CN108276309B - Foaming agent and preparation method and application thereof - Google Patents
Foaming agent and preparation method and application thereof Download PDFInfo
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- CN108276309B CN108276309B CN201810246090.0A CN201810246090A CN108276309B CN 108276309 B CN108276309 B CN 108276309B CN 201810246090 A CN201810246090 A CN 201810246090A CN 108276309 B CN108276309 B CN 108276309B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C281/00—Derivatives of carbonic acid containing functional groups covered by groups C07C269/00 - C07C279/00 in which at least one nitrogen atom of these functional groups is further bound to another nitrogen atom not being part of a nitro or nitroso group
- C07C281/20—Derivatives of carbonic acid containing functional groups covered by groups C07C269/00 - C07C279/00 in which at least one nitrogen atom of these functional groups is further bound to another nitrogen atom not being part of a nitro or nitroso group the two nitrogen atoms of the functional groups being doubly-bound to each other, e.g. azoformamide
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention provides a preparation method of a foaming agent, which comprises the steps of mixing a biurea aqueous solution containing biurea and a thickening agent with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution, wherein the pH value of the biurea aqueous solution is 1-2, the cocatalyst is ferric salt, dropwise adding hydrogen peroxide with the mass fraction of 25-35% into the precursor solution to perform an oxidation reaction to obtain primary crystals, and drying the primary crystals at the dropwise adding speed of 0.6-0.7 m L/min to obtain the foaming agent.
Description
Technical Field
The invention relates to the technical field of foaming agents, and particularly relates to a foaming agent and a preparation method and application thereof.
Background
The microcellular foam material has the advantages of high specific strength, high impact strength, high toughness, long fatigue resistance time, good thermal stability and the like, so that the microcellular foam material becomes one of research hotspots.
The azodicarbonamide foaming agent has the characteristics of large gas forming amount, wide decomposition temperature, no residue after decomposition and the like, and has good cell structures during normal-pressure foaming and pressurized foaming, so that the azodicarbonamide foaming agent is the most widely used foaming agent and accounts for about 40-50% of the consumption of a chemical foaming agent. The key of the quality of the azodicarbonamide foaming agent depends on the size of the particle size of the azodicarbonamide and the distribution of the particle size. The smaller the particle size of the azodicarbonamide is, the lower the decomposition temperature of the azodicarbonamide is, and the higher the decomposition speed is; the narrower the particle size distribution of the azodicarbonamide, the more uniform the cell structure obtained by the azodicarbonamide foaming. However, the particle size of the azodicarbonamide foaming agent in China is usually 25-50 μm and the particle size distribution is not uniform, so that the requirement of the microporous foaming material cannot be met.
In order to prepare azodicarbonamide foaming agents with small particle size and uniform distribution, a jet milling method, a urea addition method, an optimized oxidation process and a hypochlorous acid oxidation method are researched. The jet milling method is that a jet mill is used for providing high-speed airflow to impact materials, and the materials are subjected to a self-grinding effect to achieve the effect of refining particles; the urea adding method is that a certain amount of urea is added in the oxidation reaction process to obtain the azodicarbonamide foaming agent; the optimized oxidation process is to further improve the conditions of catalyst dosage, reaction temperature, reaction time and the like, and simultaneously add some surfactants to obtain the azodicarbonamide foaming agent; the hypochlorous acid oxidation method is to prepare an azodicarbonamide foaming agent by using hypochlorous acid as an oxidizing agent. Although the particle size of the prepared azodicarbonamide foaming agent can be reduced by the method, the average particle size of the azodicarbonamide foaming agent prepared by the method is only 7-9 μm at the lowest, and the requirement of a microcellular foaming material cannot be met.
Disclosure of Invention
The invention provides a preparation method of a foaming agent, and the foaming agent with small average particle size can be prepared by the method provided by the invention.
The invention provides a preparation method of a foaming agent, which comprises the following steps:
(1) providing an aqueous solution of biurea, wherein the aqueous solution of biurea comprises biurea and a thickening agent; the pH value of the biurea aqueous solution is 1-2;
(2) mixing the biurea aqueous solution obtained in the step (1) with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution; the cocatalyst contains trivalent ferric salt;
(3) dropwise adding hydrogen peroxide into the precursor solution obtained in the step (2) for oxidation reaction to obtain primary crystals, wherein the dropwise adding speed of the hydrogen peroxide is 0.6-0.7 m L/min, and the mass fraction of the hydrogen peroxide in the hydrogen peroxide is 25-35%;
(4) and (4) drying the primary crystal obtained in the step (3) to obtain the foaming agent.
Preferably, the pH value of the biurea aqueous solution in the step (1) is adjusted by acid; the acid is sulfuric acid.
Preferably, the mass ratio of the biurea, the sodium bromide and the cocatalyst in the aqueous solution of the biurea in the step (2) is 1: 0.03-0.07: 0.01-0.02;
the volume ratio of the mass of the biurea to the foaming agent in the biurea aqueous solution is 1g: 0.01-0.03 m L.
Preferably, the promoter in the step (2) is ferric chloride; the foaming agent is fatty alcohol polyoxyethylene ether sodium sulfate or lauryl sodium sulfate.
Preferably, the volume ratio of the mass of the biurea for preparing the precursor solution in the step (3) to the hydrogen peroxide is preferably 35-45 g: 50-70 m L.
Preferably, the dropping speed of the hydrogen peroxide in the step (3) is 0.5-1.0 m L/min.
Preferably, the temperature of the oxidation reaction in the step (3) is 45-55 ℃, and the time of the oxidation reaction is 1.5-2 h.
Preferably, the drying temperature in the step (4) is 40-60 ℃, and the drying time is 10-15 h.
The invention provides the foaming agent prepared by the preparation method in the technical scheme, and the particle size of the foaming agent is 100-600 nm.
The invention also provides application of the foaming agent in the technical scheme in preparation of a foaming material.
The invention provides a preparation method of a foaming agent, which comprises the following steps of providing a biurea aqueous solution, wherein the biurea aqueous solution comprises biurea and a thickening agent, the pH value of the biurea aqueous solution is 1-2, mixing the biurea aqueous solution with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution, wherein the cocatalyst is ferric salt, dropwise adding hydrogen peroxide into the precursor solution to perform an oxidation reaction to obtain primary crystals, wherein the dropwise adding speed of the hydrogen peroxide is 0.5-1.0 m L/min, the mass fraction of hydrogen peroxide in the hydrogen peroxide is 25-35%, drying the primary crystals to obtain the foaming agent, reacting the cocatalyst with the hydrogen peroxide to generate hydroxyl radicals, wherein the hydroxyl radicals have strong oxidizing property, the bromide ions of the sodium bromide are oxidized into bromine gas, the generated bromine gas reacts with the biurea to oxidize the biurea to obtain azodicarbonamide, and finally the bromine gas can become bromide ions to return to the reaction solution, and the bromine gas can generate a large amount of gas to generate the azodicarbonamide, so that the average particle size of the azodicarbonamide prepared azodicarbonamide is 100 nm, and the azo crystal foaming agent is obtained by the preparation method.
Drawings
FIG. 1 is a scanning electron microscope image of an azodicarbonamide foaming agent prepared in comparative example 1;
FIG. 2 is a scanning electron micrograph of an azodicarbonamide foaming agent prepared in example 1;
FIG. 3 is a graph showing the particle size distribution of the azodicarbonamide foaming agent prepared in example 1;
FIG. 4 is a DSC decomposition temperature profile of the azodicarbonamide foaming agent prepared in example 1 and comparative example 1.
Detailed Description
The invention provides a preparation method of a foaming agent, which comprises the following steps:
(1) providing an aqueous solution of biurea, wherein the aqueous solution of biurea comprises biurea and a thickening agent; the pH value of the biurea aqueous solution is 1-2;
(2) mixing the biurea aqueous solution obtained in the step (1) with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution; the cocatalyst contains trivalent ferric salt;
(3) dropwise adding hydrogen peroxide into the precursor solution obtained in the step (2) for oxidation reaction to obtain primary crystals, wherein the dropwise adding speed of the hydrogen peroxide is 0.6-0.7 m L/min, and the mass fraction of the hydrogen peroxide in the hydrogen peroxide is 25-35%;
(4) and (4) drying the primary crystal obtained in the step (3) to obtain the foaming agent.
In the present invention, as the raw materials in the method for producing the blowing agent, commercially available products known to those skilled in the art may be used, unless otherwise specified.
In the invention, the volume ratio of the mass of the biurea, the mass of the thickening agent and water is preferably 35-45 g: 2-6 g:100m L, more preferably 38-42 g: 3-5 g:100m L, and even more preferably 40g:4g:100m L.
In the present invention, the biurea, the thickener, the acid, and the water are preferably mixed in a manner of: the method comprises the steps of mixing biurea and water, mixing a mixed system of the biurea and the water with a thickening agent, and mixing the mixed system of the biurea, the water and the thickening agent with acid. The invention preferably adopts the mixing mode, which is favorable for fully playing the function of the thickening agent, improving the viscosity of the biurea aqueous solution, further being favorable for stabilizing bubbles to form a complete bubble liquid film state, and avoiding the phenomenon that the bubbles float above the liquid due to the over-diluted biurea aqueous solution to form a gas-liquid separation state which is not favorable for the subsequent reaction on the bubble liquid film.
In the present invention, the pH of the aqueous biurea solution is 1 to 2, preferably 1.2 to 1.8, and more preferably 1.4 to 1.6. In the present invention, the pH of the aqueous biurea solution is preferably adjusted with an acid; the acid is preferably sulfuric acid, and the mass concentration of the sulfuric acid is preferably 70% to 98%, and more preferably 80% to 90%. In the present invention, the acid serves to adjust the pH of the aqueous biurea solution. In the present invention, the acid is preferably used in such an amount that the pH of the aqueous biurea solution is adjusted to a desired pH.
After the biurea aqueous solution is obtained, the biurea aqueous solution is mixed with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution.
In the present invention, the co-catalyst is preferably ferric chloride; the foaming agent is preferably sodium fatty alcohol-polyoxyethylene ether sulfate or lauryl sodium sulfate, and more preferably sodium fatty alcohol-polyoxyethylene ether sulfate. The subsequent oxidation reaction is carried out under the action of the sodium bromide and the cocatalyst, and simultaneously, the subsequent oxidation reaction can be carried out on a bubble liquid film under the action of the bubble agent, so that the preparation of the azodicarbonamide foaming agent with smaller particle size and narrow particle size distribution is facilitated.
In the present invention, the mass ratio of the biurea in the aqueous biurea solution, the mass of the sodium bromide, and the co-catalyst is preferably 1:0.03 to 0.07:0.01 to 0.02, more preferably 1:0.04 to 0.06:0.012 to 0.018, still more preferably 1:0.045 to 0.055:0.014 to 0.016.
The mixing of the aqueous biurea solution, sodium bromide, cocatalyst and blowing agent is not particularly required in the present invention, and may be performed in a manner well known to those skilled in the art. In the invention, a biurea aqueous solution is mixed with sodium bromide, a cocatalyst and a foaming agent to obtain a mixed feed liquid containing the biurea, the sodium bromide, the cocatalyst and the foaming agent, and the mixed feed liquid is used as a precursor solution of a subsequent oxidation reaction.
After the precursor solution is obtained, hydrogen peroxide is dropwise added into the precursor solution for oxidation reaction to obtain primary crystals.
In the invention, the volume ratio of the mass of the biurea for preparing the precursor solution to the hydrogen peroxide is preferably 35-45 g to 50-70 m L, more preferably 38-42 g to 55-65 m L, more preferably 40-42 g to 60-65 m L, and the mass fraction of the hydrogen peroxide in the hydrogen peroxide is 25-35%, preferably 28-32%, and more preferably 30%.
The method comprises the steps of mixing the precursor solution with hydrogen peroxide in a manner of dropwise adding hydrogen peroxide into the precursor solution, so that the hydrogen peroxide and the precursor solution are mixed and simultaneously subjected to oxidation reaction, wherein the hydrogen peroxide reacts with a cocatalyst in the oxidation reaction process to generate hydroxyl radicals, the hydroxyl radicals have strong oxidizing property, bromide ions of sodium bromide are oxidized into bromine gas, and biurea is oxidized into azodicarbonamide by the bromine gas.
The dropping speed of the hydrogen peroxide is 0.6-0.7 m L/min, preferably 0.62-0.68 m L/min, and more preferably 0.64-0.66 m L/min.
In the invention, the temperature of the oxidation reaction is preferably 45-55 ℃, more preferably 48-53 ℃, and more preferably 50-52 ℃. In the present invention, the time of the oxidation reaction is preferably 1.5 to 2 hours, and more preferably 1.6 to 1.8 hours. In the invention, the time of the oxidation reaction is preferably the time of continuing the reaction after the dropwise addition of the hydrogen peroxide is completed.
Is counted after the dropping of the hydrogen peroxide is finished. The invention preferably controls the temperature of the oxidation reaction by means of water bath heating.
The invention controls the temperature of the oxidation reaction, is beneficial to the stable operation of the oxidation reaction and further ensures that the azodicarbonamide foaming agent with small average grain diameter and narrow grain diameter distribution is obtained.
After the oxidation reaction, the oxidation product is preferably subjected to washing and solid-liquid separation treatment in sequence to obtain clean primary crystals. In the invention, the detergent for washing is preferably clear water, and the washing degree is preferably based on that impurities in the detergent cannot be seen by naked eyes; the impurities are preferably one or more of xanthan gum, foaming agent, residual ferric chloride and sodium bromide. In the invention, the solid-liquid separation preferably adopts a centrifugal method to separate the detergent and the primary crystals, and the primary crystals are collected.
After the primary crystal is obtained, the invention dries the primary crystal to obtain the foaming agent. In the invention, the drying temperature is preferably 40-60 ℃, more preferably 45-55 ℃, and more preferably 50-52 ℃; the drying time is preferably 10-15 h, more preferably 11-14 h, and even more preferably 12-13 h. According to the invention, the azodicarbonamide foaming agent with smaller average particle size and narrower particle size distribution is obtained by drying the primary crystals.
The invention provides the foaming agent obtained by the preparation method in the technical scheme. In the present invention, the structural formula of the foaming agent is represented by formula I:
in the invention, the particle size of the foaming agent is 100-600 nm.
The invention also provides application of the foaming agent in the technical scheme in preparation of a foaming material. The method for preparing the foaming material by using the foaming agent is not particularly required, and the method for preparing the foaming material by using the foaming agent is well known to those skilled in the art.
The blowing agent, the preparation method and the application thereof in the present invention will be clearly and completely described below with reference to the examples in the present invention.
Example 1
Mixing 40g of biurea with 50m L of water, fully dissolving the biurea, adding 4g of xanthan gum as a thickening agent, adding 50m L of water, stirring to form a viscous state, slowly dropwise adding 9.8g of concentrated sulfuric acid, and adjusting the pH value of the mixed solution to 2 to obtain a biurea aqueous solution;
adding 2g of sodium bromide, 0.5g of ferric chloride and 1m of L sodium alcohol ether sulfate into the prepared biurea aqueous solution, and fully mixing by using mechanical stirring to obtain a precursor solution;
heating the precursor solution in water bath, after the temperature reaches 50 ℃, dropwise adding 60m L hydrogen peroxide at the speed of 0.66m L/min by using a peristaltic pump, wherein a large amount of gas is generated by decomposition of the hydrogen peroxide and a large amount of bubbles are generated by high-strength dispersion stirring, the oxidation reaction is carried out on a bubble liquid film, the generated azodicarbonamide crystal only grows on the liquid film, and the growth of the crystal is inhibited by the liquid film wall so as to achieve the purpose of refining;
after the reaction is finished, washing a large amount of reaction liquid with clear water, separating and pouring out upper-layer liquid through a centrifugal machine, and finally placing the reaction liquid in a 50 ℃ oven for 12 hours to obtain the azodicarbonamide foaming agent with small average particle size.
Example 2
Mixing 35g of biurea with 50m L of water, fully dissolving the biurea, adding 2g of xanthan gum as a thickening agent, adding 50m L of water, stirring to form a viscous state, slowly dropwise adding concentrated sulfuric acid, and adjusting the pH value of the mixed solution to 3 to obtain a biurea aqueous solution;
adding 1.0g of sodium bromide, 0.1g of ferric chloride and 0.5m of L m of sodium fatty alcohol polyoxyethylene ether sulfate into the prepared biurea aqueous solution, and fully mixing by using mechanical stirring to obtain a precursor solution;
heating the precursor solution in water bath, after the temperature reaches 40 ℃, dropwise adding 50m L hydrogen peroxide at the speed of 0.5m L/min by using a peristaltic pump, wherein a large amount of gas is generated by decomposition of the hydrogen peroxide and a large amount of bubbles are generated by high-strength dispersion stirring, the oxidation reaction is carried out on a bubble liquid film, the generated azodicarbonamide crystal only grows on the liquid film, and the growth of the crystal is inhibited by the liquid film wall so as to achieve the purpose of refining;
after the reaction is finished, washing a large amount of reaction liquid with clear water, separating and pouring out upper-layer liquid through a centrifugal machine, and finally placing the reaction liquid in an oven at 40 ℃ for 10 hours to obtain the azodicarbonamide foaming agent with small average particle size.
Example 3
Mixing 45g of biurea with 50m of L water, fully dissolving the biurea, adding 6g of xanthan gum as a thickening agent, adding 50m of L water, stirring to form a viscous state, slowly dropwise adding concentrated sulfuric acid, and adjusting the pH value of the mixed solution to 2 to obtain a biurea aqueous solution;
adding 4g of sodium bromide, 1.0g of ferric chloride and 2m of L sodium alcohol ether sulfate into the prepared biurea aqueous solution, and fully mixing by using mechanical stirring to obtain a precursor solution;
heating the precursor solution in water bath, after the temperature reaches 50 ℃, dropwise adding 70m L hydrogen peroxide at the speed of 1.0m L/min by using a peristaltic pump, wherein a large amount of gas is generated by decomposition of the hydrogen peroxide and a large amount of bubbles are generated by high-strength dispersion stirring, the oxidation reaction is carried out on a bubble liquid film, the generated azodicarbonamide crystal can only grow on the liquid film, and the growth of the crystal is inhibited by the liquid film wall, so that the refining purpose is achieved;
after the reaction is finished, washing a large amount of reaction liquid with clear water, separating and pouring out upper-layer liquid through a centrifugal machine, and finally placing the reaction liquid in a 60 ℃ oven for 15 hours to obtain the azodicarbonamide foaming agent with small average particle size.
Example 4
Mixing 40g of biurea with 50m of L water, fully dissolving the biurea, adding 4g of xanthan gum as a thickening agent, adding 50m of L water, stirring to form a viscous state, slowly dropwise adding concentrated sulfuric acid, and adjusting the pH value of the mixed solution to 3 to obtain a biurea aqueous solution;
adding 2.5g of sodium bromide, 0.8g of ferric chloride and 1.5m of L m of sodium fatty alcohol polyoxyethylene ether sulfate into the prepared biurea aqueous solution, and fully mixing by using mechanical stirring to obtain a precursor solution;
heating the precursor solution in water bath, after the temperature reaches 50 ℃, dropwise adding 65m L hydrogen peroxide at the speed of 0.7m L/min by using a peristaltic pump, wherein a large amount of gas is generated by decomposition of the hydrogen peroxide and a large amount of bubbles are generated by high-strength dispersion stirring, the oxidation reaction is carried out on a bubble liquid film, the generated azodicarbonamide crystal only grows on the liquid film, and the growth of the crystal is inhibited by the liquid film wall so as to achieve the purpose of refining;
after the reaction is finished, washing a large amount of reaction liquid with clear water, separating and pouring out upper-layer liquid through a centrifugal machine, and finally placing the reaction liquid in an oven at 55 ℃ for 13 hours to obtain the azodicarbonamide foaming agent with small average particle size.
Comparative example 1
The experiment was carried out as in example 1, except that no thickener and no foaming agent were added.
Scanning electron microscope analysis is carried out on the azodicarbonamide foaming agent prepared in example 1 and comparative example 1, as shown in fig. 1 and fig. 2, wherein fig. 1 is the azodicarbonamide foaming agent prepared in comparative example 1; FIG. 2 shows the azodicarbonamide blowing agent prepared in example 1. As can be seen from the test results in FIG. 1, the particle size of the azodicarbonamide foaming agent prepared in comparative example 1 is about 20 μm; as can be seen from the results of the test in FIG. 2, the azodicarbonamide foaming agent prepared in example 1 has a particle size of less than about 1 μm. Therefore, the method of the invention can prepare the azodicarbonamide foaming agent with smaller particle size.
The azodicarbonamide foaming agent prepared in example 1 was subjected to a particle size distribution test using a laser particle sizer, and the test results are shown in fig. 3. The test result of FIG. 3 shows that the particle size of the azodicarbonamide foaming agent prepared by the invention is 100-600 nm and is small.
The particle sizes of the azodicarbonamide foaming agents prepared in examples 1-4 and comparative example 1 were measured by a laser particle size analyzer, and the measurement results are shown in table 1.
TABLE 1 particle size and particle size distribution Range of blowing agents prepared in examples 1-4 and comparative example 1
The average particle diameter preferably means an average particle diameter obtained by statistically averaging all particle diameters.
The test results of the examples 1-4 and the comparative example 1 show that the average particle size of the azodicarbonamide foaming agent prepared by the preparation method provided by the invention is smaller; the method can prepare the azodicarbonamide foaming agent with the average grain diameter less than 1 mu m.
The DSC decomposition temperatures of the foaming agents prepared in example 1 and comparative example 1 were measured, and the results are shown in FIG. 4.
As can be seen from FIG. 4, the DSC decomposition temperature of the foaming agent provided in example 1 of the present invention was reduced by about 30 ℃ compared to that of the foaming agent provided in comparative example 1. The smaller the particle size, the lower the decomposition temperature. Therefore, the particle size of the blowing agent provided by the present invention is smaller as can be seen from the decomposition temperatures of example 1 and comparative example 1 of the present application.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for preparing a foaming agent comprises the following steps:
(1) providing an aqueous solution of biurea, wherein the aqueous solution of biurea comprises biurea and a thickening agent; the pH value of the biurea aqueous solution is 1-2;
(2) mixing the biurea aqueous solution obtained in the step (1) with sodium bromide, a cocatalyst and a foaming agent to obtain a precursor solution; the cocatalyst contains trivalent ferric salt;
(3) dropwise adding hydrogen peroxide into the precursor solution obtained in the step (2) for oxidation reaction to obtain primary crystals, wherein the dropwise adding speed of the hydrogen peroxide is 0.6-0.7 m L/min, and the mass fraction of the hydrogen peroxide in the hydrogen peroxide is 25-35%;
(4) drying the primary crystal obtained in the step (3) to obtain a foaming agent;
the thickening agent is xanthan gum; the foaming agent is fatty alcohol-polyoxyethylene ether sodium sulfate.
2. The method according to claim 1, wherein the pH of the aqueous solution of biurea in step (1) is adjusted with an acid; the acid is sulfuric acid.
3. The preparation method according to claim 1, wherein the mass ratio of the biurea, the sodium bromide and the cocatalyst in the aqueous solution of the biurea in the step (2) is 1: 0.03-0.07: 0.01-0.02;
the volume ratio of the mass of the biurea to the foaming agent in the biurea aqueous solution is 1g: 0.01-0.03 m L.
4. The method according to claim 1 or 3, wherein the cocatalyst in the step (2) is ferric chloride.
5. The preparation method according to claim 1, wherein the mass ratio of the biurea for preparing the precursor solution in the step (3) to the hydrogen peroxide is preferably 35-45 g: 50-70 m L.
6. The preparation method according to claim 1 or 5, wherein the dropping speed of the hydrogen peroxide in the step (3) is 0.5-1.0 m L/min.
7. The preparation method according to claim 1, wherein the temperature of the oxidation reaction in the step (3) is 45-55 ℃ and the time of the oxidation reaction is 1.5-2 h.
8. The preparation method according to claim 1, wherein the drying temperature in the step (4) is 40-60 ℃ and the drying time is 10-15 h.
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Effective date of registration: 20221125 Address after: Plant 101, building 13, industrialization base of small and medium sized enterprises, biological medicine Park, 1777 Dazheng Road, high tech Zone, Jinan City, Shandong Province Patentee after: Shandong Boke Scientific Instrument Co.,Ltd. Address before: 412000 School of Packaging and Materials Engineering, Hunan University of Technology, No. 88, Taishan West Road, Tianyuan District, Zhuzhou City, Hunan Province Patentee before: HUNAN University OF TECHNOLOGY |