30results about How to "High purity product" patented technology

A vertical and a horizontal vacuum sublimation apparatus with high efficiency and processes thereof are provided, especially for the materials having high melting point and low vapor pressure. The vertical sublimation purification apparatus comprises a sublimation channel body, a material rack, a heating evaporation device, a condensation device, an incubating device and a product scratching device. The horizontal sublimation purification apparatus comprises a sublimation channel body, a material carrier, a heating evaporation device and two end pipes. The apparatuses of the present invention can be applied on high purity chemicals from mass production, and are capable of sublimating and purifying OLED illumination layer materials including ALq₃, NPB and CuPc, which have high melting temperature and low vapor pressure.

Provided is a production method for an iodine compound in which iodine is reacted with a substrate in the presence of a porous material having a pore diameter of 500 nm or less or in the presence of the above porous material and an oxidizing agent and a production process for high purity 5-iodo-2-methylbenzoic acid comprising an iodination reaction step carried out by the above-mentioned, a crystal precipitation and separation step in which a product is precipitated by adding water or cooling and then separated and a purification step in which crystal separated is recrystallized using an organic solvent. According to the production method for an iodine compound described above, iodine can be introduced into various substrates at a high selectivity. Since expensive metals and specific reagents do not have to be used, it can readily be carried out in an industrially scale, and the product having a high purity can be obtained. Further, the process comprising the iodination reaction, separation and purification steps described above makes it possible to readily obtain at a high yield, 5-iodo-2-methylbenzoic acid having a high purity which is useful in uses for functional chemical products such as medicines. The process of the present invention comprising iodination reaction, separation and purification steps is characterized by that it is simple in terms of a procedure and that the purification load is smaller, and it is very advantageous in industrially carrying out.

The invention discloses an immobilized ionic-liquid catalyst. A preparing method of the immobilized ionic-liquid catalyst includes the following steps that 1, ionic liquid, absolute ethyl alcohol and tetraethyl orthosilicate are stirred at the constant temperature of 40 DEG C to 70 DEG C till the ionic liquid is dissolved, and the solution is clarified; then a hydrochloric acid solution is added, the mixture is continuously stirred for 1 h to 3 h to be stood and aged for 12 h to 24 h, and a primary product of the mesoporous-silica immobilized ionic-liquid catalyst is obtained; 2, the primary product of the mesoporous-silica immobilized ionic-liquid catalyst is subjected to vacuum drying for 3 h to 6 h at the temperature of 80 DEG C to 100 DEG C, and the mesoporous-silica immobilized ionic-liquid catalyst is obtained. The invention further discloses an application of the catalyst to synthesizing ester lubricating oil. According to the immobilized ionic-liquid catalyst and the application thereof to synthesizing the ester lubricating oil, the catalyst is simple in the synthesizing method and high in catalyst activity, and the process of industrial applications of the catalyst is greatly quickened.

The invention relates to a method of producing methylamine lead halide for perovskite solar cells at low cost through solid phase reaction of formaldehyde and ammonium lead halide. Halogen acid, ammonium halide, lead acetate and acetic acid are mixed according to the mole ratio of (2.1-2.1):(1.1-1.2):1:(20-40), reflux reaction is carried out after the mixture is heated to 100-120 DEG C, acetic acid and water are separated through vacuum distillation, and an ammonium halide lead crystal is generated. The ammonium halide lead crystal and paraformaldehyde are mixed according to the mole ratio of 1:(2.1-2.5), are slowly heated at 120-160 DEG C to react for 1-6h, and are further heated to 170-180 DEG C to react until there is no obvious gas emission. The reaction product is re-crystallized with polarity organic solvent, washed with fatty alcohol and vacuum-dried to get refined methylamine lead halide. The yield was 95-99.2%, and the content is 99.0-99.5%. The production technology is simple, environment-friendly and safe. There is no need for annealing treatment after coating. The methylamine lead halide can be directly used as a light absorption layer of a solar cell.

The invention discloses a method for preparing a lamellar-form borate crystal material, which comprises the following steps: dissolving borax and an ethylic acid in distilled water, then transferring the solution into a teflon-lined hydrothermal kettle; after constant-temperature heating reaction, naturally cooling the reaction product to room temperature; sequentially carrying out centrifugal washing on the obtained product in the hydrothermal kettle separately by using distilled water and absolute ethyl alcohol; and after centrifugal separation, carrying out vacuum drying so as to obtain a high-purity lamellar-form borate crystal material. Compared with borate crystals prepared by using traditional methods, borate crystals prepared by using the method disclosed by the invention has the advantages that raw materials are cheap, purity is high, grain size distribution is narrow, grain agglomeration degree is low, crystal growth is complete, form and size are controllable, the process is simple and efficient, preparation temperature is low, later crystallization does not need to be carried out, and the defects of grain growth, coarsening or curling and the like possibly caused in the process of later heat treatment can be avoided to a certain extent.

A method of refining scrap silicon using an electron beam includes a step of selectively preparing lumps of n-type scrap silicon containing a specific impurity element as a dopant, a step of crushing the prepared lumps of scrap silicon, a step of placing the crushed silicon into a vacuum vessel, a step of irradiating the crushed silicon which was placed into the vacuum vessel with an electron beam to melt it and vaporize at least a portion of the impurity element, and a step of solidifying the resulting silicon.

The invention belongs to the technical field of material preparation, in particular to a preparation method of high-purity LiNH2BH3 and NaNH2BH3. In the method of the invention, liquid-solid reaction is carried out for synthetizing LiNH2BH3 and NaNH2BH3 under an anhydrous oxygen-free inert atmosphere; after LiNH2BH3 and NaNH2BH3 are washed by solvent, the solvent is removed with a vacuum devolatilization method to obtain high-purity solid LiNH2BH3 and NaNH2BH3; and particles with different granularities are prepared by changing synthesis conditions. The method of the invention has simple technology, convenient operation, easy realization and no high requirements on equipment, can produce high-purity products, and product granularity has certain controllability.

The invention discloses a preparation method of teriparatide. The preparation method comprises steps as follows: 2-CTC resin is taken as a resin carrier and is coupled with Fmoc-Phe-OH under the action of an activator and a coupling reagent, and Fmoc-Phe-resin is obtained, an Fmoc deprotection reagent is added to the Fmoc-Phe-resin, after a reaction ends, washing is performed with N,N-DMF, Phe-resin is obtained, one-by-one extension coupling is performed on amino acid under the action of a condensation reagent and an activating reagent, and teriparatide-resin is obtained; a lysate containing PhSMe/PhOH/EDT system is added to the teriparatide-resin, and a crude product of teriparatide is obtained; the crude product of teriparatide is separated, purified and freeze-dried by use of a C18 column, and high-purity teriparatide is obtained. The preparation method of teriparatide is low in cost and adopts a simple process. The total yield of teriparatide is increased, and no harm is caused toany environment. The preparation method is suitable for large-scale production.

The invention relates to the field of medicine synthesis, and discloses a method for synthesizing ganirelix acetate. The method comprises the following steps: carrying out esterification reaction on D-alanine with a protecting group coupled to an N end, and amino resin with a protecting group coupled to amino under the action of a contracting reagent and an activating reagent to obtain peptide resin 1; carrying out gradual extending coupling on other protected amino acids under the action of the contracting reagent and the activating reagent from the peptide resin 1 according to the order from a C end of a ganirelix acetate amino acid sequence to the N end, thus obtaining corresponding peptide resin after extending coupling each time; finally obtaining ganirelix acetate resin, carrying out acidolysis to obtain a ganirelix acetate crude product; and purifying the ganirelix acetate crude product to obtain a ganirelix acetate pure product. According to the method disclosed by the invention, an appropriate synthetic scheme is selected; Ac-D-Nal is selected as the finally synthesized raw material; the whole synthesis process is optimized; an appropriate acidolysis liquid and amino resin are selected to be synthesized; the purity of the ganirelix acetate is improved; and the ganirelix acetate is relatively high in total yield, and is free of harm to any environment.

The invention discloses a preparation method of 3-methyl-1, 4, 2-dioxazole-5-one, a product and application. The method is characterized by comprising the following steps of: adding acetohydroxamic acid, dimethyl carbonate and a catalyst into a reaction flask, performing heating to 110DEG C, carrying out reaction while fractionating a byproduct methanol, carrying out the reaction for 4h, then carrying out reduced pressure distillation on the reaction liquid, and collecting 89DEG C/10mmHg fraction to obtain 3-methyl-1, 4, 2-dioxazole-5-one. According to the method, the 3-methyl-1, 4, 2-dioxazole-5-one is synthesized by using an ester exchange method, few byproducts are produced, the catalyst can be separated after being filtered, and the later purification step is greatly reduced, so that ahigh-purity product is easy to obtain.

The invention discloses a preparation method of a lorazepam intermediate, which comprises the following steps: adding 4-dimethylaminopyridine into a mixed solution of 7-chloro-2-oxo-5-(2-chlorphenyl)-1, 4-benzodiazepin-4-oxide, acetic anhydride and an aprotic polar solvent, stirring, heating, carrying out heat preservation reaction, cooling after the reaction is finished, adding water to separate out materials, filtering, washing with water, refining to obtain a target product. According to the invention, under the condition of greatly reducing the dosage of acetic anhydride, the yield of acylation and rearrangement reactions of lorazepam is ensured, and the discharge of acid-containing wastewater is greatly reduced; in addition, in the reaction process, the temperature is stable, the phenomenon of violent rising does not occur, and the production safety is greatly improved.

The invention discloses a preparation method of an oxazepam intermediate, which comprises the following steps: adding acetic anhydride and anhydrous acetate into 7-chloro-2-oxo-5-phenyl-2, 3-dihydro-1-H-1, 4-benzodiazepine-4-oxide in an aprotic polar solvent, stirring and heating to carry out heat preservation reaction, and then cooling, separating and refining to obtain the oxazepam intermediate as shown in a formula I. according to the method, acylation and rearrangement are carried out under a formed homogeneous system, so that the reaction yield is increased, the acetic anhydride consumption is greatly reduced, and the raw material cost and the sewage treatment cost are reduced; in addition, the reaction is stable in a homogeneous system, the safety is obviously improved, and the method is suitable for large-scale industrial production.

The invention provides a bifunctional ionic liquid and an application thereof, and relates to the technical field of lubricating oil, the bifunctional ionic liquid is obtained by reaction of ionic liquid 1-alkyl-3-methylimidazole bromine and bis (2-ethylhexyl) hydrogen phosphate, and the bifunctional ionic liquid is applied to synthetic ester lubricating oil as a catalyst and a lubricating oil additive. The bifunctional ionic liquid is applied to synthesis of ester lubricating oil as the catalyst, separation is not needed, and the performance of the ester lubricating oil can be improved.