CN105568762A - Preparation method and application of carbon quantum dot light stabilizer - Google Patents
Preparation method and application of carbon quantum dot light stabilizer Download PDFInfo
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- CN105568762A CN105568762A CN201510933849.9A CN201510933849A CN105568762A CN 105568762 A CN105568762 A CN 105568762A CN 201510933849 A CN201510933849 A CN 201510933849A CN 105568762 A CN105568762 A CN 105568762A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/30—Luminescent or fluorescent substances, e.g. for optical bleaching
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Abstract
The invention discloses a preparation method and application of a carbon quantum dot light stabilizer. Cheap organic carboxylic acid is adopted as a carbon source, piperylhydrazine is adopted as a modifier, and a carbon quantum dot is synthesized and modified to obtain a nitrogen-doped carbon quantum dot containing a radical scavenger fragment by hydrothermal reaction. The prepared carbon quantum dot light stabilizer is light in color and high in water solubility and light fastness, and has broad application prospect, and when the carbon quantum dot light stabilizer is applied to paper pattern coating as a high-yield pulp paper light stabilizer, a result shows that the carbon quantum dot light stabilizer has a certain inhibition effect on light-induced color reversion of paper and the initial whiteness of the paper can be improved.
Description
Technical field
The present invention relates to high yield pulp light stabilizer field, be specifically related to the methods and applications that a kind of hydro-thermal method prepares paper carbon quantum dot light stabilizer.
Background technology
Along with the raising of people's living standard, the demand of paper product is constantly risen.Meanwhile, paper grade (stock) area of woods is constantly reduced, and the problem that there is lack of raw materials becomes increasingly conspicuous, and has become one of key factor restricting global paper industry sustainable development.For this reason, how to utilize the forest reserves fully, obtain the attention that cost is low, whiteness is high, the measured high yield pulp of matter is subject to papermaking researcher day by day.
High yield pulp1 mechanical pulp has that yield is high, environmental pollution is little, low cost and other advantages, but high yield pulp remains a large amount of lignin in bleaching process, lignin is in external environment, as produced chemical reaction under the impact of light and heat etc., generate new color development or auxochrome group, cause the whiteness of paper to reduce, limit its use value and application prospect.At present, suppress the method and access of high yield pulp brightness reversion to have a variety of, and add chemical assistant and be considered to most potentiality and effective method, wherein the use of light stabilizer is the most extensive.
Current, light stabilizer mainly contains the polytypes such as photomask agent, radical scavenger, ultra-violet absorber, fluorescent whitening agent, and they can suppress the brightness reversion phenomenon of paper to a certain extent effectively.But also there is certain drawback, the first, from molecular structure, light stabilizer is all the organic compound with aromatic structure, poorly water-soluble.The second, structural stability is poor, and light resistance is not good.3rd, there is certain toxicity in its overwhelming majority, there is grave danger to ecological environment and human health.To this, researcher improves stability to reach by Small molecular type light stabilizer being carried out the approach such as producing high-molecular, reduces the objects such as toxicity, and achieves certain effect, but all cannot eliminate toxicity completely.
Carbon quantum dot is the newcomer in fluorescence nano family, and its pattern is zero-dimension nano particle, size at below 10nm, have good biocompatibility, water-soluble good, chemical inertness is high, be easy to functionalization, the advantage such as resistance to photobleaching, cheapness.Therefore carbon quantum dot one is come out, and just receives much attention.Its wide application prospect has been shown in technical fields such as opto-electronic device, nanocatalyst, fluorescence imaging, medical diagnosis.And the application still rarely seen report in light stabilizer field.The method of current synthesis carbon quantum dot has multiple, but preparation process is complicated mostly, and the cycle is long, also there are some drawbacks, and as low in fluorescence quantum yield, coloured product is dark.
Chinese patent CN103993504A provides a kind of multifunctional carbon quantum dot as the application process of fluorescent whitening agent in the fields such as textile printing and dyeing, washing agent, papermaking, plastics, leather or coating.The method take living beings as carbon source, uses strong acid and strong base to prepare carbon quantum dot by top-to-bottom method, produces a large amount of spent acid, salkali waste, cause certain influence to environment in preparation process.Prepare carbon quantum dot with biomass resource by top-to-bottom method, gained carbon quantum dot domain size distribution is uneven, and productive rate is low.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application of carbon quantum dot light stabilizer, carbon quantum dot light stabilizer prepared by the present invention is of light color, good water solubility, light resistance are strong, high yield pulp paper can be applied to as light stabilizer, and paper initial whiteness can be improved.
For achieving the above object, present invention employs following technical scheme:
A preparation method for carbon quantum dot light stabilizer, comprises the following steps:
(1) carbon source added after in deionized water and mix (10 ~ 30min) in stirred at ambient temperature, obtain precursor solution, in described precursor solution, the concentration of carbon source is 0.1 ~ 0.4mol/L, and described carbon source is multicomponent organic acid;
(2) be placed into by precursor solution after in hydrothermal reaction kettle and carry out heating reaction, the reaction temperature that precursor solution adds thermal response is 150 ~ 250 DEG C, and the reaction time is 1 ~ 12 hour, naturally cools to room temperature, obtain carbon quantum dot solution after reaction terminates;
(3) added by piperidinamine after in carbon quantum dot solution and be uniformly mixed (10 ~ 30min), obtain solution A, in described solution A, the concentration of piperidinamine is 0.02 ~ 0.1mol/L;
(4) solution A be placed into after in hydrothermal reaction kettle and carry out heating reaction, the reaction temperature that solution A adds thermal response is 100 ~ 250 DEG C, and the reaction time is 1 ~ 8 hour, naturally cools to room temperature, obtain solution B after reaction terminates;
(5) pH value of solution B to be adjusted to after neutrality to obtain solution B 1 with alkaline aqueous solution, add in solution B 1 in left at room temperature 12 ~ 24 hours after potassium borohydride, described potassium borohydride consumption is add potassium borohydride 0.01 ~ 0.05g in 1 ml soln B1; Filter after leaving standstill, gained settled solution will be filtered by 1000Da bag filter purifying, and obtain solution C;
(6) solution C is dry, obtain carbon quantum dot light stabilizer.
Described multicomponent organic acid be selected from citric acid, malic acid or ethanedioic acid one or both.
Described piperidinamine is 2,2,6,6-tetramethyl piperidine amine.
Described alkaline aqueous solution is sodium hydrate aqueous solution, potassium hydroxide aqueous solution, aqueous sodium carbonate or sodium bicarbonate aqueous solution.
Carbon quantum dot light stabilizer prepared by said method is suppressing the application in high yield pulp paper from yellowing.
Application concrete grammar comprises the following steps: described carbon quantum dot light stabilizer being dissolved in the good mass fraction of gelatinization is obtain top sizing sizing material in the oxidized starch aqueous solution of 4%, top sizing sizing material is coated the surface of high yield pulp handsheet, then air-dry under the room temperature of darkroom.
The mass fraction of described carbon quantum dot light stabilizer in described top sizing sizing material is 0.05 ~ 1.2%.
Beneficial effect of the present invention is as follows:
The present invention adopts cheap organic carboxyl acid as carbon source, using piperidinamine as dressing agent, synthesis and the modification of carbon quantum dot is completed by hydro-thermal reaction, obtain a kind of nitrogen-doped carbon quantum dot containing radical scavenger fragment, the carbon quantum dot light stabilizer adopting method of the present invention to prepare is of light color, good water solubility, light resistance are stronger, to paper light-induced color reversion, there is certain inhibitory action, can use as high yield pulp paper light stabilizer, and paper initial whiteness can be improved, there is good application prospect.
Accompanying drawing explanation
The ultra-violet absorption spectrum of the carbon quantum dot light stabilizer of Fig. 1 prepared by the embodiment of the present invention 1.
The excitation spectrum of the carbon quantum dot light stabilizer of Fig. 2 prepared by the embodiment of the present invention 1 and fluorescence emission spectrum.
The size distribution plot of the carbon quantum dot light stabilizer of Fig. 3 prepared by the embodiment of the present invention 1.
The carbon quantum dot light stabilizer aqueous solution picture under natural daylight of Fig. 4 prepared by the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is elaborated.
The invention provides a kind of preparation method of carbon quantum dot light stabilizer.
1. preparation method
Embodiment 1:
Step 1, take 1.26g citric acid and be dissolved in 30mL deionized water, room temperature lower magnetic force is uniformly mixed (10min), obtains precursor solution (citric acid concentration 0.2mol/L).
Step 2, is placed into precursor solution in polyparaphenylene lining hydrothermal reaction kettle, is warming up to 200 DEG C in baking oven, is incubated 5 hours, then naturally cools to room temperature, obtain carbon quantum dot solution.
Step 3, by 0.2g2,2,6,6-tetramethyl piperidine amine joins in carbon quantum dot solution, and room temperature lower magnetic force is uniformly mixed (10min), obtains solution A (the concentration 0.04mol/L of 2,2,6,6-tetramethyl piperidine amine).
Step 4, is placed into solution A in polyparaphenylene lining hydrothermal reaction kettle, is warming up to 180 DEG C in baking oven, is incubated 1 hour, then naturally cools to room temperature, obtains the carbon quantum dot solution modified.
Step 5, regulate the pH value of the carbon quantum dot solution modified to neutral (now system volume is about 35mL) with the NaOH aqueous solution that mass fraction is 20%, add 0.8g potassium borohydride subsequently, left at room temperature 12 hours, use 0.22 micron, aperture water system membrane filtration to remove insoluble matter after leaving standstill, gained settled solution to be dialysed purifying 24 hours by 1000Da bag filter in the glass container filling deionized water, obtains the carbon quantum dot aqueous solution after dialysing.
Step 6, carries out drying by the carbon quantum dot aqueous solution Rotary Evaporators after dialysis, obtains carbon quantum dot light stabilizer (faint yellow solid), be paper light stabilizer at 70 DEG C.
The ft-ir characteristic absorption peak of the carbon quantum dot light stabilizer of synthesis is resolved as follows: 3400 ~ 3500cm
-1place is C-OH and N-H stretching vibration, 2981cm
-1, 2829cm
-1place is methyl C-H antisymmetry and symmetrical stretching vibration, 1654cm
-1place is acid amides C=O stretching vibration, 1573cm
-1place is secondary amide N-H deformation vibration, 1230cm
-1place is acid amides C-N stretching vibration, illustrates that 2,2,6,6-tetramethyl piperidine amine are to carbon quantum dot finishing success.
As can be seen from Figure 1, this carbon quantum dot light stabilizer has good UV absorption, and its maximum absorption wavelength is 330nm.
As can be seen from Figure 2, the excitation spectrum of this carbon quantum dot light stabilizer and emission spectrum are Mirror Symmetry relation, have stronger fluorescent emission at 420nm ~ 480nm, and this region is royal purple light district, illustrates to have blue-fluorescence.
As can be seen from Figure 3, the Size Distribution of this carbon quantum dot light stabilizer is comparatively even.
As can be seen from Figure 4, the clarification of this carbon quantum dot light stabilizer aqueous solution is bright, and solution is substantially colourless.
Embodiment 2:
Step 1, take 0.55g ethanedioic acid and be dissolved in 30mL deionized water, room temperature lower magnetic force is uniformly mixed (10min), obtains precursor solution (the concentration 0.2mol/L of ethanedioic acid).
Step 2, is placed into precursor solution in polyparaphenylene lining hydrothermal reaction kettle, is warming up to 220 DEG C in baking oven, is incubated 5 hours, then naturally cools to room temperature, obtain carbon quantum dot solution.
Step 3, by 0.2g2,2,6,6-tetramethyl piperidine amine joins in carbon quantum dot solution, and room temperature lower magnetic force is uniformly mixed (10min), obtains solution A (the concentration 0.04mol/L of 2,2,6,6-tetramethyl piperidine amine).
Step 4, is placed into solution A in polyparaphenylene lining hydrothermal reaction kettle, is warming up to 180 DEG C in baking oven, is incubated 1 hour, then naturally cools to room temperature, obtains the carbon quantum dot solution modified.
Step 5, regulate the pH value of the carbon quantum dot solution modified to neutral (now system volume is about 33mL) with the NaOH aqueous solution that mass fraction is 20%, add 0.8g potassium borohydride subsequently, left at room temperature 12 hours, use 0.22 micron, aperture water system membrane filtration to remove insoluble matter after leaving standstill, gained settled solution to be dialysed purifying 24 hours by 1000Da bag filter in the glass container filling deionized water, obtains the carbon quantum dot aqueous solution after dialysing.
Step 6, carries out drying by the carbon quantum dot aqueous solution Rotary Evaporators after dialysis, obtains carbon quantum dot light stabilizer (faint yellow solid), be paper light stabilizer at 70 DEG C.
The ft-ir characteristic absorption peak of the carbon quantum dot light stabilizer of synthesis is resolved as follows: 3437cm
-1the broad peak at place is the stretching vibration of-OH and N-H.1629cm
-1place is the stretching vibration of C=C.1238cm
-1place is the stretching vibration of acid amides C-N, 1686cm
-1place is acid amides C=O stretching vibration, illustrates that 2,2,6,6-tetramethyl piperidine amine are to carbon quantum dot finishing success.
Embodiment 3:
Step 1, take 1.2g malic acid and be dissolved in 30mL deionized water, room temperature lower magnetic force is uniformly mixed (10min), obtains precursor solution (malic acid concentration 0.3mol/L).
Step 2, is placed into precursor solution in polyparaphenylene lining hydrothermal reaction kettle, is warming up to 200 DEG C in baking oven, is incubated 5 hours, then naturally cools to room temperature, obtain carbon quantum dot solution.
Step 3, by 0.2g2,2,6,6-tetramethyl piperidine amine joins in carbon quantum dot solution, and room temperature lower magnetic force is uniformly mixed (10min), obtains solution A (the concentration 0.04mol/L of 2,2,6,6-tetramethyl piperidine amine).
Step 4, is placed into solution A in polyparaphenylene hydrothermal reaction kettle, is warming up to 180 DEG C in baking oven, is incubated 1 hour, then naturally cools to room temperature, obtains the carbon quantum dot solution modified.
Step 5, regulate the pH value of the carbon quantum dot solution modified to neutral (now system volume is about 33mL) with the NaOH aqueous solution that mass fraction is 20%, add 0.8g potassium borohydride subsequently, left at room temperature 12 hours, use 0.22 micron, aperture water system membrane filtration to remove insoluble matter after leaving standstill, gained settled solution to be dialysed purifying 24 hours by 1000Da bag filter in the glass container filling deionized water, obtains the carbon quantum dot aqueous solution after dialysing.
Step 6, carries out drying by the carbon quantum dot aqueous solution Rotary Evaporators after dialysis, obtains carbon quantum dot light stabilizer (faint yellow solid), be paper light stabilizer at 70 DEG C.
The ft-ir characteristic absorption peak of the carbon quantum dot light stabilizer of synthesis is resolved as follows: 3413cm
-1the broad peak at place is the stretching vibration of-OH and N-H.1633cm
-1place is the stretching vibration of C=C.1227cm
-1place is the absworption peak of acid amides C-N, 1683cm
-1place is acid amides C=O stretching vibration, illustrates that 2,2,6,6-tetramethyl piperidine amine are to carbon quantum dot finishing success.
2. application process
Take equal in quality different carbon source and identical carbon source different quality carbon quantum dot light stabilizer respectively, be dissolved in the oxidized starch aqueous solution of the good mass fraction of gelatinization 4% and obtained top sizing sizing material, top sizing sizing material is coated the surface of high yield pulp handsheet, then air-dry under the room temperature of darkroom.
After pattern is air-dry, is placed in desk-top uviol lamp weather-resistant test box, sets interval, carry out ultraviolet light accelerated aging test, design temperature is 25 DEG C, and the wavelength of uviol lamp light pipe (totally four) is 340nm, and power output is 5.3mW/cm
2, the distance between fluorescent tube and pattern is 35cm, illumination 48h, adopts the ZB-A type chromascope of Hangzhou Zhi Bang Instrument Ltd. to detect the whiteness change of pattern before and after illumination.
As shown in Table 1, the light-induced color reversion of carbon quantum dot light stabilizer to paper prepared by above-described embodiment has certain inhibitory action, and is also improved to some extent to the initial whiteness of paper.
Table 1 different carbon quantum dot light stabilizer optimum amount and the inhibition to paper light-induced color reversion
Claims (5)
1. a preparation method for carbon quantum dot light stabilizer, is characterized in that: comprise the following steps:
(1) carbon source added after in deionized water and mix in stirred at ambient temperature, obtain precursor solution, in described precursor solution, the concentration of carbon source is 0.1 ~ 0.4mol/L, and described carbon source is multicomponent organic acid;
(2) precursor solution is placed into after in hydrothermal reaction kettle and adds thermal response 1 ~ 12 hour in 150 ~ 250 DEG C, naturally cool to room temperature after reaction terminates, obtain carbon quantum dot solution;
(3) added by piperidinamine after in carbon quantum dot solution and be uniformly mixed, obtain solution A, in described solution A, the concentration of piperidinamine is 0.02 ~ 0.1mol/L;
(4) solution A is placed into after in hydrothermal reaction kettle and adds thermal response 1 ~ 8 hour in 100 ~ 250 DEG C, naturally cool to room temperature after reaction terminates, obtain solution B;
(5) pH value of solution B to be adjusted to after neutrality to obtain solution B 1 with alkaline aqueous solution, add in solution B 1 in left at room temperature 12 ~ 24 hours after potassium borohydride, described potassium borohydride consumption is add potassium borohydride 0.01 ~ 0.05g in 1 ml soln B1; Filter after leaving standstill, gained settled solution will be filtered by 1000Da bag filter purifying, and obtain solution C;
(6) solution C is dry, obtain carbon quantum dot light stabilizer.
2. method according to claim 1, is characterized in that: described multicomponent organic acid be selected from citric acid, malic acid or ethanedioic acid one or both.
3. method according to claim 1, is characterized in that: described piperidinamine is 2,2,6,6-tetramethyl piperidine amine.
4. method according to claim 1, is characterized in that: described alkaline aqueous solution is sodium hydrate aqueous solution, potassium hydroxide aqueous solution, aqueous sodium carbonate or sodium bicarbonate aqueous solution.
5. the carbon quantum dot light stabilizer that as claimed in claim 1 prepared by method is suppressing the application in high yield pulp paper from yellowing.
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