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31results about How to "Avoid disproportionation reactions" patented technology

Method for preparing 3-methoxy-4-hydroxy mandelic acid

A method for preparing 3-methoxy-4-hydroxy mandelic acid adopts guaiacol and glyoxylic acid as raw materials, and comprises the following steps: slowly adding a 30 wt% sodium hydroxide solution into the glyoxylic acid solution with stirring, allowing the mixed solution to react at a reaction temperature of 0-50 DEG C and a pH value of 1-7 to obtain a sodium glyoxylate solution; adding the guaiacol into water with stirring and under the protection of nitrogen gas, slowly adding the 30 wt% sodium hydroxide solution, allowing the mixed solution to react at a reaction temperature of 0-50 DEG C and a pH value of 11-12 to obtain guaiacol sodium; slowly and dropwisely adding the sodium glyoxylate solution into the guaiacol sodium solution with stirring and under the protection of nitrogen gas, with the mole ratio of the sodium glyoxylate and the guaiacol sodium being 1:1.2-2, allowing the mixed solution to react at a reaction temperature of 0-20 DEG C and a pH value of 11-12, 30-90 min afterthe dropwise addition, stirring the mixed solution for 1-3 hours, stopping the reaction at the reaction temperature for 24-36 hours, then acidifying the reaction solution by a 50 wt% sulfuric acid solution to control the pH value to be 4-5. The yield of the reaction is above 95 wt%.
Owner:PETROCHINA CO LTD

High-cycling-capacity ZrCo-based hydrogen isotope storage alloy as well as preparation and application thereof

The invention discloses a high-cycling-capacity ZrCo-based hydrogen isotope storage alloy, preparation of the alloy and application of the alloy to storage, supply and recovery of hydrogen isotopes. The chemical general formula of the high-cycling-capacity ZrCo-based hydrogen isotope storage alloy is Zr(1-x)NbxCo(1-y)Niy, wherein x is larger than 0 but smaller than or equal to 0.5, and y is largerthan 0 but smaller than or equal to 0.5. A preparation method of the alloy includes the following steps that (1) Zr, Nb, Co and Ni elementary substance raw materials are mixed according to the proportion in the chemical general formula and then are placed into a magnetic suspension induction smelting furnace; and (2) smelting, cooling and solidifying are performed under the protection of an argonatmosphere to prepare the high-cycling-capacity ZrCo-based hydrogen isotope storage alloy. The method is simple in step and high in safety, the prepared hydrogen isotope storage alloy is not requiredto be subjected to vacuum operation in the circulation process, the method is still applicable in complex hydrogen isotope scenes, and the method has long-term significance in promoting application and popularization of the ZrCo-based alloy in the field of hydrogen isotope storage.
Owner:ZHEJIANG UNIV

Novel process for reducing consumption of formaldehyde in production of neopentyl glycol

The invention provides a novel process for reducing the consumption of formaldehyde in the production of neopentyl glycol, comprising the following steps of: adding recycled diluted formaldehyde into a condensation kettle; starting agitating, and adding formaldehyde with the concentration of 37% to enable formaldehyde total amount in the condensation kettle to be 24 Kmol; adding 8 Kmol of isobutyraldehyde with the concentration of 97-98% and adding 4.12 Kmol of an NaOH solution with the concentration of 30%, which is one half of the total amount, at a room temperature; controlling the temperature in the kettle to 30-35 DEG C, the pH to 9-11 and the time to 2 hours in a process of adding alkali; then, improving the pH to 12-13 and adding the residual half of 4.12 Kmol of the NaOH solution with the concentration of 30% at a constant speed; controlling the temperature of the system to 40-45 DEG C and controlling time to 2 hours; raising the temperature to 45-50 DEG C and keeping for 3-4 hours; adding formic acid to neutralize a condensed solution until the pH is 7-8; recycling superfluous formaldehyde in a condensation reaction by pressurized distilling; and dehydrating an aldehyde removing solution from an aldehyde removing tower and carrying out pre-fractionation, rectification and flaking to obtain a neopentyl glycol finished product. According to the novel process provided by the invention, the utilization rate of formaldehyde in a production process of neopentyl glycol is improved, the quality of neopentyl glycol is improved and the consumption of sodium hydroxide is reduced.
Owner:大庆三聚能源净化有限公司

Method for preparing trifluoromethyl-1,2,2-trifluoro-1,2-dichloroethyl ether

The invention discloses a method for preparing trifluoromethyl-1,2,2-trifluoro-1,2-dichloroethyl ether, which comprises the following steps of: 1) continuously introducing gaseous fluoroxy trifluoromethane thinned by using nitrogen from the lower part of a reaction tower, wherein the content of the fluoroxy trifluoromethane is 5 to 50 volume percent; 2) introducing quantitative liquid 1,2-difluoro-1,2-dichloroethylene from the upper part of the reaction tower to countercurrent contact and react with the gaseous fluoroxy trifluoromethane, controlling the reaction temperature to be between 110 DEG C below zero and 5 DEG C below zero through a heat exchange device, generating the trifluoromethyl-1,2,2-trifluoro-1,2-dichloroethyl ether, and discharging the un-reacted incoagulable gas from the top of the reaction tower for neutralization treatment; and 3) when the tail gas discharged from the top of the reaction tower contains the fluoroxy trifluoromethane or the 1,2-difluoro-1,2-dichloroethylene content of the sampled analysis liquid phase is less than 1 volume percent by detection, terminating the reaction, and stopping introducing the gaseous fluoroxy trifluoromethane. The method has the advantages of low metering requirement, convenience of operation, long service life of equipment and high yield.
Owner:ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD

Preparation method of stiripentol

The invention relates to a method for preparing stiripentol disclosed as a chemical structural formula II from 4-(2-methylallyl)-1,2-phenyldiphenol disclosed as a chemical structural formula I, which comprises the following steps: etherifying 4-(2-methylallyl)-1,2-phenyldiphenol, isomerizing, and carrying out oxidation reaction, condensation reaction and reduction reaction to obtain the stiripentol. The stiripentol is a new drug for treating epilepsy.
Owner:HUNAN UNIV

Preparation method of m-phenoxy benzaldehyde

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of m-phenoxy benzaldehyde. According to the preparation method provided by the invention, m-hydroxybenzaldehyde is salified by phenolic hydroxyl under an alkaline anhydrous condition, and then is subjected to substitution reaction with halobenzene to obtain m-phenoxy benzaldehyde, so that disproportionation reaction of aldehyde groups during reaction in an alkaline aqueous solution is avoided, the utilization rate of raw materials is increased, and side reactions are reduced. The purification of the m-phenoxybenzaldehyde product and the improvement of the yield are facilitated. The test result of the embodiment shows that the yield of m-phenoxybenzaldehyde obtained by the preparation method provided by the invention is 79.9-81%, and the yield is high; the gas phase content of m-phenoxy benzaldehyde is 98.9%-99.3%, and the purity of m-phenoxy benzaldehyde is high.
Owner:锦州三丰科技有限公司

A New Process for Reducing Formaldehyde Consumption in Neopentyl Glycol Production

The invention provides a novel process for reducing the consumption of formaldehyde in the production of neopentyl glycol, comprising the following steps of: adding recycled diluted formaldehyde into a condensation kettle; starting agitating, and adding formaldehyde with the concentration of 37% to enable formaldehyde total amount in the condensation kettle to be 24 Kmol; adding 8 Kmol of isobutyraldehyde with the concentration of 97-98% and adding 4.12 Kmol of an NaOH solution with the concentration of 30%, which is one half of the total amount, at a room temperature; controlling the temperature in the kettle to 30-35 DEG C, the pH to 9-11 and the time to 2 hours in a process of adding alkali; then, improving the pH to 12-13 and adding the residual half of 4.12 Kmol of the NaOH solution with the concentration of 30% at a constant speed; controlling the temperature of the system to 40-45 DEG C and controlling time to 2 hours; raising the temperature to 45-50 DEG C and keeping for 3-4 hours; adding formic acid to neutralize a condensed solution until the pH is 7-8; recycling superfluous formaldehyde in a condensation reaction by pressurized distilling; and dehydrating an aldehyde removing solution from an aldehyde removing tower and carrying out pre-fractionation, rectification and flaking to obtain a neopentyl glycol finished product. According to the novel process provided by the invention, the utilization rate of formaldehyde in a production process of neopentyl glycol is improved, the quality of neopentyl glycol is improved and the consumption of sodium hydroxide is reduced.
Owner:大庆三聚能源净化有限公司

Battery cathode material and high temperature solid phase synthesis method

The invention discloses a battery cathode material of which the chemical formula is LiLa0.1 Co0.1 Mn1.8 O4. The spinel structure of the battery cathode material LiLa0.1 Co0.1 Mn1.8 O4 provided by the invention has low probability of being damaged after the mixing of Co ions, the electrical conductivity of a synthetic material is enhanced, a diffusion coefficient is increased to 2.4*10<-12> - 1.4*10<-11> m<2> / s from 9.2*10<-14> - 2.6*10<-12> m<2> / s, so as to be convenient for lithium-ion taking off and embedding, after the addition of LA ions, part of Mn ions can be replaced, in a later period of slight discharging, the concentration of Mn<+3> ions is lower, disproportionation reaction is prevented, dendritic crystal forming on the surface of a positive pole is avoided, a diaphragm is pierced, and the safety performance is improved. The synthetic material adopts a spinel structure. The synthetic material is more superior in cycle performance.
Owner:GUANGXI UNIVERSITY OF TECHNOLOGY

Method for preparing 3-methoxy-4-hydroxy mandelic acid

A method for preparing 3-methoxy-4-hydroxy mandelic acid adopts guaiacol and glyoxylic acid as raw materials, and comprises the following steps: slowly adding a 30 wt% sodium hydroxide solution into the glyoxylic acid solution with stirring, allowing the mixed solution to react at a reaction temperature of 0-50 DEG C and a pH value of 1-7 to obtain a sodium glyoxylate solution; adding the guaiacol into water with stirring and under the protection of nitrogen gas, slowly adding the 30 wt% sodium hydroxide solution, allowing the mixed solution to react at a reaction temperature of 0-50 DEG C and a pH value of 11-12 to obtain guaiacol sodium; slowly and dropwisely adding the sodium glyoxylate solution into the guaiacol sodium solution with stirring and under the protection of nitrogen gas, with the mole ratio of the sodium glyoxylate and the guaiacol sodium being 1:1.2-2, allowing the mixed solution to react at a reaction temperature of 0-20 DEG C and a pH value of 11-12, 30-90 min after the dropwise addition, stirring the mixed solution for 1-3 hours, stopping the reaction at the reaction temperature for 24-36 hours, then acidifying the reaction solution by a 50 wt% sulfuric acid solution to control the pH value to be 4-5. The yield of the reaction is above 95 wt%.
Owner:PETROCHINA CO LTD
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