CN103332687A - Method for preparing boron and nitrogen codoped graphitized nano carbon by taking biomass as carbon source - Google Patents
Method for preparing boron and nitrogen codoped graphitized nano carbon by taking biomass as carbon source Download PDFInfo
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Abstract
The invention discloses a method for preparing boron and nitrogen codoped graphitized nano carbon by taking biomass as a carbon source, and relates to a synthetic method of boron and nitrogen codoped graphitized nano carbon. The method aims at solving the problem that industrial production is difficult to achieve due to the fact that the existing preparation technology of boron and nitrogen codoped graphitized nano carbon is complicated, reaction conditions are harsh, the contents of boron and nitrogen are low, the yield is low, and the cost is high. The method comprises the steps of 1, pretreatment, 2, precursor preparation, 3, carbonization treatment and 4, acid treatment. The method adopts the rich biomass in nature as the carbon source, so that a preparation technology is simple, and the synthetic cost of a material is lowered; by changing a material ratio of raw materials, the contents of nitrogen and boron in a finished product and graphitization degrees of nitrogen and boron can be adjusted and controlled, and requirements of different fields can be met; and the biomass is uniform in component, so that functionalization ions can be dispersed in the biomass very well, and a pattern and the property of the product are uniform. The method is used for preparing boron and nitrogen codoped graphitized nano carbon by taking the biomass as the carbon source.
Description
Technical field
The present invention relates to the synthetic method of the nitrogen co-doped graphitization nano carbon of boron.
Background technology
Fuel cell has energy density height, efficiency of conversion height and advantages of environment protection, therefore is considered to the most promising energy conversion device.The cathodic oxygen reduction reaction kinetics is slower, and it is the key that determines fuel battery performance.So far, precious metals pt and Pt base alloy is the most effective oxygen reduction catalyst.Yet, because expensive, the poor durability of precious metals pt, scarcity of resources, limited the commercial applications of fuel cell.Therefore, the current research person is devoted to develop cheap non noble metal oxygen reduction catalyst.
The carbon material that base metal mixes is because it has the ability that excellent oxygen reduction reaction activity and anti-carbon monoxide are poisoned, and therefore is considered to a kind of cheapness, is expected to substitute the efficient oxygen reduction reaction catalyzer of precious metal.N, the carbon material of B codoped (N-CNTs, N-Graphene etc.) has excellent ORR electro catalytic activity, characteristics such as weather resistance and environmental friendliness preferably, has potential application prospect.Usually adopt chemical Vapor deposition process to prepare the carbon material that this class is mixed, required conversion unit complexity, productive rate is low, boron nitrogen doping is uncontrollable, and cost is higher.Therefore, be necessary to develop a kind of simple, the synthetic nitrogen co-doped graphitization nano carbon non noble metal oxygen reduction of highly active boron catalyst for reaction of low cost method.
In sum, the existing nitrogen co-doped graphitization nano carbon of boron exists structure heterogeneity, boron and the nitrogen content of complicated process of preparation, severe reaction conditions, product uncontrollable, yields poorly, the cost height, thereby is difficult to realize the problem of suitability for industrialized production.
Summary of the invention
Complicated process of preparation, severe reaction conditions, boron and the nitrogen content that the present invention will solve the existing nitrogen co-doped graphitization nano carbon of boron be low, yield poorly, the cost height, thereby being difficult to realize the problem of suitability for industrialized production, is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass and provide a kind of.
A kind of is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, specifically carries out according to following steps:
One, adopt chemical method that biomass are carried out pre-treatment;
Two, the biomass after the step 1 processing are joined in the solvent, add again and contain the compound of boron, compound and the graphitization catalyst of nitrogen element, be that 25 ℃～60 ℃, stirring velocity are to stir 2h～10h under 80r/min～200r/min condition in temperature again, then temperature be under 80 ℃～110 ℃ with the solvent evaporate to dryness, obtain presoma;
Three, carbonizing treatment: the presoma that step 2 is obtained is under protection of inert gas, and the control heat-up rate is 2 ℃/min～15 ℃/min, is warming up to 600 ℃～1200 ℃, and soaking time is 30min～300min, obtains carbonized product;
Four, acid treatment: the carbonized product that step 3 is obtained joins and carries out acid treatment in the acid solution, the control acid treatment time is 4h～12h, the pH that is washed with distilled water to washing lotion again is 7, be vacuum-drying 4h～16h under 60 ℃～100 ℃ conditions in temperature then, obtain the nitrogen co-doped graphitization nano carbon of boron, namely having finished with biomass is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron, and wherein, the mass ratio of carbonized product and acid solution is 1:(30～100).
The invention has the beneficial effects as follows: the first, it is carbon source that the present invention adopts the abundant biomass of occurring in nature, preparation technology is simple, has therefore reduced the synthetic cost of material widely; The second, by changing the material ratio of raw material, can regulate and control content and the degree of graphitization of nitrogen, boron in the finished product, therefore can satisfy the needs of different field; The 3rd, the composition of biomass is even, and the functionalization ion can be dispersed in the biomass well, so product pattern and character homogeneous.
The present invention prepares the nitrogen co-doped graphitization nano carbon of boron for the preparation of carbon source.
Description of drawings
Fig. 1 is the X-ray diffraction spectrogram of the nitrogen co-doped graphitization nano carbon of boron of embodiment one preparation; Wherein a is the crystal face diffraction peak of (002) crystal face, and b is the crystal face diffraction peak of (100) crystal face;
The x-ray photoelectron spectroscopy figure of the nitrogen co-doped graphitization nano carbon of boron of Fig. 2 embodiment one preparation; Wherein a is the power spectrum peak of boron, and b is the power spectrum peak of carbon, and c is the power spectrum peak of nitrogen.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment is a kind of to be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, specifically carries out according to following steps:
One, adopt chemical method that biomass are carried out pre-treatment;
Two, the biomass after the step 1 processing are joined in the solvent, add again and contain the compound of boron, compound and the graphitization catalyst of nitrogen element, be that 25 ℃～60 ℃, stirring velocity are to stir 2h～10h under 80r/min～200r/min condition in temperature again, then temperature be under 80 ℃～110 ℃ with the solvent evaporate to dryness, obtain presoma;
Three, carbonizing treatment: the presoma that step 2 is obtained is under protection of inert gas, and the control heat-up rate is 2 ℃/min～15 ℃/min, is warming up to 600 ℃～1200 ℃, and soaking time is 30min～300min, obtains carbonized product;
Four, acid treatment: the carbonized product that step 3 is obtained joins and carries out acid treatment in the acid solution, the control acid treatment time is 4h～12h, the pH that is washed with distilled water to washing lotion again is 7, be vacuum-drying 4h～16h under 60 ℃～100 ℃ conditions in temperature then, obtain the nitrogen co-doped graphitization nano carbon of boron, namely having finished with biomass is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron, and wherein, the mass ratio of carbonized product and acid solution is 1:(30～100).
The present embodiment beneficial effect: the first, it is carbon source that the present invention adopts the abundant biomass of occurring in nature, preparation technology is simple, has therefore reduced the synthetic cost of material widely.The second, by changing the material ratio of raw material, can regulate and control content and the degree of graphitization of nitrogen, boron in the finished product, therefore can satisfy the needs of different field.The 3rd, the composition of biomass is even, and the functionalization ion can be dispersed in the biomass well, so product pattern and character homogeneous.
Embodiment two: what present embodiment and embodiment one were different is: pretreated step is as follows described in the step 1: it is that the aqueous solution, the massfraction of 10%～35% potassium hydroxide is that the aqueous solution, the massfraction of 10%～35% sodium hydroxide is that 10%～35% aqueous solution of hydrochloric acid, massfraction are that the aqueous solution of 10%～35% nitric acid or massfraction are in the aqueous solution of 10%～35% potassium permanganate that biomass are joined massfraction, be to activate 3h～8h under 90 ℃～190 ℃ conditions in activation temperature again, finish pre-treatment.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the biomass described in the step 1 are coconut husk, maize straw, palm hull, bagasse, the stem or leaf of cattail, bamboo or wood chip.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: the graphitization catalyst described in the step 2 is that iron nitrate, iron trichloride, ferrous chloride, Xiao Suangu, cobalt chloride, nickelous nitrate, nickelous chloride, the Tripotassium iron hexacyanide, yellow prussiate of potash, potassium cobalticyanide, nickel potassium cyanide or three oxalic acid close potassium ferrite.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: the compound that contains boron in the step 2 is sodium tetraborate, copper borate, zinc borate, Sodium Tetraborate, Sodium peroxoborate, boric acid, fluoroboric acid, ammonium borofluoride, fluoroborate, nickel fluoborate, Sodium tetrafluoroborate, potassium fluoborate, fluoroboric acid cobalt or zinc fluoroborate.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is: the compound that contains the nitrogen element in the step 2 is nitric acid, cyanamide, trimeric cyanamide or urea.Other is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is: the mass ratio of biomass and solvent is 1:(10～30 in the step 2), the mass ratio of biomass and graphitization catalyst is 1:(0.3～5), containing the compound of boron and the mass ratio of graphitization catalyst is 1:(0.8～6), the compound that contains boron is 1:(0.3～2.5 with the mass ratio that contains the compound of nitrogen element), wherein solvent is one or both mixing by any ratio in water and the dehydrated alcohol.Other is identical with embodiment one.
Embodiment eight: what present embodiment and embodiment one were different is: in the step 3 rare gas element be in nitrogen and the argon gas one or both by any than the mixing that mix, flow is 60mL/min～300mL/min.Other is identical with embodiment one.
Embodiment nine: what present embodiment and embodiment one were different is: acid treatment is stirring at room or reflux in the step 4.Other is identical with embodiment one.
Embodiment ten: what present embodiment and embodiment one were different is: acid solution is hydrochloric acid soln, salpeter solution or acetum in the step 4, and the mass concentration of acid solution is 6%～20%.Other is identical with embodiment one.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
Present embodiment is a kind of to be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, specifically carries out according to following steps:
One, the 6g maize straw being joined in the aqueous solution that massfraction is 25% sodium hydroxide, is to activate 3h under 120 ℃ of conditions in activation temperature again;
Two, the maize straw after the step 1 processing is added to the water, add again and contain boric acid, urea and nickel potassium cyanide, be that 35 ℃, stirring velocity are to stir 4h under the 120r/min condition in temperature again, be with the solvent evaporate to dryness under 105 ℃ in temperature then, obtain presoma, wherein, the mass ratio of maize straw and water is 1:20, the mass ratio of maize straw and nickel potassium cyanide is 1:0.4, and the mass ratio of boric acid and nickel potassium cyanide is 1:3;
Three, carbonizing treatment: the presoma that step 2 is obtained is under nitrogen protection, and the control heat-up rate is 4 ℃/min, is warming up to 800 ℃, and soaking time is 60min, obtains carbonized product;
Four, acid treatment: the carbonized product that step 3 is obtained join the 150mL mass concentration be in 20% the salpeter solution temperature be 110 ℃ of conditions next time stream carry out acid treatment, the control returned acid treatment time is 6h, the pH that is washed with distilled water to washing lotion again is 7, be vacuum-drying 6h under 90 ℃ of conditions in temperature then, obtain the nitrogen co-doped graphitization nano carbon of boron, namely having finished with biomass is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron.
The X-ray diffraction spectrogram of the nitrogen co-doped graphitization nano carbon of boron of present embodiment preparation as shown in Figure 1, wherein a is the crystal face diffraction peak of (002) crystal face, b is the crystal face diffraction peak of (100) crystal face; As can be seen from Figure 1, at (002) and (100) amount crystal face tangible crystal face diffraction peak is arranged, illustrate that this material has the graphitized carbon structure.The x-ray photoelectron spectroscopy figure of the nitrogen co-doped graphitization nano carbon of boron of present embodiment preparation as can be seen from Figure 2 has the power spectrum peak of tangible nitrogen, boron, carbon as shown in Figure 2, and wherein a is the power spectrum peak of boron, and b is the power spectrum peak of carbon, and c is the power spectrum peak of nitrogen; Illustrate that surface sample is the nitrogen co-doped carbon material of boron.
Claims (10)
1. one kind is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, and it is characterized in that a kind of is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, specifically carries out according to following steps:
One, adopt chemical method that biomass are carried out pre-treatment;
Two, the biomass after the step 1 processing are joined in the solvent, add again and contain the compound of boron, compound and the graphitization catalyst of nitrogen element, be that 25 ℃～60 ℃, stirring velocity are to stir 2h～10h under 80r/min～200r/min condition in temperature again, then temperature be under 80 ℃～110 ℃ with the solvent evaporate to dryness, obtain presoma;
Three, carbonizing treatment: the presoma that step 2 is obtained is under protection of inert gas, and the control heat-up rate is 2 ℃/min～15 ℃/min, is warming up to 600 ℃～1200 ℃, and soaking time is 30min～300min, obtains carbonized product;
Four, acid treatment: the carbonized product that step 3 is obtained joins and carries out acid treatment in the acid solution, the control acid treatment time is 4h～12h, the pH that is washed with distilled water to washing lotion again is 7, be vacuum-drying 4h～16h under 60 ℃～100 ℃ conditions in temperature then, obtain the nitrogen co-doped graphitization nano carbon of boron, namely having finished with biomass is the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron, and wherein, the mass ratio of carbonized product and acid solution is 1:(30～100).
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that pretreated step is as follows described in the step 1: biomass are joined the aqueous solution that massfraction is 10%～35% potassium hydroxide, massfraction is the aqueous solution of 10%～35% sodium hydroxide, massfraction is 10%～35% aqueous solution of hydrochloric acid, massfraction is that the aqueous solution of 10%～35% nitric acid or massfraction are in the aqueous solution of 10%～35% potassium permanganate, be to activate 3h～8h under 90 ℃～190 ℃ conditions in activation temperature again, finish pre-treatment.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that the biomass described in the step 1 are coconut husk, maize straw, palm hull, bagasse, the stem or leaf of cattail, bamboo or wood chip.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that the graphitization catalyst described in the step 2 is that iron nitrate, iron trichloride, ferrous chloride, Xiao Suangu, cobalt chloride, nickelous nitrate, nickelous chloride, the Tripotassium iron hexacyanide, yellow prussiate of potash, potassium cobalticyanide, nickel potassium cyanide or three oxalic acid close potassium ferrite.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, the compound that it is characterized in that containing in the step 2 boron is sodium tetraborate, copper borate, zinc borate, Sodium Tetraborate, Sodium peroxoborate, boric acid, fluoroboric acid, ammonium borofluoride, fluoroborate, nickel fluoborate, Sodium tetrafluoroborate, potassium fluoborate, fluoroboric acid cobalt or zinc fluoroborate.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, the compound that it is characterized in that containing in the step 2 nitrogen element is nitric acid, cyanamide, trimeric cyanamide or urea.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that the mass ratio of biomass and solvent is 1:(10～30 in the step 2), the mass ratio of biomass and graphitization catalyst is 1:(0.3～5), containing the compound of boron and the mass ratio of graphitization catalyst is 1:(0.8～6), the compound that contains boron is 1:(0.3～2.5 with the mass ratio that contains the compound of nitrogen element), wherein solvent is one or both mixing by any ratio in water and the dehydrated alcohol.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that rare gas element in the step 3 be in nitrogen and the argon gas one or both by any than the mixing that mix, flow is 60mL/min～300mL/min.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that acid treatment is stirring at room or reflux in the step 4.
According to claim 1 a kind of be the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron with biomass, it is characterized in that acid solution is hydrochloric acid soln, salpeter solution or acetum in the step 4, the mass concentration of acid solution is 6%～20%.
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