39 results about "Sodium amide" patented technology

The invention provides a synthesis method of tris (dimethylamino) cyclopentadienyl hafnium, which comprises the following steps: reacting hafnium tetrachloride with sodium dimethylamino at a first temperature under the protection of inert gas to form an intermediate; heating and settling, cooling to a second temperature, dropwise adding cyclopentadiene, and filtering, distilling and purifying to obtain a target product. According to the method, high yield and high purity are achieved by optimizing the raw material ratio and controlling the dropwise adding temperature and the use amount of cyclopentadiene. The byproduct sodium chloride is large in particle and easy to filter, the post-treatment process is remarkably simplified, and the process safety, controllability and industrial adaptability are improved.

The invention belongs to the technical field of synthesis of food additive cooling agent intermediates, and particularly relates to a method for efficiently preparing 2, 2-diisopropyl propionitrile. According to the method, the solubility of sodium amide is promoted through the complexing action of the nitrogen-containing organic solvent in the reaction process, the reaction rate is increased, the situation that ultralow-temperature conditions and pressure-resistant equipment need to be used in the reaction process is avoided, and the operation difficulty of the reaction is reduced. The technical scheme provided by the invention simultaneously has the advantages of a liquid ammonia method and a solvent method in the prior art, the production energy consumption is reduced, the reaction rate is accelerated, and the production safety coefficient is improved. The industrial production is favorably realized.

The invention belongs to the field of fine chemical engineering, and discloses a method for synthesizing 2, 3-dimethyl-2-isopropyl butyronitrile, which comprises the following steps of: adding an organic amine solvent into a high-pressure reaction kettle, adding sodium amide, sodium iodide and a phase transfer catalyst into the reaction kettle under the protection of nitrogen and in a stirring state, stirring for a certain period of time, and reacting for 2-3 hours to obtain 2, 3-dimethyl-2-isopropyl butyronitrile. Dropwise adding a mixed solution of propionitrile and 2-bromopropane into the reactor, controlling the dropwise adding speed and the reaction temperature, continuously reacting for a period of time after the dropwise adding is finished to obtain a reactant solution, cooling the reactant solution, adding water, standing for layering, collecting an organic phase, distilling the organic phase at normal pressure to recover a solvent, and rectifying at reduced pressure to obtain 2, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3-pentanediol. According to the method, the sodium iodide, the phase transfer catalyst and the organic amine have a synergistic effect, so that the reaction time is shortened, and the yield of the product is improved.

The application discloses a preparation method and application of a bimodal linear polyethylene chromium carbene catalyst, and belongs to the technical field of chemical synthesis. The preparation method comprises the following steps: 1-nitro-2-aromatic sulfide benzene is prepared by taking 1-fluoro-2-nitrobenzene, aromatic mercaptan and potassium tert-butanolate as raw materials; 1-amino-2-aromatic sulfide benzene is prepared by taking 1-nitro-2-aromatic sulfide benzene and hydrazine hydrate as raw materials; 8-hydroxyimidazol[1,5-alpha] quinolinium salt is prepared by taking 1-amino-2-aromatic sulfide benzene, 8-hydroxyquinoline-2-methyl formaldehyde, formaldehyde solution and hydrogen chloride-1,4-dioxane solution as raw materials; and finally, the reaction is carried out by taking 8-hydroxyimidazol[1,5-alpha] quinolinium salt, silver trifluoromethanesulfonate, sodium bis(trimethylsilyl) amide and chromium trichloride as raw materials to obtain the bimodal linear polyethylene chromium carbene catalyst. According to the preparation method, the catalyst is effectively prevented from being poisoned, the catalytic activity of the catalyst is improved, and the catalyst has good thermal stability.

The invention discloses a preparation method of nitrogen-oxygen co-doped microporous carbon based on pre-oxidation assisted sodium amide activation, and the method comprises the following steps: 1, carrying out mechanical crushing and screening on raw coal to obtain powder with a target particle size; 2, weighing coal powder, putting the coal powder into a muffle furnace, heating the coal powder to a target temperature in an air atmosphere, preserving heat for 2-4 hours, then naturally cooling the coal powder to room temperature, and taking out the coal powder for later use; 3, weighing the air pre-oxidized pulverized coal obtained in the step 2, adding an activating agent, and performing solid-phase premixing in a mortar; heating the mixture to a target temperature in an inert protective atmosphere, preserving heat for 0.5-2 hours, cooling to room temperature, and taking out; and 4, repeatedly washing the mixture obtained in the step 3 with deionized water until the pH value reaches 7, and then drying with hot air to obtain the nitrogen-oxygen co-doped microporous carbon. According to the method, porous carbon with large specific surface area and high microporosity / ultra-microporosity is prepared at a lower activation temperature in one step, and efficient doping of nitrogen and oxygen atoms is realized.

The present invention relates to the technical field of pharmaceutical chemistry, and to a method for synthesizing a doravirine intermediate. The synthesis method of the present invention comprises: (1) mixing ethyl 2-fluoroacetate with 4-ethoxy-1,1,1-trifluoro-3-buten-2-one in a first solvent and adding sodium bis(trimethylsilyl)amide for a reaction to generate compound 1; (2) adding triethylamine and trifluoroacetic anhydride to a reaction solution of compound 1 for a reaction to generate compound 2; (3) adding an ammonia source to a reaction solution of compound 2 to obtain compound 3 and compound 4; and (4) adding a second solvent and heating the resulting mixture for cyclization to obtain 2-hydroxy-3-fluoro-4-trifluoromethylpyridine. The present invention has low raw material cost and is a synthesis method, which has a short process cycle, is environmentally friendly, and is suitable for scale-up process production.

The invention provides lubricating grease and a preparation method thereof. The lubricating grease comprises an alkyl phosphonate compound, an antirust agent, an antioxidant, a sodium amide thickening agent and a main amount of lubricating base oil, and a preparation method of the alkyl phosphonate compound comprises the following steps: in the presence of an imine catalyst, enabling alkyl phosphonic acid to react with alkyl alcohol and / or alkylphenol, and collecting a product. The lubricating grease disclosed by the invention has excellent low-volatility performance, oxidation resistance, extreme pressure performance and wear resistance, and is suitable for a lubricating system of space equipment.

The invention relates to a preparation method of (bis (trimethylsilyl) amino) tris (pyrrolidinyl) hafnium, which comprises the following steps: (1) reacting bis (trimethylsilyl) sodium amide with hafnium tetrachloride to obtain (bis (trimethylsilyl) amino) hafnium trichloride; (2) reacting tetrahydropyrrole with sodium hydride to obtain sodium pyrrolidinyl; and (3) carrying out a reaction on the (bis (trimethylsilyl) amino) hafnium trichloride obtained in the step (1) and the sodium pyrrolidinyl obtained in the step (2) to obtain the (bis (trimethylsilyl) amino) tris (pyrrolidinyl) hafnium. By optimizing the preparation method of (bis (trimethylsilyl) amino) tri (pyrrolidinyl) hafnium in the prior art, the obtained method is short in synthesis path and simple in synthesis operation, the use of n-butyllithium is avoided, the danger is reduced, the reaction convenience is improved, the raw material cost is low, the product yield and purity are high, and the method is suitable for industrial production. The industrial large-scale production is facilitated.

The invention provides a sodium amide content determination method, which adopts an ultraviolet-visible spectrophotometer method, and comprises the following steps: dissolving a sodium amide sample in an organic solvent, placing in a container pre-filled with an absorption liquid, sequentially adding an alkaline liquid, a potassium sodium tartrate aqueous solution and a Nessler reagent, uniformly shaking, and standing to obtain a test solution; the organic solvent is one of methanol, ethanol, propanol and isopropanol; the absorption liquid is acidic liquid. Compared with a titration method (related to an operation method of an operator, and large in individual experiment result difference), instrument detection of the method is more sensitive and accurate; sample treatment is simple and safe, testing is accurate, and the recovery rate is high.

The invention relates to the field of high polymer materials, and mainly relates to an ATzP monomer, PATzP wear-resistant resin with a rigid-tough synergistic characteristic and a preparation method of the ATzP monomer and the PATzP wear-resistant resin. The invention relates to a preparation method of an ATzP monomer. The preparation method comprises the following steps: carrying out a reaction on melamine and 4-chloropyrrolopyrimidine to prepare a compound-A; reacting the compound-A with sodium amide to obtain a compound-B; and mixing the compound-B, an acid-binding agent and a polar aprotic solvent B, and then condensing with methacryloyl chloride at the temperature of-35 + / -5 DEG C to obtain the ATzP monomer. The invention relates to a PATzP wear-resistant resin with a rigid-tough synergistic characteristic. The PATzP wear-resistant resin is prepared from the following raw materials: an initiator and an ATzP monomer. On the premise of maintaining high rigidity, the toughness, impact resistance and wear resistance of the material are remarkably improved.

The application belongs to the technical field of photoinitiator preparation, and particularly relates to a preparation method of a photoinitiator FMT, which comprises the following steps: reacting a compound of formula I-1 with an organic metal lithium to obtain a compound of formula I-2; reacting the compound of formula I-2 with titanium tetrachloride to obtain a compound of formula I-3; reacting cyclopentadiene with sodium amide to obtain sodium cyclopentadiene; and reacting the compound of formula I-3 with sodium cyclopentadiene to obtain the photoinitiator FMT shown in formula I. The yield of the photoinitiator FMT product prepared by the preparation method can reach 90% to 95%, the product purity is greater than 99.5%, the solvents used can be recycled and reused, cost is saved, and industrial waste liquid is avoided.

The invention discloses a green and efficient preparation method of 2, 2-dialkyl nitrile, and belongs to the field of organic synthesis. According to the method, a composite catalyst (represented by M1X1-M2X2) composed of an alkali metal chloride and a transition metal halide or thiocyanide is used, in the presence of a saturated fatty alcohol cocatalyst, saturated fatty nitrile, halogenated hydrocarbon and sodium amide are used as raw materials to react at a relatively low temperature, and the 2, 2-alkyl fatty nitrile can be synthesized at a high yield.

The invention belongs to the technical field of environmental functional materials, and particularly relates to a cobalt-nitrogen modified zero-valent iron ternary nitride material, preparation thereof and application of the cobalt-nitrogen modified zero-valent iron ternary nitride material in removal of chlorinated hydrocarbon. The invention provides a cobalt nitrogen modified zero-valent iron ternary nitride material which can be used for removing chlorinated hydrocarbon in a water body. Zero-valent iron serves as a matrix, cobalt powder, sodium amide and zero-valent iron powder are mixed through a mechanochemical method, ball milling is carried out under the inert atmosphere, and the cobalt-nitrogen synergistic modified ternary nitride structure is formed. The cobalt powder and the sodium amide are doped into the surface and the interior of the zero-valent iron, so that the zero-valent iron generates lattice strain, the chlorohydrocarbon dechlorination capacity is improved, the preparation process is simple, low in cost, free of pollution and suitable for large-scale application, and the problems of low degradation efficiency and poor selectivity in chlorohydrocarbon pollution treatment are solved.

An organic solid electrolyte contains sodium bis(fluorosulfonyl)amide (NaFSA) and polyethylene oxide (PEO), and if EO is a constituent unit of PEO, the molar ratio of Na:EO between NaFSA and PEO is in the range of 1:20 to 1:50. A solid-state sodium-ion battery comprises a cathode layer, an organic solid electrolyte layer consisting of the aforementioned organic solid electrolyte layer, an inorganic solid electrolyte layer, and an anode layer, in that order in terms of thickness.

The present invention provides a method for preparing high-purity all-cis-jasmone, belonging to the technical field of organic chemistry. Sodium amide is prepared by reacting sodium with liquid ammonia, a catalyst is added, and the reaction is carried out with stirring. The solvent is removed under reduced pressure. Under the protection of an inert gas and under the condition of an ice-water bath, 2-formylmethyl-3-methyl-cyclopentene-2-one and toluene are added, and the reaction is carried out with heating and stirring. After cooling to room temperature, the product is collected by vacuum distillation to obtain high-purity all-cis-jasmone. The method of the present invention greatly improves the activity and reaction selectivity of the catalyst, enables the reaction to produce cis-jasmone, has a high yield, good selectivity, mild preparation conditions, a simple reaction method, and high product purity.

The invention relates to a synthesis method of a doravirin intermediate, and belongs to the technical field of medicinal chemistry. The synthesis method comprises the following steps: (1) mixing ethyl 2-fluoroacetate and 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone with a solvent I, adding bis (trimethylsilyl) sodium amide, and reacting to generate a compound 1; (2) adding triethylamine and trifluoroacetic anhydride into the reaction liquid of the compound 1, and reacting to generate a compound 2; (3) adding an ammonia source into the reaction liquid of the compound 2 to obtain a compound 3 and a compound 4; and (4) adding a solvent II, heating, and carrying out ring closing, so as to obtain the 2-hydroxy-3-fluoro-4-trifluoromethylpyridine. The synthesis method is low in raw material cost, short in process period, green, environment-friendly and suitable for process amplification production.

The present invention belongs to the technical field of asphalt flue gas purification and discloses a catalyst for rubber asphalt flue gas purification and a preparation method thereof. The preparation method comprises the following steps: using crop waste as a carbon source, drying and crushing the crop waste, and then carbonizing the crop to obtain biochar; mixing the biochar with sodium amide and then activating the biochar to obtain modified biochar; mixing the modified biochar with an acid solution, then hydrothermally reacting the crop waste, filtering, washing, and drying the crop waste to obtain a precursor; placing the precursor in a metal salt solution and ultrasonically treating the mixture to obtain a mixed solution; adding ascorbic acid to the mixed solution, stirring the mixture, filtering, washing, and drying the mixture to obtain the catalyst for rubber asphalt flue gas purification. The catalyst has low preparation cost, a convenient preparation process, and high preparation efficiency, and has good application prospects and industrialization potential. The catalyst prepared by the present invention can quickly and efficiently purify pollutants such as sulfur oxides, nitrogen oxides, and hydrogen sulfide in rubber asphalt flue gas.

The invention belongs to the field of environmental chemistry, and particularly relates to a preparation method and application of a nitrogen-modified zero-valent iron composite material based on the molten salt effect, and the preparation method specifically comprises the steps that iron powder, ferroferric oxide and sodium amide are mixed and subjected to ball milling, and the nitrogen-modified zero-valent iron material is obtained. In the ball milling process, a NaOH-NaNH2 melting interface can be formed in the ball milling tank, so that in-situ formation of nitrogen modified zero-valent iron is promoted. The trichloroethylene removal capability of the nitrogen-modified zero-valent iron material obtained in the preparation process is remarkably enhanced. According to the method, the problem that the nitrogen-modified zero-valent iron is difficult to prepare is solved, and a technical foundation is laid for safe and efficient low-cost short-range macro preparation of the nitrogen-modified zero-valent iron. The method provided by the invention is simple and efficient in process, low in cost and environment-friendly, and can be widely applied to preparation of nitrogen-modified zero-valent iron.

The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing a 1, 3-diboron ester naphthalene compound through aromatization driving, which comprises the following steps: mixing a benzo cyclohexanone derivative with an enol leaving group, bis (pinacol) borate and organic alkali (bis (trimethylsilyl) sodium amide) in a solvent (trifluorotoluene and cyclohexane); the preparation method comprises the following steps: firstly, stirring at room temperature for pre-complexing, then heating to 30-70 DEG C (preferably 40 DEG C), and carrying out double boronation and aromatization reaction to generate the 1, 3-diboron ester naphthalene compound. The preparation method is simple, does not need a transition metal catalyst, avoids the problems of heavy metal residues and biotoxicity, realizes efficient and regioselective double boronation reaction, and solves the problems that a traditional method depends on a metal catalyst and the regioselectivity is poor.

The present invention discloses a green and efficient preparation method of 2,2-diisopropylpropionitrile, which includes: adding an organic solvent into a stainless steel reaction kettle, and adding sodium amide and a metal organic ligand catalyst into the stainless steel reaction kettle under stirring. After stirring at room temperature for half an hour, a dropping reaction is carried out; mixing propionitrile and 2-bromopropane evenly, and then slowly dropping the mixed solution into the reaction kettle, and controlling the dropping time; after the dropping is completed, continue the heat preservation reaction, and sample during the reaction to monitor the end point of the reaction by gas chromatography; after the reaction is completed, cool down and put the reaction solution into a centrifuge to separate the solid and liquid phases, and add the washing solvent into the centrifuge for multiple times, and finally collect the organic phase uniformly; put the organic phase into a distillation kettle, first carry out desolvation under normal pressure, and then carry out vacuum rectification to obtain 2,2-diisopropylpropionitrile. By adopting the above preparation method, the present invention avoids the generation of side reactions under high temperature conditions, thereby achieving the purpose of improving the production yield, reducing the raw material consumption and energy consumption.

The application discloses a preparation method of 2,2-diisopropylpropionitrile and belongs to the technical field of food additive intermediate synthesis. The method comprises the following steps: S1, adding sodium amide, a solvent and a catalyst into a reactor, stirring until being uniformly dispersed, and obtaining a reaction system; S2, uniformly mixing 2,3-dimethylbutyronitrile and 2-bromopropane to form a premix; dropping the premix into the reaction system, continuing to stir for 0.5-1 hours after dropping is completed; S3, adding deionized water into the reaction system to quench the reaction; after quenching the reaction, cooling and stirring the reaction system, layering after standing, and reserving an upper organic phase; S4, transferring the organic phase into a distillation device, performing normal pressure distillation, and separating the solvent; the normal pressure distillation temperature is 60-90 DEG C; performing vacuum distillation on the organic phase after the normal pressure distillation, collecting a distillate, and obtaining a product. The prepared 2,2-diisopropylpropionitrile has high yield and high purity.

The invention discloses a preparation method of unsaturated fatty acid cis-9-tetradecenoic acid, and belongs to the technical field of organic compound preparation. The preparation method provided by the invention comprises the following steps: reacting azelaic acid monomethyl ester with a borane reagent to obtain 9-hydroxy methyl nonanoate; then, the 9-formyl methyl nonanoate reacts with a Dess-Martin oxidizing agent, and 9-formyl methyl nonanoate is obtained; then reacting with n-amyl triphenyl phosphorus bromide or diethyl amyl phosphonate in the presence of bis (trimethylsilyl) sodium amide, so as to obtain cis-9-tetradecenoic acid methyl ester; and finally, carrying out hydrolysis reaction to obtain the cis-9-tetradecenoic acid. According to the method disclosed by the invention, the high-purity cis-9-tetradecenoic acid is efficiently and highly selectively prepared by taking the cheap and easily available monomethyl azelate as a starting raw material through key steps of reduction, oxidation, high-selectivity Wittig alkylenation and the like, and large-scale production is facilitated.

This invention discloses a sodium amide quaternary ammonium salt sulfonate type surfactant, its preparation method, and its application, belonging to the field of fine chemical technology. The molecular structure of the sodium amide quaternary ammonium salt sulfonate type surfactant is as follows: The sodium amide quaternary ammonium salt sulfonate type surfactant is prepared from the following molar ratio of raw materials: cocoylpropyl dimethyl tertiary amine, water, and sodium 2-chloroethyl sulfonate monohydrate in a molar ratio of 1:(35-60):(1.00-1.09). The sodium amide quaternary ammonium salt sulfonate type surfactant of this invention has abundant hydrophilic groups, good antifoaming ability, emulsifying ability, and good surface activity, and can be used as an antifoaming agent, a low-foaming surfactant, or an emulsifier.

The present application provides a method for continuously synthesizing sodium amide and a production device thereof. The method of the present application uses a primary reaction device, continuously adds sodium metal and ammonia gas, and makes the sodium metal react with the ammonia gas to generate sodium amide and hydrogen. The sodium metal and the sodium amide are stratified in the reaction device, the stratified sodium amide forms a settling zone at the lower part of the reaction device, and the sodium amide is continuously removed from the reaction device from the settling zone. The method has the advantages of process stability, low investment, few devices, high ammonia gas utilization rate, low energy consumption and convenient operation, overcomes the defects in the prior art that continuous production must use multiple reaction kettles, and especially overcomes the difficulty that a high-temperature pump must be used to remove the sodium amide product, and for the first time realizes single-tower continuous industrial production.

The invention discloses an ion functionalized biochar material and a preparation method and application thereof, and relates to the field of biochar-based materials, biomass charcoal and sodium amide are mixed and subjected to primary antipyresis for 5-30 min in a protective atmosphere at the temperature of 450-750 DEG C, and sodium amide modified biochar is obtained; mixing the sodium amide modified biochar with chloride and deionized water, carrying out dipping treatment, taking out the sodium amide modified biochar after dipping treatment, and carrying out secondary pyrolysis for 5-30 minutes in a protective atmosphere at the temperature of 450-750 DEG C, so as to obtain the ion functionalized biochar material. Through the short-time pyrolysis and impregnation processing technology, the processing process is simple and convenient to operate, the preparation period is greatly shortened, and the energy consumption is reduced.

The invention relates to a doravirin intermediate as well as application and a synthesis method thereof, and belongs to the technical field of medicinal chemistry. The synthetic method of the doravirin intermediate comprises the following steps: (1) mixing ethyl 2-fluoroacetate and 4-ethoxy-1, 1, 1-trifluoro-3-butene-2-ketone with a solvent I, and dropwise adding bis (trimethylsilyl) sodium amide to form a compound 1; (2) adding an ammonia source into the reaction liquid of the compound 1 to obtain a compound 2; (3) dissolving the compound 2 in a solvent 2, adding a catalyst, and heating for cyclization to obtain a compound 3; and (4) dissolving the compound 3 in toluene, adding thionyl chloride, and dropwise adding pyridine to obtain the 2-hydroxy-3-fluoro-4-trifluoromethylpyridine. The synthesis method is low in raw material cost, short in process period, green, environment-friendly and suitable for process amplification production.

An organic solid electrolyte includes sodium bis(fluorosulfonyl)amide (NaFSA), and polyethylene oxide (PEO), and when a constituent unit of PEO is EO, a molar ratio of Na:EO between NaFSA and PEO is within a range of 1:20 to 1:50. An all-solid-state sodium-ion battery includes a cathode layer, an organic solid electrolyte layer that is made of the above organic solid electrolyte, an inorganic solid electrolyte layer, and an anode layer, in this order in a thickness direction.

The invention belongs to the field of fine chemicals and discloses a method for synthesizing 2,3-dimethyl-2-isopropylbutyronitrile. The method comprises the following steps: adding an organic amine solvent into a high-pressure reactor, and adding sodium amide, sodium iodide and a phase transfer catalyst into the reactor under nitrogen protection and stirring. After stirring for a certain period of time, a mixed solution of propionitrile and 2-bromopropane is added dropwise into the reactor, the dropping speed and the reaction temperature are controlled, and the reaction is continued for a period of time after the dropwise addition is completed to obtain a reactant solution. The reactant solution is cooled and then water is added, the solution is allowed to stand for stratification, an organic phase is collected, the organic phase is first subjected to atmospheric distillation to recover the solvent, and then vacuum distillation is performed to obtain a 2,3-dimethyl-2-isopropylbutyronitrile product. The method shortens the reaction time and improves the product yield through the synergistic effect of the sodium iodide, the phase transfer catalyst and the organic amine.

The invention relates to the technical field of organic synthesis, in particular to a reaction method for activating aromatic boronation of an inert alkenyl C-O bond with participation of a boron reagent, which comprises the following steps: mixing a substrate (such as diethylcarbamic acid benzocyclohexenyl ester or a derivative thereof) containing the inert alkenyl C-O bond, the boron reagent (such as biborate) and a solvent in an inert atmosphere; adding sodium bis (trimethylsilyl) amide, stirring and reacting for 6-16 hours at the temperature of 30-60 DEG C, and finally quenching, extracting, drying and purifying to obtain a target product. The method has the advantages that transition metal catalysis is not needed, cheap and easily available reagents are utilized, the efficient aromatic boronation reaction of inert alkenyl C-O bonds is realized under mild conditions, and the problems of excessive dependence on noble metals, single reaction type, harsh conditions and narrow substrate application range in the prior art are effectively solved.

The invention relates to the technical field of organic chemical synthesis, and particularly discloses a DIPPN synthesis method based on propionitrile, and the DIPPN synthesis method based on propionitrile comprises the following steps: reacting acrylonitrile with hydrogen under the action of a magnetic core-shell bimetallic catalyst, and regenerating the catalyst by adopting supercritical CO2 to obtain DIPPN; high-purity propionitrile is obtained through gas-liquid separation and molecular sieve adsorption purification; then adding a premix of isopropyl bromide and ethyl lactate into a system containing propionitrile, sodium amide and tea saponin for reaction in an inert atmosphere, electrolyzing sodium hydroxide and bromine gas in a regenerated water phase after quenching and layering, and performing reduced pressure distillation and ultrasonic-assisted cooling crystallization on an organic phase to obtain a high-purity DIPPN solid; through supercritical CO2 regeneration of the catalyst, cyclic utilization of reaction byproducts and an ultrasonic-assisted crystallization process, the reaction efficiency, the product purity and the like are remarkably improved, and the obtained DIPPN is suitable for the fields of medicines, materials and the like.