CN111485448B - Preparation method of paper-based photoelectrocatalysis material for catalyzing oxidation of xylose - Google Patents

Preparation method of paper-based photoelectrocatalysis material for catalyzing oxidation of xylose Download PDF

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CN111485448B
CN111485448B CN202010369363.8A CN202010369363A CN111485448B CN 111485448 B CN111485448 B CN 111485448B CN 202010369363 A CN202010369363 A CN 202010369363A CN 111485448 B CN111485448 B CN 111485448B
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pulp
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stirring
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CN111485448A (en
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斯惠仙
张义忠
刘冬
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Dongyang City Ju Ran Electronic Science And Technology Co ltd S
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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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/66—Salts, e.g. alums
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
    • D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/13—Silicon-containing compounds
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
    • D21H17/55—Polyamides; Polyaminoamides; Polyester-amides
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/64—Alkaline compounds
    • 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/65—Acid compounds
    • 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
    • D21H21/18—Reinforcing agents
    • D21H21/20—Wet strength agents

Abstract

The invention relates to the field of chemical industry, in particular to a preparation method of a paper-based photoelectrocatalysis material for catalyzing oxidation of xylose; the invention relates to a preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation, which comprises the steps of preparing polyamide polyamine epoxy chloropropane resin and polyethylene glycol ether into transparent paper scraps, then depositing indium sulfide on the surface of the transparent paper scraps, co-depositing nickel iron double hydroxide on the surface layer of the indium sulfide, combining the high carrier mobility and the environmental stability of the indium sulfide with the characteristics of the nickel iron double hydroxide, such that the photo-induced cavity accumulation is reduced, and the oxygen release kinetics is enhanced, such that the water oxidation efficiency of the catalyst is obviously enhanced, and xylose can be converted to produce xylonic acid by using the catalyst, such that the production cost can be effectively reduced, the xylonic acid production industrialization can be more rapidly achieved, agricultural wastes can be effectively utilized, and great significance is provided for environmental protection and sustainable development of resources.

Description

Preparation method of paper-based photoelectrocatalysis material for catalyzing oxidation of xylose
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of a paper-based photoelectrocatalysis material for catalyzing oxidation of xylose.
Background
The photocatalytic technology is a technology that relies on the property of the semiconductor catalyst itself to absorb light and convert the light energy into chemical energy.
201711268355.9 discloses a method for preparing an electrode of photoelectrocatalysis material. In the invention, TiO2nano-Ce is prepared by adopting a sol-gel method, and Ti/TiO is prepared by adopting an anodic oxidation method2NTs, preparation of Ti/TiO by pulse electrodeposition2/PbO2/TiO2nano-Ce. The invention dopes rare earth element Ce to lead PbO2The particles become smaller and the specific surface area increases significantly. And pure PbO2Compared with the electrode, the catalyst has higher catalytic activity, longer service life and better stability. By pulse electrodeposition of TiO2nano-Ce is modified into the nano-tube to make Ti/TiO2NTs electrode as anode, Pt sheet as cathode, saturated calomel electrode as reference electrode, TiO-containing material2In nano-Ce electroplating solution, Ti/TiO is prepared by adopting a special formula and a voltage-stabilizing pulse current deposition method2/PbO2/TiO2The nano-Ce electrode is simple to operate, improves the purity, density and uniformity of a deposition layer, reduces the porosity of the deposition layer, and improves the stability and catalytic performance of the electrode.
201910858755.8 provides an active regulation method of photoelectrocatalysis semiconductor material, which adopts halogen ion to modify the surface of electrode material made of semiconductor material. The method of the invention can obviously improve the catalytic activity of the semiconductor material and reduce the catalytic cost.
201711268355.9 relates to a preparation method of a novel photoelectrocatalysis material electrode. In the invention, TiO is prepared by adopting a sol-gel method2nano-Ce, preparing Ti/TiO by anode oxidation method2NTs, preparation of Ti/TiO by pulse electrodeposition2/PbO2/TiO2nano-Ce. The invention dopes rare earth element Ce to lead PbO2The particles become smaller and the specific surface area increases significantly. And pure PbO2Compared with the electrode, the catalyst has higher catalytic activity, longer service life and better stability. By pulse electrodeposition of TiO2nano-Ce is modified into the nano-tube to make Ti/TiO2NTs electrode as anode, Pt sheet as cathode, saturated calomel electrode as reference electrode, TiO-containing material2In nano-Ce electroplating solution, Ti/TiO is prepared by adopting a special formula and a voltage-stabilizing pulse current deposition method2/PbO2/TiO2The nano-Ce electrode is simple to operate, improves the purity, density and uniformity of a deposition layer, reduces the porosity of the deposition layer, and improves the stability and catalytic performance of the electrode.
The N-polyamide polyamine epichlorohydrin resin PAE is usually used as a wet strength agent for papermaking and is water-soluble, cationic or thermosetting resin. It has the features of high efficiency, being suitable for neutral papermaking, easy to recover broke or waste paper, no toxicity, etc. The product is suitable for manufacturing various papers with wet strength, and can be used as a wet strength agent, a retention aid for emulsion rosin size and reinforced rosin size, a synergist for neutral sizing agent, and a cationic starch modifier to improve the paper size stability.
In the prior art, the preparation reaction equation of the N-polyamide polyamine epichlorohydrin resin is as follows:
Figure 948446DEST_PATH_IMAGE001
the N-polyamide polyamine epichlorohydrin resin is used as a paper wet strength agent, is matched with polyhydroxy carboxymethyl cellulose, and enhances the absorption on the fiber. However, there are still many disadvantages that the water solubility is deteriorated due to the excessive alkyl group, which affects the bridging effect with the polyhydroxycarboxymethylcellulose and reduces the wet strengthening effect.
Sugars are an important component of biological xylans, most of which are present in plants, and of course some of the xylose is present in animal heparins and chondroitins. Xylonic acid is a new chemical product in recent years, is one of important metabolites of vitamin C, and plays a very important role in regulating the circulation and metabolism of vitamin C in organisms. Most of xylonic acids are converted by xylose oxidation, and nowadays, research methods for converting xylose into xylonic acid mainly focus on biological conversion methods, mainly convert xylose into xylonic acid by using some bioactive enzymes, but the existing biocatalysis has the defects of poor stability, low conversion efficiency and poor recycling property.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a paper-based photoelectric catalytic material for catalyzing xylose oxidation.
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 2.4-16.2 parts of citric acid into 160 parts of 100-one organic solvent by mass, stirring and mixing uniformly, adding 0.3-3.5 parts of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 1-3, then adding 0.42-4.8 parts of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 1-20 parts of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 80-100 ℃, stirring and reacting for 10-20 hours, filtering after the reaction is finished, taking out a sample, cleaning and drying ethanol, adding the obtained material into a hydrothermal reaction kettle, adding 0.6-4.2 parts of nickel nitrate, 0.2-2.4 parts of 1, 1' -bis (dimethylsilyl) ferrocene, 1.6-14.2 parts of urea and 50-80 ℃ deionized water, stirring and mixing uniformly, controlling the temperature to be 130 ℃, carrying out hydrothermal reaction for 5-10h, filtering, washing and drying after the reaction is finished to obtain the paper-based photoelectrocatalysis material for catalyzing xylose oxidation.
The preparation method of the surface nano-fibrillated transparent paper scrap comprises the following steps:
according to the mass parts, 100-200 parts of paper pulp with the mass percentage concentration of 20-40 percent is added into a beating machine, adding into 1.2-3.5 portions of zinc chloride and 400 portions of hydrochloric acid with the mass percentage concentration of 1-5%, stirring at 40-60 deg.C for 5-10h, filtering, washing with water to pH =7, filtering, then evenly mixing with 10-18 parts of N-polyamide polyamine epichlorohydrin resin, 5-11 parts of 3-aminopropyl trihydroxy silane, 200-300 parts of water and 1.2-3.4 parts of sodium hydroxide, then treating 30000-50000 turns in a refiner, then placing the obtained slurry at 0-10 ℃ for 12-36h, then diluting the pulp to 0.5-5g/L, and carrying out suction filtration on the pulp to obtain paper with the thickness of 17-24 g/m.2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80-100 ℃ for 30-60s under the pressure of 0.1-1MPa, repeating the hot pressing for 3-5 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The partial reaction is schematically shown below:
(1) chlorination of pulp:
pulp cellulose, the most basic component of fiber cells, is chloridized to obtain chloridized paper cellulose, and hydrochloric acid is removed by filtering and washing.
Figure DEST_PATH_IMAGE002
(2) The N-polyamide polyamine epichlorohydrin resin and the 3-aminopropyl trihydroxy silane are further reacted with chlorinated paper cellulose:
Figure DEST_PATH_IMAGE003
the paper pulp is reed pulp, bagasse pulp, bamboo pulp or cotton pulp.
The organic solvent is ethanol or methanol or isopropanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode slice by pressure of 5-15MPa for use.
According to the preparation method of the paper-based photoelectric catalytic material for catalyzing xylose oxidation, the polyamide polyamine epoxy chloropropane resin and the 3-aminopropyl trihydroxy silane are prepared into the transparent paper scraps, the N-polyamide polyamine epoxy chloropropane resin and the 3-aminopropyl trihydroxy silane are further reacted with the chlorinated paper cellulose, so that the water solubility is improved, the bridging effect with the polyhydroxy carboxymethyl cellulose is enhanced, and the wet reinforcement performance is improved.
And then indium sulfide is deposited on the surface of the transparent paper scrap, nickel iron double hydroxide is co-deposited on the surface layer of the indium sulfide, the high carrier mobility and the environmental stability of the indium sulfide are combined with the characteristics of the nickel iron double hydroxide of reducing photoproduction cavity accumulation and enhancing oxygen release kinetics, so that the water oxidation efficiency of the catalyst is obviously enhanced, xylose can be converted to produce xylonic acid by using the catalyst, the production cost can be effectively reduced, the xylonic acid production industrialization can be more quickly realized, meanwhile, agricultural wastes can be effectively utilized, and the catalyst has great significance for environmental protection and sustainable development of resources.
Drawings
FIG. 1 is a Fourier infrared spectrum of the surface nanofibrillated transparency chips prepared in example 2.
At 1124cm-1An antisymmetric telescopic absorption peak of carbon and oxygen of ether exists nearby and is 769cm-1A carbon-chlorine telescopic absorption peak exists nearby, which indicates that chlorinated pulp participates in the reaction; at 1686cm-1The telescopic absorption peak of carbonyl of amide exists nearby and is 1278cm-1The absorption peak of amide carbon nitrogen near the absorption peak was 3368/1590cm-1The expansion/variable angle absorption peak of nitrogen and hydrogen exists nearby, which indicates that the N-polyamide polyamine epichlorohydrin participates in the reaction; at 1080cm-1In the vicinity of which silicon oxide is presentHas an absorption peak of 1421cm-1The in-plane bend absorption peak of the hydroxyl group is present in the vicinity of 1045cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, and the 3-aminopropyl trihydroxy silane participates in the reaction.
Detailed Description
The invention is further illustrated by the following specific examples:
in order to test the capacity of the prepared material for photoelectrocatalysis xylose oxidation, a three-electrode system is adopted at room temperature, AM 1.5G simulated sunlight and ultraviolet light with the wavelength of 360nm are used for irradiating the photoelectric material, 30ml of xylose solution and 30ml of sodium sulfate solution are added into an electrolytic cell, the xylose solution is subjected to oxidative degradation for 60min under the constant voltage of 0.2V, and the residual quantity of xylose in the electrolytic cell is measured by a phloroglucinol method.
Example 1
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 2.4g of citric acid into 100g of organic solvent, stirring and mixing uniformly, adding 0.3g of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 1, then adding 0.42g of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 1g of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 80 ℃, stirring and reacting for 10 hours, filtering and taking out a sample after completion, cleaning with ethanol, drying, adding the obtained material into a hydrothermal reaction kettle, adding 0.6 g of nickel nitrate, 0.2g of 1, 1' -bis (dimethylsilyl) ferrocene, 1.6g of urea and 50 g of deionized water, stirring and mixing uniformly, controlling the temperature to be 100 ℃, carrying out hydrothermal reaction for 5 hours, filtering after completion of the reaction, washing, and drying to obtain the paper-based photocatalytic material for catalyzing xylose oxidation.
Adding 100g of paper pulp with the mass percent concentration of 20% into a pulping machine, adding 1.2g of zinc chloride and 400g of hydrochloric acid with the mass percent concentration of 1%, stirring for 5h at 40 ℃, filtering, washing with water until the pH =7, filtering, then uniformly mixing with 10g of N-polyamide polyamine epichlorohydrin resin, 5g of 3-aminopropyltrihydroxysilane and 200g of water, 1.2g of sodium hydroxide, then processing for 30000 turns in a pulping machine, then placing the obtained pulp for 12h at 0 ℃, and then standingDiluting the pulp to 0.5g/L, and filtering the pulp to form paper with the thickness of 17g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80 ℃ for 30s under the pressure of 0.1MPa, repeating the hot pressing for 3 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The paper pulp is reed pulp.
The organic solvent is ethanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 5MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 12.4 percent, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 6.3 percent.
Example 2
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 10.2g of citric acid into 130g of organic solvent, stirring and mixing uniformly, adding 2.4g of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 2, then adding 2.6g of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 10g of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 90 ℃, stirring and reacting for 15 hours, filtering and taking out a sample after completion, cleaning with ethanol, drying, adding the obtained material into a hydrothermal reaction kettle, adding 2.3g of nickel nitrate, 1.4g of 1, 1' -bis (dimethylsilyl) ferrocene, 7.6g of urea and 70 g of deionized water, stirring and mixing uniformly, controlling the temperature to be 120 ℃, carrying out hydrothermal reaction for 8 hours, filtering after completion of the reaction, washing, and drying to obtain the paper-based photocatalytic material for catalyzing xylose oxidation.
The preparation method of the surface nano-fibrillated transparent paper scrap comprises the following steps:
adding 120g of pulp with the mass percent concentration of 25% into a beater, adding 1.8g of zinc chloride and 500g of hydrochloric acid with the mass percent concentration of 3%, stirring for 7h at 45 ℃, filtering, washing with water until the pH is =7, filtering, and mixing with 15g of N-polyamide polyamine epichlorohydrin resin, 7g of 3-aminopropyltrihydroxysilane, 255g of water and 1.5g of sodium hydroxideHomogenizing, processing at 35000 r in a pulping machine, standing at 3 deg.C for 18h, diluting to 3g/L, vacuum filtering to obtain paper with thickness of 19g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing for 35s at 90 ℃ under the pressure of 0.4MPa, repeating the hot pressing for 4 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The paper pulp is bagasse pulp.
The organic solvent is methanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 10MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 11.4 percent, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 5.8 percent.
Example 3
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 16.2g of citric acid into 160g of organic solvent, stirring and mixing uniformly, adding 3.5g of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 3, then adding 4.8g of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 20g of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 100 ℃, stirring and reacting for 20 hours, filtering and taking out a sample after completion, cleaning with ethanol, drying, adding the obtained material into a hydrothermal reaction kettle, adding 4.2g of nickel nitrate, 2.4g of 1, 1' -bis (dimethylsilyl) ferrocene, 14.2g of urea and 80 g of deionized water, stirring and mixing uniformly, controlling the temperature to be 130 ℃, carrying out hydrothermal reaction for 10 hours, filtering after completion of the reaction, washing, and drying to obtain the paper-based photocatalytic material for catalyzing xylose oxidation.
The preparation method of the surface nano-fibrillated transparent paper scrap comprises the following steps:
200g of 40% strength by mass pulp are placed in a beater, 3.5g of zinc chloride and 800g of 5% strength by mass hydrochloric acid are stirred for 10h at 60 ℃, filtered, washed with water to pH =7, filtered and then admixed with 18g of N-polyamideUniformly mixing polyamine-epichlorohydrin resin, 11g of 3-aminopropyltrihydroxysilane, 300g of water and 3.4g of sodium hydroxide, processing the mixture in a pulping machine for 50000 turns, standing the obtained slurry at 10 ℃ for 36 hours, diluting the slurry to 5g/L, and filtering the slurry to obtain paper with the thickness of 24g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing for 60s at 100 ℃ under the pressure of 1MPa, repeating the hot pressing for 5 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The paper pulp is cotton pulp.
The organic solvent is isopropanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 15MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 11.1 percent, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 5.6 percent.
Comparative example 1
Adding 100g of paper pulp with the mass percent concentration of 20% into a pulping machine, adding 1.2g of zinc chloride and 400g of hydrochloric acid with the mass percent concentration of 1%, stirring for 5h at 40 ℃, filtering, washing with water until the pH =7, filtering, then uniformly mixing with 10g of N-polyamide polyamine epoxy chloropropane resin, 200g of water and 1.2g of sodium hydroxide, then processing in a pulping machine for 30000 r, then placing the obtained pulp at 0 ℃ for 12h, then diluting the pulp to 0.5g/L, and carrying out suction filtration on the pulp to form paper with the thickness of 17g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80 ℃ for 30s under the pressure of 0.1MPa, repeating the hot pressing for 3 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
Otherwise, the same as example 1;
the paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 5MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 17.2%, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 9.4%.
Comparative example 2
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 2.4g of citric acid into 100g of organic solvent, stirring and mixing uniformly, adding 0.42g of thioacetamide into a reaction kettle, stirring and mixing uniformly, adding 1g of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 80 ℃, stirring and reacting for 10 hours, filtering after the reaction is finished, taking out a sample, cleaning with ethanol, drying, adding the obtained material into a hydrothermal reaction kettle, adding 0.6 g of nickel nitrate, 1.6g of urea and 50 g of deionized water, stirring and mixing uniformly, controlling the temperature to be 100 ℃, carrying out hydrothermal reaction for 5 hours, filtering after the reaction is finished, washing, and drying to obtain the paper-based photocatalytic material for catalyzing xylose oxidation.
Adding 100g of paper pulp with the mass percent concentration of 20% into a pulping machine, adding 1.2g of zinc chloride, 400g of hydrochloric acid with the mass percent concentration of 1%, stirring for 5h at 40 ℃, filtering, washing with water until the pH =7, filtering, then uniformly mixing with 10g of N-polyamide polyamine epichlorohydrin resin, 5g of 3-aminopropyltrihydroxysilane, 200g of water and 1.2g of sodium hydroxide, then processing for 30000 turns in a pulping machine, then placing the obtained pulp for 12h at 0 ℃, then diluting the pulp to 0.5g/L, and carrying out suction filtration on the pulp to form paper with the thickness of 17g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80 ℃ for 30s under the pressure of 0.1MPa, repeating the hot pressing for 3 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The paper pulp is reed pulp.
The organic solvent is ethanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 5MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 57.9 percent, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 54.2 percent.
Comparative example 3
A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 2.4g of citric acid into 100g of organic solvent, stirring and mixing uniformly, adding 0.3g of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 1, then adding 0.42g of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 1g of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 80 ℃, stirring and reacting for 10 hours, filtering and taking out a sample after completion, cleaning with ethanol, drying, adding the obtained material into a hydrothermal reaction kettle, adding 0.2g of 1, 1' -bis (dimethylsilyl) ferrocene, 1.6g of urea and 50 g of deionized water, stirring and mixing uniformly, controlling the temperature to be 100 ℃, carrying out hydrothermal reaction for 5 hours, filtering after completion of the reaction, washing, and drying to obtain the paper-based photocatalytic material for catalyzing xylose oxidation.
Adding 100g of paper pulp with the mass percent concentration of 20% into a pulping machine, adding 1.2g of zinc chloride, 400g of hydrochloric acid with the mass percent concentration of 1%, stirring for 5h at 40 ℃, filtering, washing with water until the pH =7, filtering, then uniformly mixing with 10g of N-polyamide polyamine epichlorohydrin resin, 5g of 3-aminopropyltrihydroxysilane, 200g of water and 1.2g of sodium hydroxide, then processing for 30000 turns in a pulping machine, then placing the obtained pulp for 12h at 0 ℃, then diluting the pulp to 0.5g/L, and carrying out suction filtration on the pulp to form paper with the thickness of 17g/m2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80 ℃ for 30s under the pressure of 0.1MPa, repeating the hot pressing for 3 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
The paper pulp is reed pulp.
The organic solvent is ethanol.
The paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode plate under the pressure of 5MPa for use.
The residual amount of xylose in the electrolytic cell under the irradiation of simulated sunlight is 18.4 percent, and the residual amount of xylose in the electrolytic cell under the irradiation of ultraviolet light with the wavelength of 360nm is 12.7 percent.

Claims (5)

1. A preparation method of a paper-based photoelectrocatalysis material for catalyzing xylose oxidation comprises the following operation steps:
adding 2.4-16.2 parts of citric acid into 160 parts of 100-one organic solvent by mass, stirring and mixing uniformly, adding 0.3-3.5 parts of indium chloride into a reaction kettle, stirring and mixing uniformly, controlling the pH value to be 1-3, then adding 0.42-4.8 parts of thioacetamide into the reaction kettle, stirring and mixing uniformly, adding 1-20 parts of surface nano-fibrillated transparent paper scraps, controlling the temperature to be 80-100 ℃, stirring and reacting for 10-20 hours, filtering after the reaction is finished, taking out a sample, cleaning and drying ethanol, adding the obtained material into a hydrothermal reaction kettle, adding 0.6-4.2 parts of nickel nitrate, 0.2-2.4 parts of 1, 1' -bis (dimethylsilyl) ferrocene, 1.6-14.2 parts of urea and 50-80 ℃ deionized water, stirring and mixing uniformly, controlling the temperature to be 130 ℃, carrying out hydrothermal reaction for 5-10h, filtering, washing and drying after the reaction is finished to obtain the paper-based photoelectrocatalysis material for catalyzing xylose oxidation;
the preparation method of the surface nano-fibrillated transparent paper scrap comprises the following steps:
according to the mass parts, 100-200 parts of paper pulp with the mass percentage concentration of 20-40 percent is added into a beating machine, adding into 1.2-3.5 portions of zinc chloride and 400 portions of hydrochloric acid with the mass percentage concentration of 1-5%, stirring at 40-60 deg.C for 5-10h, filtering, washing with water to pH =7, filtering, then evenly mixing with 10-18 parts of N-polyamide polyamine epichlorohydrin resin, 5-11 parts of 3-aminopropyl trihydroxy silane, 200-300 parts of water and 1.2-3.4 parts of sodium hydroxide, then treating 30000-50000 turns in a refiner, then placing the obtained slurry at 0-10 ℃ for 12-36h, then diluting the pulp to 0.5-5g/L, and carrying out suction filtration on the pulp to obtain paper with the thickness of 17-24 g/m.2Then clamping the paper by a polytetrafluoroethylene film, carrying out hot pressing at 80-100 ℃ for 30-60s under the pressure of 0.1-1MPa, repeating the hot pressing for 3-5 times, and finally crushing the obtained transparent paper to obtain the surface nano-fibrillated transparent paper scrap.
2. The preparation method of the paper-based photoelectrocatalysis material for catalyzing xylose oxidation according to claim 1, which is characterized in that: the paper pulp is reed pulp, bagasse pulp, bamboo pulp or cotton pulp.
3. The preparation method of the paper-based photoelectrocatalysis material for catalyzing xylose oxidation according to claim 1, which is characterized in that: the organic solvent is ethanol or methanol or isopropanol.
4. The preparation method of the paper-based photoelectrocatalysis material for catalyzing xylose oxidation according to claim 1, which is characterized in that: the paper-based photoelectrocatalysis material for catalyzing xylose oxidation is pressed into an electrode slice by pressure of 5-15MPa for use.
5. The preparation method of the paper-based photoelectrocatalysis material for catalyzing xylose oxidation according to claim 1, which is characterized in that: the N-polyamide polyamine epichlorohydrin resin, 3-aminopropyl trihydroxy silane and chlorinated paper cellulose are reacted to improve the wet reinforcement performance.
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