Hami" melon, dragon fruit, banana, mangosteen, passion fruit, persimmon, blueberry, jujube Mixture, grain is rice, light flour, maize flour, black soya bean face, soy noodle, mung bean face, rde bean face, in red bean face One or more, flowers are a kind of or more in Chinese rose flower, rose flower, sweet osmanthus, white orchid, Jasmine, chrysanthemum flower Kind mixture, Chinese herbal medicine for folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii, wilsonii, pueraria lobata, Chinese prickly ash, fennel fruit Perfume, Moringa, Radix Glycyrrhizae, Fructus Forsythiae, gleditsia sinensis, aloe, reed root, caulis bambusae in taenian, Radix Isatidis, dandelion, plantain seed, honeysuckle, black tea, white tea, One or more kinds of mixtures in green tea, jasmine tea, Radix Salviae Miltiorrhizae, ginseng, ganoderma lucidum, ginkgo leaf.
The preparation method of carbon quantum dot described in present embodiment, in the raw material pre-treatment in step 2 using pulverizer into Row crushes, and the raw material after crushing crosses 100 mesh sieves and sieved, and according to mass ratio is 1 by the raw material handled well:100 add in originally Water.
The preparation method of carbon quantum dot described in present embodiment, the highly basic in step 3 are sodium hydroxide or potassium hydroxide In one kind, adjust solution pH be 10.
The preparation method of carbon quantum dot described in present embodiment, the fluid density after centrifuging in step 6 are 1.02g/ cm3
The preparation method of carbon quantum dot described in present embodiment, bag filter molecular cut off is 500Da in step 7.
The preparation method of carbon quantum dot described in present embodiment, carbon quantum dot are a large amount of existing, the productions of carbon quantum dot Rate is 76.59%.
Specific embodiment four:
A kind of preparation method of carbon quantum dot, includes the following steps:
Step 1, raw material prepare:Weigh raw material A, raw material B, raw material C, the raw material A be agriculture and forestry organic waste material, the original Material B is rubbish from cooking, and the raw material C is one or more kinds of mixing in veterinary antibiotics, grain, flowers, Chinese herbal medicine Object, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added Enter the tap water of certain mass, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the mixed liquor and the graphite are added in step 3 treated mixed liquor Mass ratio be 30:0.5, it is then ultrasonically treated, sonification power 500W, ultrasonic time 200min, is ultrasonically treated Mixture afterwards, for use;
Step 5, hydro-thermal process:The mixture that step 4 is obtained carries out hydro-thermal reaction or microwave hydrothermal reaction, control reaction 80 DEG C, reaction time 180h of temperature, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, the liquid after centrifugation is collected, treats With;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water Middle dialysis treatment, obtains carbon quantum dot.
The preparation method of carbon quantum dot described in present embodiment, the raw material A described in step 1 is with raw material B and raw material C's Mass ratio is 1:100:100;
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, straw straw One or more kinds of mixtures in stalk, cotton stalk and its leaf, the rubbish from cooking described in step 1 are carbohydrate Or one or more kinds of mixtures in Fruit Peel, the Fruit Peel is pomelo peel, banana skin, orange peel, mangosteen One or more kinds of mixtures in skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, in fresh ginger One or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, grape, Honey dew melon, muskmelon, one or more kinds of mixtures in "Hami" melon, grain is rice, in light flour, maize flour, bean flour One or more, flowers are Chinese rose flower, one or more kinds of mixtures in rose flower, chrysanthemum flower, and Chinese herbal medicine is Folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii, one or more kinds of mixtures in wilsonii.
The preparation method of carbon quantum dot described in present embodiment, in the raw material pre-treatment in step 2 using pulverizer into Row crushes, and the raw material after crushing crosses 100 mesh sieves and sieved, and according to mass ratio is 1 by the raw material handled well:50 add in originally Water.
The preparation method of carbon quantum dot described in present embodiment, the highly basic in step 3 are sodium hydroxide, ammonium hydroxide or hydrogen-oxygen Change one kind in potassium, the pH for adjusting solution is 10.
The preparation method of carbon quantum dot described in present embodiment, the fluid density after centrifuging in step 6 are 1.03g/ cm3
The preparation method of carbon quantum dot described in present embodiment, bag filter molecular cut off is 800Da in step 7.
The preparation method of carbon quantum dot described in present embodiment, carbon quantum dot are a large amount of existing, the productions of carbon quantum dot Rate is 66.61%.

Claims (8)

1. a kind of preparation method of carbon quantum dot, it is characterised in that:Include the following steps:
Step 1, raw material prepare:Weigh raw material A either raw material B or raw material C or weighing raw material A, raw material B or weighing raw material A, raw material B, raw material C, the raw material A are agriculture and forestry organic waste material, and the raw material B is rubbish from cooking, and the raw material C is vegetable One or more kinds of mixtures in dish, fruit, grain, flowers, Chinese herbal medicine, for use;
Step 2, raw material pre-treatment:By the load weighted raw material of step 1, after crushing, sieving, the raw material handled well is added in one Determine the tap water of quality, after mixing for use;
Step 3, pH are adjusted:Organic acid or highly basic or weak base are added in into step 2 treated mixed liquor, adjusts mixed liquor PH, for use;
Step 4 is ultrasonically treated:Graphite, the matter of the mixed liquor and the graphite are added in step 3 treated mixed liquor Amount is than being 30:0.1~10, be then ultrasonically treated, sonification power be 100~1000W, 5~300min of ultrasonic time, Mixture after supersound process, for use;
Step 5, hydro-thermal process:The mixture that step 4 is obtained carries out hydro-thermal reaction or microwave hydrothermal reaction, controlling reaction temperature 20~180 DEG C, 1~300h of reaction time, the mixture after reaction, for use;
Step 6, centrifugal treating:Step 4 treated mixed liquor is subjected to centrifugal treating, collects the liquid after centrifugation, for use;
Step 7, dialysis treatment:Solution is obtained after step 6 is centrifuged to be fitted into bag filter, is placed in the beaker equipped with distilled water thoroughly Analysis is handled, and obtains carbon quantum dot.
2. the preparation method of carbon quantum dot according to claim 1, it is characterised in that:Raw material A and original described in step 1 The mass ratio for expecting B is 1:1~100 or the mass ratio of the raw material A and raw material B and raw material C be 1:(1~100):(0.5~ 100);
Agriculture and forestry organic waste material described in step 1 is maize straw, soybean stalk, wheat stalk, broomcorn straw, rice straw, cotton One or more kinds of mixtures in chopped straw stalk, various flower straws and its leaf and seed, the food waste described in step 1 Rubbish is one or more kinds of mixtures in carbohydrate or Fruit Peel, and the Fruit Peel is pomelo peel, perfume (or spice) Any of several broadleaf plants skin, orange peel, mangosteen skin, pineapple peel, apple skin, pear skin, mangrove bark, coconut skin, muskmelon skin, passion fruit skin, melon skin, purple One or more kinds of mixtures in potato skin, potato peel, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot;
Vegetables described in step 1 are spinach, rape, pakchoi, celery, fennel, caraway, garlic, onion, fresh ginger pachyrhizus, In purple sweet potato, carrot, ternip, Green Radish, Raphanus sativus var.niger, carrot, Chinese yam, wild cabbage, broccoli, cucumber, balsam pear, sponge gourd, wild vegetables One or more kinds of mixtures, fruit is apple, shaddock, pineapple, Kiwi berry, orange, hawthorn, mango, coconut, grape, in vain Blue melon, muskmelon, one or more kinds of mixing in "Hami" melon, dragon fruit, banana, mangosteen, passion fruit, persimmon, blueberry, jujube Object, grain for rice, light flour, maize flour, black soya bean face, soy noodle, mung bean face, rde bean face, one kind in red bean face or Several, flowers are the mixed of the one or more in Chinese rose flower, rose flower, sweet osmanthus, white orchid, Jasmine, chrysanthemum flower Close object, Chinese herbal medicine is folium artemisiae argyi, sweet wormwood, Radix Notoginseng, safflower, lotus leaf, mulberry leaf, tripterygium wilfordii is wilsonii, pueraria lobata, Chinese prickly ash, fennel seeds, peppery Wood, Radix Glycyrrhizae, Fructus Forsythiae, gleditsia sinensis, aloe, reed root, caulis bambusae in taenian, Radix Isatidis, dandelion, plantain seed, honeysuckle, black tea, white tea, green tea, One or more kinds of mixtures in jasmine tea, Radix Salviae Miltiorrhizae, ginseng, ganoderma lucidum, ginkgo leaf.
3. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Raw material pre-treatment in step 2 Middle to be crushed using pulverizer, the raw material after crushing is crossed 20~100 mesh sieves and is sieved, by the raw material handled well according to quality Than for 1:10~200 add in tap water or distilled water.
4. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Organic acid in step 3 is lemon One kind in lemon acid, acetic acid, malic acid or tartaric acid, highly basic are one kind in sodium hydroxide or potassium hydroxide, ammonium hydroxide, urea, Weak base is one kind in sodium carbonate or sodium acid carbonate, and the pH for adjusting solution is 2~10.
5. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Mixed liquor described in step 4 Mass ratio with the graphite is 30:1.
6. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Microwave hydrothermal in step 5 is anti- Microwave power is 100~1000W, 10~300min of microwave time in answering.
7. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Liquid after being centrifuged in step 6 Density is 1.02~1.10g/cm3
8. the preparation method of carbon quantum dot according to claim 1 or 2, it is characterised in that:Bag filter retention point in step 7 Son amount is 500~3000Da.
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Application publication date: 20180529