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50results about How to "High yield in one pot" patented technology

Synthetic method of nano aluminum-rich beta-zeolite

A method for synthesizing nano aluminum-rich beta-zeolite comprises the steps as follows: (1) an alumino silica gel which is formed by mixing an aluminum source and acid is evenly mixed with aluminum source particles, dried and crushed into alumino silica gel particles, wherein, the mol ratio of the aluminum source to the silicon source is 0.05-0.2; and (2) a template agent is added to the alumino silica gel particles obtained in the step (1) and evenly mixed to produce a reaction mixture which is crystallized at the temperature of 80-190 DEG C for 1-6 days, therefore a product is obtained through recovery. The mol ratios of the feeding ingredients of the reaction mixture are as follows: the mol ratio of the template agent to the silicon source equals 0.1-1.0, and that of water to the silicon source equals 2-12. The template agent is a mixture of a tetraethylammonium compound and a fluoride, or tetraethylammonium fluoride dihydrate. The method provided by the invention is characterized by high yield of a single kettle and low moisture of the synthesis system. The beta-zeolite synthesized by the method provided by the invention has high relative crystallinity, few lattice defects and good thermal stability, and the ratio between the silicon and aluminum of the synthesized beta-zeolite is 5-20, which is up to the nano crystal grain dimension.
Owner:CHINA PETROLEUM & CHEM CORP +1

Mordenite preparation method

A mordenite preparation method is characterized in that after being reacted with diluted hydrochloric acid according to molar ratio of HCl/Al203 ranging from 0.04 to0.05 and molar ratio of H2O/Al203 ranging from 70-75, pseudo-boehmite is added into silica gel powder according to silicon to aluminum molar ratio ranging from 11.0 to 12.5 to realize pulping, uniform mixing and drying, then mixture is added into liquor mixture added with crystallized mother liquor, sodium chloride and sodium hydroxide according to molar ratio of Na2O/SiO2 ranging from 0.25 to 0.30, molar ratio of H2O/Na2O rangingfrom 25.0 to 30.0 and molar ratio of Cl/Al203 ranging from 0.4 to 0.5 and is stirred for 1 hour to 8 hours, and then two sections of thermal crystallization are realized at the temperature of 120 DEGC for 8 hours to 14 hours and at the temperature of 200 DEG C for 36 hours to 72 hours; and mordenite with the grain size ranging from 10 micrometers to 20 micrometers, silicon to aluminum molar ratio ranging from 11.0 to12.0 and a pure MOR (mordenite) structure is prepared. Compared with a conventional product, the mordenite prepared by the method has the advantages that crystallinity is improved by 30%, Langmuir specific surface area is larger than or equal to 400 square meters per gram, the mordenite is extremely rich in acid site density, and activity is improved when the mordenite is used in catalyst. In addition, any organic additives are not added in a preparation process, yield of a single kettle is high, the mother liquor can be recycled, emission is reduced, and the mordenite preparation method belongs to clean, high-efficiency, safe and green preparation technology.
Owner:山东荣创催化新材料有限公司

Method for solid-phase synthesis of ZSM-5 molecular sieve by using silica fume

The invention discloses a method for synthesizing ZSM-5 molecular sieve in solid phase by using lignite, which belongs to the technical field of molecular sieve preparation; the invention uses industrial waste micro-silica powder, without any pretreatment, and directly mixes it with sodium silicate, template agent and alkali Sources were ground and mixed, and crystallized at 130-220°C for 1-48 hours. The reaction product was ground, dissolved, filtered, and dried to obtain ZSM-5 molecular sieve. The present invention uses micro-silicon powder that does not require any pretreatment as a silicon-aluminum source to replace Si and Al pure chemical reagents to synthesize molecular sieves, which not only reduces the synthesis cost of ZSM-5 molecular sieves, but also reduces environmental dust pollution caused by micro-silicon powder , It also realizes the high-value utilization of micro-silica fume. At the same time, the synthesis route only involves the mixing of initial raw materials without using any solvent, which avoids the waste caused by the use of a large amount of clean water resources and the pollution caused by a large amount of waste liquid containing organic plates. The synthesis process is simple, energy saving and emission reduction, There are huge industrial application prospects.
Owner:YUNNAN UNIV

Method for synthesizing ZSM-5 molecular sieve by using silica fume

The invention discloses a method for synthesizing a ZSM-5 molecular sieve by using silica fume, belonging to the technical field of molecular sieve preparation. The method comprises the following steps: directly and uniformly mixing the industrial waste silica fume with a template agent and ammonia water; transferring into a polytetrafluoroethylene-lined steel reaction kettle, and performing a crystallization reaction for certain time at certain temperature; washing the reaction product; performing suction filtration; and drying for 12h at 60 DEG C to obtain the ZSM-5 molecular sieve. In the invention, the silica fume without any pretreatment serves as all silicon sources aluminum sources and replaces the Si and Al chemical reagents such as sodium silicate, silica sol, fumed silica, white carbon black and aluminum sulfate to synthesize the molecular sieve; and thus, the synthesis cost of the ZSM-5 molecular sieve is lowered, the high-value utilization of the silica fume is realized, and environmental dust pollution caused by the silica fume is also reduced. Meanwhile, the synthesis path only involves the mixing with initial raw materials, the use of large quantity of solvents is avoided, the waste of water resources and the waste liquid pollution of organic plate agents are eliminated, the synthesis technology is simple, the energy is saved while the emission is reduced, and the method has a huge industrial application prospect.
Owner:YUNNAN UNIV

H[beta] molecular sieve preparing method capable of increasing silicon-aluminum ratio

The invention relates to an H[beta] molecular sieve preparing method capable of increasing the silicon-aluminum ratio. The preparing method comprises following steps: (1) mixing a silicon dioxide source, an aluminum oxide source, a sodium oxide source and water, wherein molar ratios of the raw materials are described as follows: SiO2/Al2O3=5-25, Na2O/SiO2=0.18-0.5 and H2O/SiO2=1-6, stirring the raw materials to generate initial gel and continuously stirring the gel until the gel is turned into dry gel, adding a [beta]-molecular sieve seed crystal, performing hydrothermal crystallization at 100-180 DEG C for 12-130 h, and filtering and washing a reaction product to obtain Na[beta] zeolite; and (2) adding water to the Na[beta] zeolite sample with pulping, adding an ammonium salt and an acid, performing a reaction at 20-110 DEG C for 0.5-24 h, filtering and washing a reaction product, and drying and roasting the reaction product to obtain an H[beta] molecular sieve. Because that the preparation process is free of organic template agents, a high-temperature roasting for removing the organic template agent is not required, so that the preparing method is reduced in cost effectively and is reduced in pollutant discharge. By means of the method in the invention, the high-quality H[beta] molecular sieve being 6-200 in the silicon-aluminum ratio can be synthesized with a low cost. The H[beta] molecular sieve can be used in conversion of hydrocarbons, and especially can be used as an excellent catalyst component in catalytic cracking, hydroisomerization and hydrocracking.
Owner:PETROCHINA CO LTD

Biurea production process through urea method

InactiveCN104788346AHigh yield in one potOrganic chemistryHydrazine dihydrochlorideCentrifugation
The invention discloses a biurea production process through a urea method. The process comprises the following steps: mixing a urea solution with sodium hypochlorite, performing reaction to generate a crude solution containing hydrazine hydrate, and removing sodium carbonate in the crude solution; adding 10-15% hydrochloric acid recovered in an ADC oxidation process into the crude solution without sodium carbonate to neutralize to enable the PH value to be 2-3, performing multi-effect evaporation and concentration to obtain a hydrazine dihydrochloride solution of which the concentration is 20-30%, conveying precipitated sodium chloride to a centrifuger to enable solid sodium chloride to be separated out, conveying the hydrazine dihydrochloride solution to a concentration kettle, adding solid urea to react to produce biurea, and performing centrifugation, washing and drying to obtain the biurea product. The biurea production process provided by the invention has the benefits that a rectification procedure in a conventional hydrazine hydrate production process through evaporation, rectification and concentration of a crude solution is eliminated, and a defect that multiple-effect evaporation cannot be realized in the conventional evaporation, rectification and concentration process as hydrazine hydrate is likely to decompose at high temperature is overcome, so that plenty of steam can be saved, and single kettle yield of the condensation kettle is greatly improved.
Owner:HANGZHOU HI TECH FINE CHEM

Organic-template-free [beta]-molecular sieve synthesizing method

The invention relates to an organic-template-free [beta]-molecular sieve synthesizing method which includes following steps: mixing a silicon dioxide source, an aluminum oxide source, a sodium oxide source and water, wherein molar ratios of the raw materials are described as follows: SiO2/Al2O3=5-25, Na2O/SiO2=0.18-0.5 and H2O/SiO2=1-7.6, stirring the raw materials to generate initial gel and continuously stirring the gel until the gel is turned into dry gel, adding a [beta]-molecular sieve seed crystal, and performing hydrothermal crystallization at 100-180 DEG C for 12-130 h to obtain the [beta]-molecular sieve, wherein the ratio of SiO2 to Al2O3 in the [beta]-molecular sieve seed crystal is 11-70 and the addition amount of the [beta]-molecular sieve seed crystal is 0.5-5% by mass of the silicon dioxide source. By means of the method, the high-quality [beta]-molecular sieve crystal can be directly synthesized. Because that the addition amount of the seed crystal is less and the synthetic temperature is low, the synthesizing method is effectively reduced in cost. Because that none organic template free is added, the [beta]-molecular sieve has unobstructed pore channels without roasting, thereby further reducing the energy consumption during the production process. Because that the added water is quite less in amount, the synthesizing method is increased in utilization rate of the silicon source and is greatly increased in yield of single kettle.
Owner:PETROCHINA CO LTD

Synthetic method of nano aluminum-rich beta-zeolite

A method for synthesizing nano aluminum-rich beta-zeolite comprises the steps as follows: (1) an alumino silica gel which is formed by mixing an aluminum source and acid is evenly mixed with aluminum source particles, dried and crushed into alumino silica gel particles, wherein, the mol ratio of the aluminum source to the silicon source is 0.05-0.2; and (2) a template agent is added to the alumino silica gel particles obtained in the step (1) and evenly mixed to produce a reaction mixture which is crystallized at the temperature of 80-190 DEG C for 1-6 days, therefore a product is obtained through recovery. The mol ratios of the feeding ingredients of the reaction mixture are as follows: the mol ratio of the template agent to the silicon source equals 0.1-1.0, and that of water to the silicon source equals 2-12. The template agent is a mixture of a tetraethylammonium compound and a fluoride, or tetraethylammonium fluoride dihydrate. The method provided by the invention is characterized by high yield of a single kettle and low moisture of the synthesis system. The beta-zeolite synthesized by the method provided by the invention has high relative crystallinity, few lattice defects and good thermal stability, and the ratio between the silicon and aluminum of the synthesized beta-zeolite is 5-20, which is up to the nano crystal grain dimension.
Owner:CHINA PETROLEUM & CHEM CORP +1

Method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction

The invention relates to a method for preparing fluorocarbon alkyl imidazonline through fixed bed catalytic reaction. The method comprises taking perfluoro-carboxylic acid and polyethylene-polyamine at a mole ratio of acid to amide being 1 to 1.02-1 to1.1; adding the polyethylene-polyamine into a preheater, heating the polyethylene-polyamine to 30-35 DEG C, adding the perfluoro-carboxylic acid under stirring, increasing the temperature to 110-150 DEG C and performing heat preservation for 30-40 minutes; circulating preheated liquid through a fixed bed feeding pump and a fixed bed reflux pump at a reaction temperature of 150-160 DEG C; providing a vacuum degree of 0-0.03 MPa for a fixed bed, pumping out produced water, and after 4-6 hours' reaction, testing whether the content of a product is greater than 96% through the ultraviolet spectrophotometry, if so, determining that the product is qualified, wherein the obtained product is N-aminoethyl (or diethyltoluenediamine)-fluorocarbon alkyl imidazonline. The method for preparing the fluorocarbon alkyl imidazonline through fixed bed catalytic reaction has the advantages of being simple in process, free from solvent, stable in operation and control, short in reaction time, high in single-reactor yield and purity, low in three-waste pollution, environmentally friendly and easy to industrialize.
Owner:SHAANXI YANCHANG PETROLEUM GRP
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