20 results about "Sodium amide" patented technology

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 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 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 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 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.

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 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.

The invention discloses a preparation method of 2, 2-diisopropyl propionitrile, and belongs to the technical field of synthesis of food additive intermediates. Comprising the following steps: S1, adding sodium amide, a solvent and a catalyst into a reactor, and stirring until the materials are uniformly dispersed to obtain a reaction system; s2, uniformly mixing 2, 3-dimethyl butyronitrile and 2-bromopropane to form a premixed solution; dropwise adding the premixed solution into a reaction system, and continuously stirring and reacting for 0.5-1 hour after dropwise adding; s3, dropwise adding deionized water into the reaction system to quench the reaction; after the quenching reaction, cooling and stirring a reaction system, standing for layering, and retaining an upper organic phase; s4, transferring the organic phase into a distillation device, carrying out atmospheric distillation, and separating out a solvent; the atmospheric distillation temperature is 60-90 DEG C; and carrying out reduced pressure distillation on the organic phase after atmospheric distillation, and collecting fractions to obtain the product. The 2, 2-diisopropyl propionitrile prepared by the method disclosed by the invention is high in yield and high in purity.

The application belongs to the technical field of luminescent materials, and relates to an interstitial carbene-copper(I)-carbazole compound with room-temperature phosphorescence and a preparation method thereof. The method specifically comprises the following steps: under the atmosphere of an inert gas, taking an interstitial carbene precursor as a starting material, deprotonating the C4 position of the interstitial carbene precursor by sodium bis(trimethylsilyl)amide in the presence of a solvent and cuprous iodide to obtain a double-coordinated interstitial carbene copper(I) complex, and then reacting the double-coordinated interstitial carbene copper(I) complex with a potassium carbazole salt to obtain the interstitial carbene-copper(I)-carbazole compound. The application first uses an interstitial carbene as an organic ligand, develops a novel synthesis method of a linear double-coordinated interstitial carbene-copper(I)-carbazole compound with room-temperature phosphorescence, enriches the types of copper(I) complexes with phosphorescence emission, and realizes fine adjustment of phosphorescence properties by changing the substituent groups of the 2nd carbon atom on the carbene ring.

The invention discloses a preparation method of m-dibutylaminophenol, and relates to the technical field of carbocyclic compound preparation, the m-dibutylaminophenol comprises the following raw materials: 2-chlorophenol, 2, 6-di-tert-butyl-4-methylphenol, zinc chloride, tetrabutylammonium bromide, sodium amide, potassium tert-butoxide, an activated 3A molecular sieve, di-n-butylamine and triethylamine; according to the invention, 2-chlorophenol is used as a core reaction substrate, the structure arrangement of ortho-position chlorine atoms and hydroxyl is highly adaptive, hydrogen chloride can be accurately removed under the action of strong alkali to generate a benzyne intermediate, and a stable benzene ring skeleton is provided for a target product; through the synergistic effect of the activated 3A molecular sieve, the 2, 6-di-tert-butyl-4-methylphenol and the potassium tert-butoxide, the total impurity content is greatly reduced, the product purity and color are remarkably optimized, and the synchronous improvement of the reaction efficiency and the product quality is realized.

The application discloses a biomass-based activated carbon material, relates to the technical field of activated carbon material preparation, and comprises the following components in parts by weight: 1 part of mandarin peel meal; and 1-2 parts of fir bark. The application further discloses a preparation method of the biomass-based activated carbon material, and specifically comprises the following steps: S1, drying, crushing and mixing the mandarin peel meal and the fir bark to obtain mixed raw material A; S2, placing the mixed raw material A into an evaporator and evaporating at low temperature to obtain mixed raw material A with high sulfuric acid salt content; S3, ultrasonic immersion and drying the mixed raw material A with high sulfuric acid salt content, and then carbonizing and activating the mixed raw material A to obtain mixed carbon material B; and S4, mixing the mixed carbon material B with sodium amide, and activating in an air-tight manner to obtain the biomass-based activated carbon material. The biomass-based activated carbon material with stable quality is prepared by solving the problem of unstable quality of the biomass-based activated carbon material caused by unstable quality of desulfurization waste liquid in the prior art, the pore structure of the biomass-based activated carbon material is further optimized, and the adsorption performance is improved.