75 results about "Propyne" patented technology

The invention relates to an alkynyl-modified acyl covalent organic framework (COF) material and application thereof, and relates to the field of preparation of crystalline porous materials and fuel cells. The material is a covalent organic framework material which is synthesized by taking 1, 3, 5-triformyl phloroglucinol and 2, 5-bis (2-propynyloxy) terephthaloyl hydrazine as raw materials through solvothermal reaction under specific conditions, and has relatively high crystallinity. The material has good performance in the aspect of proton conductivity, the highest proton conductivity can reach 6.16163 * 10 <-4 > S / cm, and the mechanical property is enhanced due to introduction of alkynyl. Alkynyl is used as an active functional group, and various chemical reactions can be derived, so that the potential application value of the material is greatly improved.

The invention relates to a preparation method of propargyl alcohol, and belongs to the technical field of organic chemistry. The reaction formula is as follows: # imgabs0 #; comprising the following steps: (1) taking Z-1, 3-dichloropropene as a raw material, adding dimethyl sulfoxide and solid alkali into an organic solvent, heating, carrying out heat preservation reaction until the content of the Z-1, 3-dichloropropene is less than or equal to 1%, and cooling to room temperature; (2) adding a phase transfer catalyst and water into the reaction liquid obtained in the step (1), heating, and carrying out a heat preservation reaction until an intermediate 3-chloropropyl-2-ene-1-ol is less than or equal to 0.5%; cooling to room temperature; (3) filtering, separating liquid, and adding an extracting agent into a water phase for extraction; and rectifying the extracted organic phase to obtain propargyl alcohol. By controlling the alkaline strength and reaction parameters in the reaction, the production of organic impurity ether compounds can be effectively controlled, the purity and yield of the product are improved, and meanwhile, the reaction time is shortened.

The invention discloses a method for preparing 3, 3, 3-trifluoro-1-propyne through a two-step method, the 3, 3, 3-trifluoro-1-propyne is prepared through a production system and collected through a material collecting system, and the preparation steps of the production system comprise: (1) in a first solvent, carrying out an addition reaction on 3, 3, 3-trifluoro-1-propylene and ICl to obtain 2-iodo-1-chloro-3, 3, 3-trifluoropropane; (2) in a second solvent, enabling the 2-iodine-1-chloro-3, 3, 3-trifluoropropane to react with alkali to eliminate bimolecular hydrogen halide so as to obtain 3, 3, 3-trifluoro-1-propyne; the temperature of the material receiving system is-196 to-60 DEG C, and the pressure of the material receiving system is-0.03 MPa to normal pressure. The 3, 3, 3-trifluoro-1-propyne is prepared by taking trifluoropropene as a raw material through two-step reaction, and the method has the advantages of simple preparation steps, high reaction yield, small amount of three wastes, low production cost and the like, and is very suitable for industrial production.

The present invention belongs to the technical field of heterogeneous catalysts, and particularly relates to a nickel-based sulfur-resistant catalyst for selective hydrogenation of propyne to propylene, a preparation method and an application thereof. A nickel-based sulfur-resistant catalyst for selective hydrogenation of propyne to propylene, the catalyst is composed of a main active component, a first co-metal, a second co-metal and a composite carrier, the main active component is nickel, accounting for 0.5% to 5.0% of the mass of the composite carrier; the first co-metal accounts for 0.5% to 5.0% of the mass of the composite carrier based on the total mass of metal atoms; the second co-metal accounts for 0.5% to 5.0% of the mass of the composite carrier based on the total mass of metal atoms. The catalyst prepared by the method has the advantages of small active metal nickel grains, high specific surface area, good sulfur resistance, etc., and can show excellent conversion rate and propylene selectivity in the reaction of selective hydrogenation of propyne to propylene.

The invention discloses a gram-level synthesis method of Dactyllactone A. The gram-level synthesis method of Dactyllactone A is shown in the description. The method comprises the following steps: with simple and easily available aryl iodide, aziridine and triisopropyl silylacetylene as starting materials, stirring and reacting in an organic solvent at 60-70 DEG C under the action of a palladium catalyst, a phosphine ligand, a norbornene derivative and alkali to obtain a key intermediate; the key intermediate is condensed with iodo gem-dimethyl ester furanone prepared from propiolic acid and dimethyl malonate iodine ylide, and then the condensation product is subjected to an Au / Ag catalyzed intramolecular hydroamination reaction, photocatalytic 6-pi electro-cyclization and two-step conversion, so that the natural product Dactyllactone A can be obtained, wherein the iodo gem-dimethyl ester furanone and iodo gem-dimethyl ester furanone are prepared from propiolic acid and dimethyl malonate iodine ylide. The method has the advantages of cheap and easily available raw materials, short reaction steps, high reaction efficiency, large preparation scale, simple preparation process and the like, has great application potential, and lays a good foundation for industrial production.

The invention discloses a preparation method of 3-((1r, 3r, 5r, 7r)-adamantane-2-yl) propiolic acid. The preparation method provided by the invention comprises the following steps: (1) taking adamantanone as a starting raw material, and carrying out French reaction to prepare a compound 2; (2) the compound 2 is subjected to a dehydroxylation reaction under the action of boron trifluoride diethyl etherate and triethyl silane, and a compound 3 is prepared; and (3) carrying out hydrolysis reaction on the compound 3 under the action of LiOH to obtain a target product, namely 3-((1r, 3r, 5r, 7r)-adamantane-2-yl) propiolic acid. The preparation method disclosed by the invention is short in process route, simple and convenient to operate, mild in reaction condition, easy to control, high in yield, few in by-products, relatively low in cost and suitable for process amplification.

Disclosed are a cationic radical-type triazine-based polyacetylene, a preparation method thereof, and photocatalytic applications. The chemical structure is shown in Formula 3. The preparation method comprises the following steps: using 2,4,6-tris(4-pyridyl)-1,3,5-triazine shown in Formula 1 and propargyl bromide shown in Formula 2 as raw materials, without a catalyst or initiator, to directly prepare the cationic radical-type triazine-based polyacetylene Tz-IRPA-1 shown in Formula 3 in one step through a quaternization-induced in-situ polymerization reaction. The functional polymer prepared by the present invention has a simple process, requiring only a one-step reaction to in-situ prepare the non-metallic polymer catalyst Tz-IRPA-1. The prepared Tz-IRPA-1 is used in a photocatalytic cycloaddition reaction of an epoxy compound and CO2, exhibiting excellent heterogeneous photocatalytic activity under normal temperature and pressure conditions.

The present invention discloses a method for synthesizing substituted pyrrole compounds. The specific steps are as follows: under inert gas protection, an aryl-1-propyne compound, a nitrile compound, and a base are mixed in a molar ratio of 1:1.2:3 in an aprotic solvent for reaction, quenched by adding a saturated aqueous ammonium chloride solution, filtered, washed, evaporated to dryness under reduced pressure, and separated by column chromatography to obtain the substituted pyrrole compound. The present invention reacts under metal-free conditions, has readily available raw materials, has good substrate universality, and is simple to prepare and operate.

The invention discloses a multilayer polycyclic aromatic hydrocarbon organic membrane as well as a preparation method and application thereof. The preparation method comprises the following steps: cleaning and drying a polyacrylonitrile substrate; dropwise adding a poly [1-(trimethylsilyl)-1-propyne] solution on the polyacrylonitrile substrate, and carrying out spin coating to form a uniform supporting layer; the preparation method comprises the following steps: preparing pre-prepared hexa (tripyridine) hexaphenylbenzene polycyclic aromatic hydrocarbon into a hexa (tripyridine) hexaphenylbenzene polycyclic aromatic hydrocarbon monomolecular layer compressed film by adopting a Langeron film preparation instrument, and transferring the monomolecular layer compressed film to the surface of a polyacrylonitrile substrate spin-coated with a poly [1-(trimethylsilyl)-1-propyne] layer; the multi-layer polycyclic aromatic hydrocarbon organic membrane is obtained by repeating the monomolecular layer compression and horizontal contact transfer process, the efficient size exclusion effect is achieved, and the method has the advantages of high permeability, high selectivity, rapidness and low-cost preparation.

A high-precision separation device and method for dissolved gas components in transformer oil, belonging to the technical field of transformer fault detection, relates to solving the problems of large error and low precision in existing detection technologies due to low content of dissolved gas components in transformer oil; the high-precision separation device for dissolved gas components in transformer oil adopts a central cutting analysis method to fully analyze the dissolved gas hydrogen, methane, carbon monoxide, carbon dioxide, ethylene, ethane, acetylene, propylene, propane and propyne components in transformer oil through the connection and switching between a first switching valve, a second switching valve, a third switching valve, a fourth switching valve and a first chromatographic column, a second chromatographic column, a third chromatographic column and a fourth chromatographic column, without interference peaks between the components, and a quantitative loop is set in the device for sampling, thereby realizing quantitative and accurate analysis, greatly reducing the sampling error, and the sensitivity can reach the μmol / mol level.

The invention belongs to the technical field of petroleum and natural gas yield increase, and particularly relates to a preparation method of an anti-shearing polymer fracturing fluid. The preparation method comprises the following steps: preparing a monomer with high strength and shear fracturing resistance from methyl propiolate, aluminum chloride, cyclooctene and other raw materials, adding the monomer into N-vinyl pyrrolidone, 2-acrylamido-2-methylpropanesulfonic acid and acrylamide to prepare a polymer, and mechanically stirring at a high speed to obtain the polymer. And completely dissolving the reaction monomer. And adding an initiator to initiate the monomers to polymerize under the irradiation of an ultraviolet lamp, and reacting at a constant temperature to obtain a product. The synthesis method disclosed by the invention has the characteristics of low cost, high yield and simple preparation process, no by-product is generated, and the obtained product has good anti-shearing performance and has a relatively good application prospect in oil field fracturing and recovery efficiency improvement.

The present invention discloses a Zr-MOF material for one-step purification of ethylene and propylene and a preparation method thereof. This material can purify olefins in a one-step manner from a C2 or C3 three-component mixed gas, and has two mutually perpendicular one-dimensional pore channels in the shapes of "pear" and rhombus, with a structural general formula of ZrO(C 34 H 24 O 16 S2). This MOF material exhibits a high alkane adsorption capacity and a high separation selectivity for olefins. This material can purify ethylene in a one-step manner from a C2 three-component mixed gas (ethane / ethylene / acetylene) and purify propylene in a one-step manner from a C3 three-component mixed gas (propane / propylene / propyne) in a dynamic breakthrough experiment. The novel Zr-MOF material constructed in the present invention (named NKU-301) not only has high stability and can purify olefins in a one-step manner from a three-component mixed gas in an industrial environment, but also provides a new design strategy and theoretical guidance for the design and synthesis of adsorbent materials for highly efficient one-step separation of olefins.

The present invention relates to the technical field of organic electrochemical synthesis, and in particular to a method for preparing propargyl alcohol by electrolyzing glycerol. The specific method comprises the following steps: adding glycerol and an aqueous chloride solution of an alkali metal or an alkaline earth metal into an electrolytic cell, electrolyzing under the action of a direct current to obtain an electrolyte containing propargyl alcohol, chlorine and hydrogen, and separating the electrolyte by a membrane to obtain propargyl alcohol. The method of the present invention produces propargyl alcohol by dehydrating glycerol in an electrolytic cell, and other substances involved in the reaction are recycled, and the entire reaction process is green and environmentally friendly. The method is simple and safe, and the propargyl alcohol is easily separated and has a high yield.

The invention discloses a method for preparing 1,1,2,3-tetrachloropropylene, which belongs to the field of fine chemicals. 3-chloropropyne is used as a starting material, 3-chloropropyne is reacted with N-chlorosuccinimide ( NCS) is chlorinated under alkaline conditions to obtain 1,3-dichloropropyne; then chlorine is introduced under the action of a catalyst to prepare 1,1,2,3-tetrachloropropylene. The overall two-step process of the present invention is simple, the raw material market source is abundant, and after the step-by-step reaction, chlorine is finally added with a specific catalyst, which has the advantages of easy product purification, relatively high yield and low cost.

The invention discloses a preparation method of 3, 3, 3-trifluoro-1-propyne, which comprises the following steps: (1) taking E-1-chloro-3, 3, 3-propylene as a raw material, and carrying out chlorine or bromine addition to obtain a compound as shown in a formula (I); (2) in a first solvent, in the presence of alkali, the compound shown in the formula (I) is subjected to an elimination reaction to obtain 1, 2-diX-3, 3, 3-trifluoropropene shown in the following formula (II) and / or 2-X-1-chloro-3, 3, 3-trifluoropropene shown in the following formula (III), X is chlorine or bromine, when X is chlorine, the structures of the formula (II) and the formula (III) are the same, and the formula (II) and the formula (III) are 1, 2-dichloro-3, 3, 3-trifluoropropene; and (3) in a second solvent, in the presence of a reducing agent, carrying out elimination reaction on the compound as shown in the formula (II) and / or the formula (III) to obtain the 3, 3, 3-trifluoro-1-propyne. According to the method, the trifluoropropyne is prepared by taking E-1233zd as a raw material, the technical problems of low conversion rate and poor selectivity in the process of preparing the trifluoropropyne through an E-1233zd raw material route are solved, the raw materials are easy to obtain, the cost is low, the method is very suitable for industrial application, and the market competitiveness of the product can be greatly improved.

The invention belongs to the field of chemical engineering, and particularly relates to purification of butadiene, in particular to a butadiene purification system and a control method for the content of propyne in a propyne tower. According to the butadiene purification system disclosed by the invention, the propyne recovery system is arranged, so that recycling of propyne is realized, and environmental pollution is reduced. The invention further provides a method for controlling the content of the propyne in the propyne tower, whether the propyne in the propyne tower is discharged or not is controlled according to the pressure and / or temperature of the top end of the propyne tower, and the yield and purification efficiency of 1, 3-butadiene are balanced.

The invention discloses a synthesis method of furatadone, which comprises the following steps: by taking 1-(4-morpholinyl)-2-propyne as a raw material, carrying out [3 + 2] cycloaddition reaction on the 1-(4-morpholinyl)-2-propyne and di-tert-butyl azodicarboxylate to obtain a 3, 5-disubstituted oxazolone intermediate; then under the action of a Pd / C catalyst, carrying out a hydrogenation reaction of olefin to obtain N-Boc protected AMOZ; finally, the AMOZ protected by N-Boc and 5-nitrofurfural are subjected to a condensation reaction under the action of hydrogen chloride, and the product furaltadone is obtained. The synthesis method is simple, environmentally friendly and suitable for large-scale production.

A method for removing acetylene from ethane cracking to olefins involves selectively hydrogenating a mixture of C2 and C3 hydrocarbons from ethane cracking to remove acetylene, propyne, and propadiene. Reaction conditions: inlet temperature 50℃~95℃, pressure 1.5~3.0MPa, space velocity 8000~14000h⁻¹ ‑1 The catalyst support is alumina or mainly alumina, and has a bimodal pore distribution structure with a micropore size of 40–70 nm and a macropore size of 200–500 nm. The specific surface area of ​​the catalyst support is 4–15 m². 2 / g. The catalyst contains at least Pd, Fe, Ni, and Cu, with Pd supported in both microemulsion and solution formats, Ni and Cu supported in microemulsion, and Fe supported in solution. The solution-supported Pd and Fe are mainly loaded in micropores of 40–70 nm, while the microemulsion-supported Ni, Cu, and Pd are mainly distributed in macropores of 200–500 nm. This alkyne removal method exhibits low reduction temperature, low "green oil" formation, and excellent catalytic performance and anti-coking properties.

The utility model relates to the field of chemical separation, in particular to a separation and purification system for synthesizing propargyl alcohol, which comprises a gas mixing device, an acetylene gas pressurizing device, an ethynylation reaction device, a gas-liquid separator, a butynediol separation tower, a formaldehyde recovery tower, a methanol separation tower, a propargyl alcohol product tower and a chromatography device which are connected in sequence. The system disclosed by the utility model can improve the selectivity of propargyl alcohol in the production process of butynediol under the condition of ensuring the safety of high-pressure acetylene, and effectively realize the separation of propargyl alcohol, so that the supply capacity of propargyl alcohol in the market is obviously improved. The device disclosed by the utility model not only improves the yield of the byproduct propargyl alcohol in BYD production, but also separates and extracts important chemical raw materials such as 1, 4 butynediol.

The present invention provides a refrigerant-containing composition having a lower GWP than that of R410A and having a COP equivalent to that of R410A. Specifically, the present invention provides a composition containing a refrigerant, the refrigerant containing CO2 (R744) and a compound (A), the compound (A) being at least one type selected from the group consisting of trans-1, 2-difluoroethylene [(E)-HFO-1132], cis-1, 2-difluoroethylene [(Z)-HFO-1132], vinyl fluoride (HFO-1141), and 3, 3, 3-trifluoropropyne (TFP).

The application relates to a kind of 2H-chromene phenyl ketone derivatives of double halogen substitution and preparation method and application thereof, belong to the technical field of organic room temperature phosphor material technology.The preparation method of derivative of the application comprises the following steps: (1) under inert gas protection, with halogenated salicylaldehyde and 1-(3-bromine prop-1-alkyne-1-yl) halogenated benzene as raw material, potassium carbonate as base, acetonitrile as solvent, reflux reaction is carried out, the reaction solution is extracted, dried, column chromatography separation, and intermediate 1 is obtained; (2) under inert gas protection, intermediate 1 is dissolved in dichloromethane, boron trifluoride ether is added, and stirring reaction is carried out, and the reaction solution is extracted, dried, column chromatography separation, and the application is obtained.The synthesis route of derivative of the application is simple, high in yield, easy to purify, and the prepared room temperature phosphor material can be widely applied in the field of organic light emitting diode, information encryption, biological imaging and optical sensing.

This utility model relates to the field of pesticide production technology, specifically to a device for preparing a compound suspension of propyzamide and metolachlor, comprising a mixing tank, a sealing cover fixedly connected to the upper end of the mixing tank, and a stirring assembly provided on the surface of the sealing cover. The stirring assembly includes a servo motor, a first bevel gear, a stirring frame, a connecting shaft, a second bevel gear, a first stirring blade, a stirring shaft, a third bevel gear, and a second stirring blade. A device housing is fixedly connected to the upper surface of the sealing cover, and a feed chute is provided on the left side of the device housing. Viewing windows are provided on both the front and rear sides of the sealing cover. Through the cooperation of the servo motor, the first bevel gear, the second bevel gear, the third bevel gear, the stirring frame, and the stirring shaft, the first and second stirring blades are driven to rotate in opposite directions, preventing the pesticide solution from rotating in the same direction, facilitating rapid dispersion of the internal suspension, and effectively improving the mixing efficiency and mixing effect of the pesticide solution.

This application provides a method for flotation separation of chalcopyrite and pyrite, relating to the field of mineral flotation. The method involves mixing and flotation of the minerals to be processed, including chalcopyrite and pyrite, with a chalcopyrite collector to obtain chalcopyrite concentrate and pyrite tailings. The general structural formula of the chalcopyrite collector is: [Formula omitted]. This chalcopyrite collector utilizes the high selective affinity of its propyne ester group for copper-active sites on the chalcopyrite surface and its inertness to iron sites on the pyrite surface, achieving precise identification and collection of chalcopyrite from the molecular structure of the reagent, significantly improving the grade and recovery rate of the copper concentrate. The R group is a hydrophobic group facing the pulp, significantly enhancing the surface hydrophobicity of the chalcopyrite particles, thereby enabling them to adhere to flotation bubbles and float.

The present invention provides a synthesis method, a forming method and an application of a metal-organic framework material. The synthesis method of the present invention includes: reacting a calcium salt with squaric acid to obtain calcium squarate, wherein the calcium salt is a weak acid salt of calcium ions. The synthesis method of the present invention does not require the additional use of an alkaline additive to promote the dissolution of squaric acid, and can achieve the large-scale synthesis of the metal-organic framework material at room temperature. The reaction conditions are mild, the process is simple and easy to operate, the reaction yield is high, and the product purity is high. The present invention also avoids pore blockage by adding a suitable binder during the forming process of the metal-organic framework, and the formed material has excellent adsorption and separation effects on propyne and propylene gases.

The application relates to a preparation method of a novel microporous copper-based metal organic framework material (Cu-MOF) and gas separation application thereof. Cu metal centers are all in a four-coordination mode, each independent Cu atom is coordinated with one oxygen atom on a BODC ligand, carboxyl O atoms on the BODC ligand all participate in coordination, and a propeller binuclear coordination geometry of the Cu-MOF is formed; wherein each BODC ligand acts as a four-connected node and is connected with four crystallographically independent Cu centers, and the carboxyl on the BODC ligand is connected and supported, and the bridge ring in the middle section contains rich methylene groups, and the rich H atoms can all act as potential action sites. The regularly arranged BODC ligands in the Cu-MOF channel provide hydrogen bond acceptors, which are favorable for strengthening the action force between low-carbon hydrocarbon gas molecules and the framework, so that the effects of preferentially adsorbing acetylene, ethane, propylene, propyne and sulfur hexafluoride gas in acetylene / carbon dioxide, ethane / ethylene, propylene / ethylene, propyne / propylene, sulfur hexafluoride / nitrogen and other mixed gases are realized.

To provide an azeotropic mixture and a method for reducing 2333 - trifluoropropyne (TFPY) which is an impurity in the production of 333 - tetrafluoropropene (HFO - 1234yf).SOLUTION: A heterogeneous azeotrope or azeotrope-like composition comprising TFPY and hydrogen fluoride (HF), wherein the composition may comprise from about 71. 5wt.% to about 98. 8wt.% TFPY and from about 1. 2wt.% to about 28. 5wt.% hydrogen fluoride, and wherein the composition has a boiling point from about - 10.0 °C. to about 25.0 °C. at a pressure from about 61psia to about 171psia. This azeotrope or azeotrope-like composition can be used to separate TFPY as an impurity from 2-chloro - 333 - trifluoropropene (1233xf), 2-chloro - 1112 - tetrafluoropropane (HCFC - 244bb), or HFO - 1234yf compositions.SELECTED DRAWING: Figure 1

The present application provides a refrigerant and a method for preparing the same. The refrigerant is composed of a first component, a second component and a third component, wherein: the first component is 3,3,3-trifluoropropyne; the second component is trifluoroiodomethane; the third component is one of propylene or fluoroethane; in the refrigerant, the content of the first component is a first preset value, the content of the second component is a second preset value, and the content of the third component is a third preset value; satisfying: the first preset value, the second preset value and the third preset value are all greater than zero, and the sum is 100%. The present application is a refrigerant composed of three components, with a GWP of less than 150 and an ODP of 0. Under the premise of ensuring good environmental performance of the refrigerant, the thermal performance is equivalent to R290, and the flammability is greatly reduced, which can solve the technical problems of high flammability and poor safety performance of R290 refrigerant.

The invention discloses a process for preparing 3-chloropropyne through concerted catalysis of phosphine ligand-transition metal in the technical field of organic synthesis. The process realizes efficient synthesis through specific steps: firstly, mixing a porous nitrogen-doped carbon-loaded phosphine ligand-metal nano composite material, palladium chloride and triethylamine under the protection of nitrogen to form a catalytic system; dissolving propargyl alcohol and N-chlorosuccinimide in anhydrous tetrahydrofuran, and mixing in an ice bath to obtain a pre-reaction mixture; then adding the pre-reaction mixture into a catalytic system, stirring and reacting at a specific temperature under the protection of nitrogen, and monitoring the progress through thin layer chromatography in the reaction; and after the reaction is finished, filtering and separating the catalyst, evaporating filtrate under reduced pressure to remove the solvent, and purifying by column chromatography to obtain a target product. The process is high in catalytic efficiency, good in selectivity, high in product yield and environment-friendly.

The present invention provides a composition comprising a refrigerant (mixed refrigerant) having three types of performance, i.e., a coefficient of performance (COP) and refrigerating capacity (Cap) that are equivalent to or higher than those of R410A, and a sufficiently low GWP. Specifically, the present invention provides a composition comprising a refrigerant, the refrigerant comprising CF3I, CO2 (R744), and at least one compound A selected from the group consisting of trifluoroethylene (HFO-1123), trans-1,2-difluoroethylene [(E)-HFO-1132], cis-1,2-difluoroethylene [(Z)—HFO-1132], fluoroethylene (HFO-1141), and 3,3,3-trifluoropropyne (TFP).