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38results about How to "One-step synthesis" patented technology

One-step synthesis method of surface loaded magnetic Fe2O3 nano-particle colloidal carbon ball

The invention belongs to the nanometer / micrometer scale carbon sphere material preparation technical field, and in particular relates to a method of one-step synthesis for a colloidal carbon sphere with magnetic Fe2O3 nano-particles loaded on the surface. The method comprises the following steps of: dispersing 4-ferrocenyl butyric acid into de-ionized water, the dosage of the 4-ferrocenyl butyric acid in the water being between 1.25 and 8.75 mg / mL; adding the acquired mixture into a reaction kettle; placing the reaction kettle filled with the mixture into a temperature control furnace, heating the reaction kettle to a temperature of between 140 and 180 DEG C, and reacting for 12 to 24 hours, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature to acquire a black product, washing and centrifugalizing, thereby acquiring the required product. The method has the advantages of adjustable technological parameter, simple operation of the whole preparation process, easily-controlled conditions and convenient after-treatment of the product, so the method can be easy for mass production. The method does not generate byproducts which pollute environment during preparation, and accords with the requirement of sustainable development, thereby being an environment-friendly synthesis process.
Owner:TONGJI UNIV

Nitrogen-doped graphene and nitrogen-doped nano tin dioxide composite material and preparation method and application thereof

ActiveCN110148721AControl the speed of the hydrolysis reactionEvenly distributedMaterial nanotechnologyCell electrodesTin dioxideTotal nitrogen
The invention provides a nitrogen-doped graphene and nitrogen-doped nano tin dioxide composite material and a preparation method and application thereof, and the preparation method comprises the following steps: respectively preparing graphene, a tin salt and a nitrogen-containing compound serving as raw materials into solutions; and carrying out mixing, heat treatment, heat preservation and drying to obtain the composite material. In the composite material, the mass percentage ratio of the nitrogen-doped graphene to the nitrogen-doped nano tin dioxide is 5%: 95%-30%: 70%. The crystal grain size of the nitrogen-doped nano tin dioxide is 1-5 nm, the Nitrogen-doped nano tin dioxide is uniformly loaded on the nitrogen-doped graphene. The total nitrogen doping amount of the nitrogen-doped graphene and nitrogen-doped nano tin dioxide composite material is 0.5%-1% of atomic ratio, and the specific surface area is 300-450m<2>/g. By use of the composite material disclosed by the invention, theelectron and lithium ion transmission speed can be effectively improved; the composite material can be used as a negative electrode material of a lithium ion battery; and the method has the advantages of few process steps, easiness in control, high repeatability and high product yield, thereby being beneficial to large-scale popularization.
Owner:FUJIAN JIANGXIA UNIV

Method for preparing bis(hydroxyethyl) bisphenol A ether

The invention relates to a method for preparing bis(hydroxyethyl) bisphenol A ether. The method comprises the following steps: (1) washing a high-pressure reaction kettle with distilled water for several times, and cooling to room temperature for later use; (2) adding bisphenol A and a compound catalyst, vacuumizing to replace air, closing vacuum and beginning to warm when the vacuum degree is greater than or equal to -0.096MPa; (3) heating to 160 DEG C, carrying out vacuum degassing for 10 minutes, lastingly adding ethylene oxide, controlling the reaction temperature to be 150-175 DEG C and the pressure in the reaction kettle to be -0.05MPa to 0.5MPa, carrying out heat preservation after adding is ended, and further reacting until the pressure is not lowered more; and (4) cooling to 100 DEG C after reaction is ended, and carrying out vacuum degassing for 20 minutes, adding a certain amount of glacial acetic acid for neutralizing, cooling to 80 DEG C and emptying to obtain the finished product. The content of bis(hydroxyethyl) bisphenol A ether is greater than or equal to 95.0%; the content of mono-hydroxyethyl bisphenol A ether is smaller than or equal to 0.05%; the residual bisphenol A is smaller than or equal to 3ppm; the hydroxyl value is 350-355mgKOH/g; and the color and luster are 0-30# (Pt-Co unit).
Owner:ZHEJIANG LYUKEAN CHEM

Method for synthesizing sodium diacetate crystal in one step

The invention relates to a method for synthesizing a preservative and antistaling agent, and in particular relates to a method for synthesizing a sodium diacetate crystal in one step. The following raw materials are adopted in percent by weight: 70.4-72.4% of glacial acetic acid, 10.8-12.0% of ionic membrane method caustic soda flake and 16.5-18.6% of anhydrous sodium carbonate. The synthesis steps are as follows: (1) mixing the ionic membrane method caustic soda flake with the anhydrous sodium carbonate, slowly adding the glacial acetic acid and then naturally heating, controlling total reaction time to be 30-50 minutes, and controlling maximum reaction temperature to be 65-85 DEG C; and (2) cooling the temperature below 50-60 DEG C after the reaction is completed, and discharging. By applying the method provided by the invention, solid-liquid separation equipment, drying equipment and a reaction heating device are eliminated, a sodium diacetate crystal one-step synthesis method is realized, process is simple and safe, energy is saved, production cost can be greatly reduced, yield of the product reaches up to more than 97%, product quality is easy to control, and the standard of FAO/WHO (Food and Agriculture Organization/World Health Organization) is met.
Owner:广饶县多利多新型材料有限公司

Sialic acid-carboxylic acid compound conjugate and preparation method thereof

The invention discloses a sialic acid-carboxylic acid compound conjugate and a preparation method thereof. The sialic acid-carboxylic acid compound conjugate is obtained by subjecting a sialic acid glucocinolate donor and a carboxylic acid compound to direct glycosylation reaction and is a compound with carboxylate at an anomeric position of sialic acid. The preparation method includes: (1), sequentially adding the sialic acid glucocinolate donor, a newly-activated molecular sieve and the carboxylic acid compound into a reaction container, adding redistilled dichloromethane for dissolution, and stirring for 15min at 25 DEG C under argon shield; (2), sequentially adding an activation system, boron trifluoride diethyl ether and iodosuccinimide quickly, and stirring for reaction at 25 DEG C for 5-10min; (3), filtering a reaction system, using an organic solvent to dilute, using a saturated sodium thiosulfate solution to wash an organic phase once, using the organic solvent to extract an aqueous phase for three times, merging the organic phase, using anhydrous sodium sulfate to dry, filtering, spin-drying, and using a silica gel column for chromatography and elution to obtain the sialic acid-carboxylic acid compound conjugate. By the preparation method, the sialic acid-carboxylic acid compound conjugate which is efficient can be provided to benefit society.
Owner:EAST CHINA UNIV OF SCI & TECH

A kind of fluorine-modified titanium aluminum phosphate molecular sieve f-tapo-5 and preparation method thereof

The invention provides a fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 and a preparation method thereof. The preparation method comprises the steps that 1, a phosphorus source, an aluminum source, a fluorine-containing titanium source, a templating agent and deionized water are mixed to be uniform according to the molar ratio of 0.96:1.5:(0.04-0.3):0.8:50 under vigorous stirring, stirring is conducted for 20-40 min at the temperature of 25-35 DEG C, and molecular sieve precursor sol is obtained; the precursor sol is converted into a hydrothermal reactor with a PTFE lining, crystallization treatment is conducted for 18-30 h at the temperature of 160-185 DEG C, after crystallization is finished, solids are separated out through centrifugation, the solids are washed with distilled water and then dried by 10-15 h at the temperature of 90-110 DEG C, and fluorine-containing titanium and aluminum phosphate molecular sieve raw powder is obtained; 2, the molecular sieve raw powder obtained in the step 1 is put into a tubular furnace constant temperature area, calcination is conducted for 4-8 h at the temperature of 500-650 DEG C in an oxygen atmosphere to remove the templating agent, and the fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 is obtained. The fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 obtained through the method has high Lewis acid and surface hydrophobicity and can be applied in a catalytic cyclohexanone ammoximation reaction.
Owner:SHANXI UNIV

Sialic acid-carboxylic acid compound conjugate and preparation method thereof

The invention discloses a sialic acid-carboxylic acid compound conjugate and a preparation method thereof. The sialic acid-carboxylic acid compound conjugate is obtained by subjecting a sialic acid glucocinolate donor and a carboxylic acid compound to direct glycosylation reaction and is a compound with carboxylate at an anomeric position of sialic acid. The preparation method includes: (1), sequentially adding the sialic acid glucocinolate donor, a newly-activated molecular sieve and the carboxylic acid compound into a reaction container, adding redistilled dichloromethane for dissolution, and stirring for 15min at 25 DEG C under argon shield; (2), sequentially adding an activation system, boron trifluoride diethyl ether and iodosuccinimide quickly, and stirring for reaction at 25 DEG C for 5-10min; (3), filtering a reaction system, using an organic solvent to dilute, using a saturated sodium thiosulfate solution to wash an organic phase once, using the organic solvent to extract an aqueous phase for three times, merging the organic phase, using anhydrous sodium sulfate to dry, filtering, spin-drying, and using a silica gel column for chromatography and elution to obtain the sialic acid-carboxylic acid compound conjugate. By the preparation method, the sialic acid-carboxylic acid compound conjugate which is efficient can be provided to benefit society.
Owner:EAST CHINA UNIV OF SCI & TECH

Method for synthesizing sodium diacetate crystal in one step

The invention relates to a method for synthesizing a preservative and antistaling agent, and in particular relates to a method for synthesizing a sodium diacetate crystal in one step. The following raw materials are adopted in percent by weight: 70.4-72.4% of glacial acetic acid, 10.8-12.0% of ionic membrane method caustic soda flake and 16.5-18.6% of anhydrous sodium carbonate. The synthesis steps are as follows: (1) mixing the ionic membrane method caustic soda flake with the anhydrous sodium carbonate, slowly adding the glacial acetic acid and then naturally heating, controlling total reaction time to be 30-50 minutes, and controlling maximum reaction temperature to be 65-85 DEG C; and (2) cooling the temperature below 50-60 DEG C after the reaction is completed, and discharging. By applying the method provided by the invention, solid-liquid separation equipment, drying equipment and a reaction heating device are eliminated, a sodium diacetate crystal one-step synthesis method is realized, process is simple and safe, energy is saved, production cost can be greatly reduced, yield of the product reaches up to more than 97%, product quality is easy to control, and the standard of FAO / WHO (Food and Agriculture Organization / World Health Organization) is met.
Owner:广饶县多利多新型材料有限公司

Universal preparation method of nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide

The invention relates to a universal preparation method of a nitrogen and phosphorus co-doped carbon-loaded transition metal phosphide. The method comprises the following steps: taking melamine polyphosphate as a carbon source, a nitrogen source and a phosphorus source, compounding the melamine polyphosphate with a transition metal raw material, and calcining at high temperature to obtain the nitrogen-phosphorus co-doped carbon-loaded transition metal phosphide. In the preparation method provided by the invention, melamine polyphosphate is pyrolyzed to obtain a nitrogen-phosphorus co-doped carbon material while a transition metal raw material is converted into a corresponding phosphide, so that one-step synthesis of the carbon-loaded transition metal phosphide is realized. Compared with the prior art, the preparation method has the advantages that complicated precursor preparation and phosphating treatment processes are not needed, and the preparation process of the carbon material loaded transition metal phosphide is remarkably simplified. The method provided by the invention is low in raw material cost, high in universality and simple to operate, can realize large-scale preparation of the carbon-loaded transition metal phosphide, and has important application value.
Owner:NORTHWESTERN POLYTECHNICAL UNIV
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