40results about How to "Uniform crystal" patented technology

The present invention relates to a preparation method and applications of a mesoporous metal organic complex base composite material, and belongs to the technical fields of material science, nanometer materials, chemical industry, catalysis and the like. According to the present invention, copper nitrate, a cyanuric chloride tricarboxylic acid H3L and tetraethyl orthosilicate are subjected to one-step ultrasound to prepare Cu-MOF@SiO2, the Cu-MOF@SiO2 is impregnated in a silver nitrate solution, and ultraviolet irradiation is adopted to reduce Ag<+> to prepare the magnetic metal organic polymer-supported noble metal catalyst with the nanometer Ag anchored on the surface, wherein the catalyst is the Cu-MOF@SiO2@Ag. The catalysis has the excellent performance of catalytic reduction of unsaturated organic compounds, and has good application prospects in heterogeneous catalytic reduction reactions.

The invention relates to a preparation method of acetylisovaleryltylosin tartrate. The method comprises the following steps: adjusting the pH of acetylisovaleryltylosin fermentation liquor to 1-1.5 by using oxalic acid, and standing for 20-30 minutes; adjusting the pH of acetylisovaleryltylosin back to 4.5-5.5 by using 10-15 percent liquid alkali; standing for 20-30 minutes once again; performing plate frame filtering, diluting, decolorizing, nano-filtering, crystalizing, water washing, salifying and spray drying on the fermentation liquor to obtain the acetylisovaleryltylosin tartrate. By adopting the preparation method, the conventional crystallizing process is eliminated, the yield of acetylisovaleryltylosin tartrate is increased by virtue of extracting, crystallizing and synthesizing processes, the cost is lowered, and the product quality is improved. The method is suitable for industrial production.

The invention provides a preparation process of high-purity oxymatrine. The method comprises the following steps of: firstly, heating purified water in a water bath to a certain temperature; adding hydrogen peroxide and slowly adding oxymatrine to react at the certain temperature until the hydrogen peroxide is completely consumed; then, extracting residual less oxymatrine; decompressing and concentrating a reaction solution and adding an alcohols substance into the concentrated solution to be dissolved; adding a de-coloring agent for decoloring and filtering; continually decompressing and concentrating; adding an acetones substance to crystallize; and re-crystallizing to obtain the oxymatrine. The process method disclosed by the invention has the advantages of simplicity and practical applicability, low cost and high yield; and more importantly, the purity is high and the preparation process is suitable for industrial production.

The invention relates to a method of producing wet-process phosphoric acid and alpha-hemihydrate phosphogypsum from middle grade phosphorus ore and is an energy-saving and low-consumption wet-processphosphoric acid producing method. The method includes: decomposition reaction, solid-liquid separation, hemihydrates conversion reaction, and filtration and washing, wherein the technical parameters in the steps are controlled to finally produce a high-concentration final product of phosphoric acid and high-quality alpha-hemihydrate phosphogypsum; the final product of phosphoric acid is 35-42 wt%in concentration; the alpha-hemihydrate phosphogypsum is 13-15% in omega(H2O), is not more than 0.25% in omega(insoluble P2O5) and is not more than 0.1% in omega(soluble P2O5). Through the classification technology, zero emission of the byproduct, phosphogypsum, is achieved.

The invention discloses a high-temperature phosphating process for a nipple threading connector of an oil drill collar, which comprises three steps of surface treatment before phosphating, high-temperature phosphating and surface treatment after phosphating. The surface treatment before phosphating is oil removal treatment. The treatment of high-temperature phosphating comprises the steps that: firstly, the phosphating solution in an open container is heated up to between 85 and 95 DEG C; then the nipple threading connector of the drill collar and the circular head are wholly immersed in the phosphating solution for 12 to 15 minutes; and then the connecter is taken out from the phosphating solution, a temperature of the phosphated surface is reduced and the surface is dried naturally. At last, the surface treatment after phosphating comprises the steps that: the dried phosphated surface is painted with an antirust oil layer and a thread-protecting oil layer. The invention has simple and convenient procedures, easy operation and good quality of the phosphated surface, thereby effectively improving antirust capability and wear resistance of the drill collar and reducing the phenomenon of gear adhesion during meshing. The process is particularly suitable for phosphating the end part of long rod components.

The invention relates to a method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography and belongs to the field of natural medicine extraction. Radix glycyrrhizae is smashed and then undergoes extraction by ammonia and alcohol, continuous chromatographic adsorption, ethanol eluting 1, combined spin, polyamide adsorption, ethanol eluting 2 and rotary drying to obtain glycyrrhiza flavonoids; NaOH aqueous solution elution, pH adjustment, spin drying, filtering drying and recrystallization are performed to obtain glycyrrhizic acid. A production device adopted for the method is a continuous chromatographic separation system which is controlled under a logic control valve and is composed of 12 chromatographic columns, and the chromatographic column in the system is divided into four areas which are an adsorption area, a flavonoid analysis area, a glycyrrhizic acid analysis area and a resin regeneration area. The production process is simple to operate, the glycyrrhizic acid and glycyrrhiza flavonoids can be extracted simultaneously, waste of the glycyrrhiza flavonoids in conventional industrial production is reduced, the acid liquor pollution is avoided, so that the yield and purity of the obtained glycyrrhizic acid and glycyrrhiza flavonoids are high, and the method can be suitable for large-scale production.

The invention relates to a method for producing wet-process phosphoric acid and alpha hemihydrate phosphogypsum by using medium-grade phosphorite. The method is an energy-saving low-consumption wet-process phosphoric acid production method. The method comprises the steps of decomposition reaction, solid-liquid separation, hemihydrate conversion reaction, and filtration and washing, and the high-concentration finished product phosphoric acid and the high-quality alpha hemihydrate phosphogypsum are obtained by controlling process parameters of the steps. The concentration of the obtained finished product phosphoric acid reaches 35-42 wt.%, omega(H2O) of the alpha hemihydrate phosphogypsum is in a range of 13-15% and omega(insoluble P2O5) is less than or equal to 0.1%. Through a grading technology, zero emission of the byproduct phosphogypsum is realized.

The invention discloses a method for improving corrosion resistance of the surface of magnesium alloy on the basis of micro-arc oxidation and laser remelting. Firstly, after micro-arc oxidation treatment is conducted on the surface of the magnesium alloy, a layer of ceramic film is obtained, the film layer is prefilled with a thin layer of graphene oxide particles through ultrasonic oscillating, then microcracks and holes of the ceramic film are filled with molten graphene oxide particles effectively through laser remelting technology, and thus corrosion resistance of the surface of the magnesium alloy is improved greatly. The method is environmentally friendly in process and high in repeatability, and a novel way is developed for improving the corrosion resistance of the surface of the magnesium alloy.

The invention relates to rare-earth type lithium iron phosphate serving as the cathode material of a lithium secondary battery and a preparation method thereof. The rare-earth type lithium iron phosphate contains 100 mole fractions of lithium iron phosphate, 3.9-7.8 mole fractions of rare-earth alloy and 1.1-2.2 mole fractions of cellulose acetate. The preparation method of the rare-earth type lithium iron phosphate comprises the following steps of: putting an iron source compound, a lithium source compound, a phosphorus source compound and a rare-earth material into a powder mixer for powder mixing; in the powder mixing process, gradually spraying cellulose acetate dissolved in acetone to the mixed powder so that cellulose acetate is uniformly stuck on the mixture particles of the four materials, and drying; pre-sintering the dried mixture particles in an atmosphere furnace under inert gas protection; and carrying out heat preservation on the pre-sintered powder in the atmosphere furnace under inert gas protection to obtain the rare-earth type lithium iron phosphate. The rare-earth type lithium iron phosphate provided by the invention has the advantages of good conductive performance, relatively short preparation time and the like.

The invention discloses a riboflavin sodium phosphate compound. The riboflavin sodium phosphate is measured by using powder X-ray diffractometry, and characteristic diffraction peaks are displayed at positions of 11.87 degrees, 12.56 degrees, 13.90 degrees, 16.22 degrees, 16.98 degrees, 18.13 degrees, 19.02 degrees, 20.92 degrees, 21.54 degrees, 24.17 degrees, 24.89 degrees, 25.38 degrees, 26.78 degrees and 28.45 degrees in an X-ray powder diffraction pattern expressed by a 2theta diffraction angle. The invention also discloses a method for preparing the riboflavin sodium phosphate compound as well as freeze-dried powder injection, hydro-acupuncture or sterile powder injection prepared by utilizing the riboflavin sodium phosphate compound. The riboflavin sodium phosphate compound prepared by the invention has the advantages of stable property, oxidation difficulty and high water solubility.

The invention discloses a preparation method of a (2S,3S)-2-hydroxy-4-phenylbutane derivative. The preparation method comprises the steps of enabling (3S)-3-(tert-Butoxycarbonyl)amino-1-chloro-4-phenyl-2-butanone, carbonyl reductase and excess isopropyl alcohol to be subjected to a biological enzyme catalytic reaction to obtain transformation liquid, and then performing continuous concentrating and crystallizing to obtain target product crystals. The carbonyl reductase has the characteristic of tolerance to high-concentration isopropyl alcohol through directional mutation, so as to realize thepurpose of solubilization of a substrate with the excessive isopropyl alcohol, the addition quantity of the substrate is further increased, the conversion rate is increased, the yield of products isnot lower than 95%, and the chirality purity is not lower than 99.95%. Through continuous concentrating and crystallizing on the transformation liquid, the crystalinity of the obtained products is 95%or above, the crystals are uniform, the purity of impurities is not less than 99.95%, and the content is not lower than 99%.

The invention discloses a production process for producing microcrystal alpha-alumina through microwave calcination, belonging to the technical field of production processes for calcined alumina. The production process specifically comprises the following steps: (1) adding a composite mineralizer into an alumina raw material, and conducting uniform mixing to obtain a mixture; (2) putting the mixture into a ball mill for ball milling so as to obtain a ground material; (3) adding a wave-absorbing agent with a certain proportion into the ground material, conducting uniform stirring, and then performing extruding by using a press machine to prepare a green body of alumina; (4) drying the green body of aluminato adjust a water content in the green body of alumina; (5) feeding the dried green body of alumina into a microwave kiln, heating the microwave kiln to a set temperature, and conducting calcining for a certain time to obtain alpha-alumina clinker; and (6) crushing the alpha-alumina clinker to obtain the microcrystal alpha-alumina. According to the invention, product quality is stable, product yield is higher than product yield of a traditional kiln production mode, energy consumption during alpha-alumina preparation can be greatly reduced, and zero emission of harmful gas is achieved.

The invention belongs to the field of medical intermediate preparation, and especially relates to a method used for purifying methyl 1, 2, 4-triazole-3-carboxylate coarse product. The wet methyl 1, 2, 4-triazole-3-carboxylate coarse product prepared by acylation, cyclization, esterification, diazotization and nitrogen-releasing suction filtration is used as a raw material. The method used for purifying the methyl 1, 2, 4-triazole-3-carboxylate coarse product comprises following steps: the wet coarse product is re-dissolved in methanol solvent; active carbon is added for decoloration; temperature reduction is controlled for recrystallization; and wet crystals obtained after recrystallization is dried so as to obtain finished products. The steps of the method are simple; the coarse product is re-dissolved, active carbon is used for adsorption, and temperature is controlled for recrystallization, so that the finished products with high purity and uniform crystals are obtained, and the finished products are of significant benefits on improvement of the quality of later produced medicine products, and are suitable for wide popularization and application.

The invention discloses an anti-crusting wear-resistant castable for a limekiln. The anti-crusting wear-resistant castable comprises base materials, auxiliary materials and an additive, wherein the base materials are mainly composed of, by weight, 10 to 15 parts of Cr2AlC, 5 to 8 parts of Ti2AlC, 20 to 25 parts of fused magnesium-zirconium spinel, 25 to 28 parts of sintered fused alumina zirconia, 20 to 30 parts of fused mullite, 5 to 10 parts of fused magnesia-calcium clinker and 3 to 8 parts of fused calcium aluminate cement. The castable provided by the invention is especially applicable to the limekiln, has uniform interior structure and uniform crystals, maintains integral performance, presents enhanced resistance to erosion and scouring and, more importantly, can effectively prevent crusting, resolve blockage and ensure ventilation and smoothness of a system in the kiln.

The invention discloses a preparation method of L-carnitine tartrate in the field of compound preparation. According to the method, most fishy smell in an L-carnitine product can be removed in presence of an anhydrous organic solvent and a deodorant, the reaction method and the reaction condition are controlled in the process of preparation of L-carnitine tartrate through tartaric acid salifying,and the L-carnitine tartrate without the fishy smell is obtained. Compared with the prior art, the method has the advantages that the obtained product has good quality and no fishy smell, the reactionprocess is convenient to operate and high safety, the method is suitable for industrial production and the like and can be widely applied to the field of preparation of the L-carnitine tartrate.

The invention provides a making method of a cream juice honey product. The making method comprises the following steps: firstly, adding juice into honey and uniformly stirring to obtain a honey and juice mixture, then adding glucose into the honey and juice mixture to obtain a second honey and juice mixture, uniformly stirring the second honey and juice mixture, filtering the mixture through a 80-mesh sieve so as to obtain a filtrate, carrying out vacuum heating concentration on the filtrate until water content is not more than 19 wt%, rapidly putting the product into an environment of 10-15 DEG C until the product is completely crystallized so as to obtain the cream juice honey product. According to the making method of the cream juice honey product, honey, juice and glucose are used as raw materials to form the cream product. Thus, types of existing honey products are enriched. Cream products with juice and honey mutually blended are convenient to carry and eat. By adding glucose into the honey and juice mixture, crystallization of the mixture is promoted. Meanwhile, as glucose is an inherent ingredient in honey, addition of glucose will not influence mouthfeel of the honey product.

The invention relates to an aqueous solution crystallization method of D-pantolactone, which comprises the following steps: by using an inorganic salt aqueous solution containing 15-23% of D-pantolactone as a raw material, concentrating until the concentration of D-pantolactone is 28-35%, cooling to 0-5 DEG C at the speed of 2-8 DEG C / h, and carrying out heat preservation crystallization. According to the method provided by the invention, crystallization is realized by adjusting the concentration of D-panolactone in the inorganic salt aqueous solution and controlling the cooling speed, and themethod is preferably suitable for preparing a mixed solution of D-panolactone by taking D-pantoic acid as a raw material and adopting a lactonization process. The method has the characteristics of simple steps, easiness in operation control, higher quality and the like, and is an effective method for crystallizing and purifying D-panolactone .

The present invention provides a process for preparing cytisine from thermopsis lanceolata glasses or seeds. The process comprises: crushing thermopsis lanceolata glasses into coarse powder (1-3 cm) or breaking thermopsis lanceolata seeds, weighing a certain amount of thermopsis lanceolata glass coarse powder or broken thermopsis lanceolata seeds, adding an alkaline solution to moisten for 6-8 h, adding chloroform to carry out reflux extraction, mixing the extraction solutions, carrying out reduced pressure concentration to recover the chloroform, adding ethanol to dissolve, adopting a decoloration agent to carry out decoloration, filtering, carrying out reduced pressure recovery of ethanol, adding acetone to carry out crystallization to obtain a cytisine crude product, and adding petroleum ether to carry out re-crystallization to obtain the cytisine fine product. The process method has characteristics of simpleness, practicality, low cost and high purity, and is suitable for industrial production.

The invention provides a preparation method high-purity high-yield oxysophocarpine. The method comprises the following steps: firstly heating purified water in a water bath to a certain temperature, adding hydrogen peroxide, slowly adding sophocarpine, reacting at a certain temperature till hydrogen peroxide is completely consumed, then extracting the residual small amount of sophocarpine; performing reduced pressure concentration of the reaction solution, adding alcohol substances into the concentrate for dissolution, adding alumina for decoloring, performing suction filtration; continuing to perform reduced pressure concentration, adding ketone substances for crystallization, and performing recrystallization to obtain oxysophocarpine. The process method is simple and practical, low in cost, high in purity, high in yield, and suitable for industrial production.

The present invention relates to an aqueous solution crystallization method of D-pantolactone, which comprises the following steps: using an aqueous inorganic salt solution containing 15-23% D-pantolactone as a raw material, concentrating and making D-pantolactone in it When the concentration of the ester reaches 28-35%, the temperature is lowered to 0-5°C at a rate of 2-8°C / h, and the temperature is maintained for crystallization. The method provided by the invention realizes crystallization by adjusting the concentration of D-pantoic acid lactone in an aqueous solution of inorganic salt and controlling the cooling rate, and is preferably suitable for using D-pantoic acid as a raw material and adopting a lactonization process to prepare D ‑A mixed solution obtained from pantotolactone. The method has the characteristics of simple steps, easy operation and high quality, and is an effective method for the crystallization and purification of D-pantolactone.

The invention discloses a tundish for vacuum smelting furnace casting. The tundish comprises a blank body, a buffer bag and leaking holes, wherein the buffer bag is a hemispherical buffer bag and is arranged on the bottom surface of the blank body, the leaking holes are formed in the bottom surface of the blank body and are uniformly distributed around the buffer bag. When the tundish is used, the problems of water cooling ingot mold burnthrough, product coarse crystallization and the like can be effectively solved, the operation safety is improved, and the production cost is reduced.

The invention relates to a composite photoanode and a preparation method thereof. The preparation method comprises the following steps: firstly, preparing composite nanofibers by electrostatic spinning; then, preparing alpha-Fe2O3 nanocrystals with specific morphology in ammonia water by a hydrothermal method; adding GO in a hydrothermal process under alkaline conditions, so that the GO is compounded with the alpha-Fe2O3 nanocrystals to prepare alpha-Fe2O3 / RGO; and preparing pure Fe2O3 nanocrystals and alpha-Fe2O3 / RGO composite nanomaterials into a photoanode, wherein the photoelectric performance evaluation is completed by utilizing a light source electrochemical workstation; and the optimal proportion is found out by changing the doping amount of the alpha-Fe2O3 / RGO composite nanomaterials.

The invention provides a method for preparing high-purity high-yield oxysophoridine. The preparation method comprises the following steps of: heating purified water in an oxidation tank to a certain temperature in water bath; adding hydrogen peroxide; uniformly mixing by stirring; slowly adding sophoridine; stirring until the sophoridine is dissolved; after hydrogen peroxide is completely reacted at a certain temperature, extracting residual sophoridine by using benzene or ether to obtain a reacted solution; concentrating the reacted solution under reduced pressure to obtain a concentrated solution; adding alcohol to dissolve the concentrated solution; decoloring a solution by adding a decoloring agent; performing suction filtration on the decolored solution to obtain filtrate; concentrating the filtrate under reduced pressure; adding ketone substances and performing crystallization to obtain a coarse product of oxysophoridine; and performing re-crystallization to obtain purified oxysophoridine. The process method is simple and practical and is applied to industrialized production, the cost is low, the purity is high, and the product yield is high.

The invention discloses a preparation method of 18 alpha type diammonium glycyrrhizinate. Under a certain alkali concentration, 18 beta type diammonium glycyrrhizinate is converted into 18 alpha type diammonium glycyrrhizinate. The end point is judged according to a principle that under a certain chromatographic condition, the retention time of 18 beta type diammonium glycyrrhizinate and the retention time of 18 alpha type diammonium glycyrrhizinate are different, and high performance liquid chromatography (HPLC) is used to judge the end point. The obtained 18 alpha type diammonium glycyrrhizinate is added into stronger ammonia water, and after refinement, qualified diammonium salt can be obtained. Compared with the conventional technology, the reaction temperature is reduced by about 10 DEG C, the time is also shortened, thus the energy loss of industrial production can be largely reduced; at the same time, the service life of equipment is prolonged, and the cost is reduced. Furthermore, the high temperature of conventional technology will deepen the product color, and the post treatment becomes difficult. The prepared 18 alpha type diammonium glycyrrhizinate has the advantages of good color, high yield and high content. The preparation method is suitable for industrial massive production, the product color is good, the crystals are uniform, and the quality is good.

A method for preparing L-carnitine tartrate applied in the field of compound preparation, the method can remove most of the fishy smell in L-carnitine products in the presence of anhydrous organic solvent and deodorant, And the process of preparing L-carnitine tartrate by forming salt with tartaric acid controls the reaction method and reaction conditions to obtain L-carnitine tartrate without fishy smell. Compared with the prior art, the obtained product has the advantages of good quality, no fishy smell, simple and convenient operation of the reaction process, high safety, suitable for industrial production, etc., and will be widely used in the field of preparation of L-carnitine tartrate.

The invention discloses a diammonium glycyrrhizinate salt preparation method. According to the method, according to the special physical and chemical properties of glycyrrhizic acid, the diammonium glycyrrhizinate salt with characteristics of good color, good character, high content and meeting of the industry standard is produced by using an ammonium glycyrrhizinate salt as a raw material. Compared to the method in the prior art, the method of the present invention has significant advantages of novel process, simple operation, energy saving, environmental protection, strong practicality, mild reaction condition, high conversion rate, easy quality control, reduction of the use of other solvents, reduction of impurity introduction, good product color, simple operation process, low equipment and material cost, high treatment capacity, good product chrominance, good product yield, high content, excellent product color, uniform crystal and good quality, and is suitable for industrial production.

The invention relates to a method for simultaneously extracting and separating glycyrrhizic acid and glycyrrhiza flavonoids of glycyrrhiza based on continuous chromatography and belongs to the field of natural medicine extraction. Radix glycyrrhizae is smashed and then undergoes extraction by ammonia and alcohol, continuous chromatographic adsorption, ethanol eluting 1, combined spin, polyamide adsorption, ethanol eluting 2 and rotary drying to obtain glycyrrhiza flavonoids; NaOH aqueous solution elution, pH adjustment, spin drying, filtering drying and recrystallization are performed to obtain glycyrrhizic acid. A production device adopted for the method is a continuous chromatographic separation system which is controlled under a logic control valve and is composed of 12 chromatographic columns, and the chromatographic column in the system is divided into four areas which are an adsorption area, a flavonoid analysis area, a glycyrrhizic acid analysis area and a resin regeneration area. The production process is simple to operate, the glycyrrhizic acid and glycyrrhiza flavonoids can be extracted simultaneously, waste of the glycyrrhiza flavonoids in conventional industrial production is reduced, the acid liquor pollution is avoided, so that the yield and purity of the obtained glycyrrhizic acid and glycyrrhiza flavonoids are high, and the method can be suitable for large-scale production.

The invention relates to a forging and pressing method of aluminium alloy with good forging and pressing property. The aluminium alloy with good forging and pressing property is obtained by adopting the forming and pressing method; two-stage isothermal tempering is carried out in an aluminium alloy tempering stage; the forging temperature of the aluminium alloy material is 330-380 DEG C; after the forging is ended, the isothermal water quenching is carried out.