651 results about "Formic Aldehyde" patented technology

The invention relates to a crown ether covalent organic framework material as well as a preparation method and application thereof. The preparation method comprises the following steps: dissolving a crown ether monomer and an amino monomer in an o-dichlorobenzene solvent, adding a catalyst acetic acid aqueous solution, and uniformly dispersing to form a reaction solution; the method comprises the following steps: freezing a reaction solution through a liquid nitrogen bath, vacuumizing, filling nitrogen, carrying out a heating reaction, and carrying out post-treatment operations such as washing and drying on a reaction product, so as to obtain the crown ether covalent organic framework material BADT-DB18C6-COF. The crown ether covalent organic framework material is formed by condensation of a crown ether aldehyde monomer and an amino monomer, the crown ether monomer is 4, 4 ', 4' ', 4 '''-(6, 7, 9, 10, 17, 18, 20, 21-octahydrodibenzo [B, K] [1, 4, 7, 10, 13, 16] hexaoxacyclo octadecene-2, 3, 13, 14-tetrayl) tetrabenzaldehyde, and the crown ether monomer is 4, 4 ', 4' ', 4'''-(6, 7, 9, 10, 17, 18, 20, 21-octahydrodibenzo [B, K] [1, 4, 7, 10, 13, 16] hexaoxacyclo octadecene-2, 3, 13, 14-tetrayl) tetrabenzaldehyde. The amino monomer is 4 ', 5'-bis (4-aminophenyl)-[1, 1 ': 2', 1 ''-terphenyl]-4, 4''-diamine. The crown ether covalent organic framework material BADT-DB18C6-COF prepared by the invention is mainly used as an adsorbent, is used for adsorbing and recovering uranium, thorium and americium ions from a solution, shows good adsorption capacity on radionuclides U-238, Th-232 and Am-243, and is particularly suitable for the field of spent fuel post-treatment in the nuclear industry.

The invention discloses a phenanthridine-6-formaldehyde derivative and a preparation method and application thereof.The preparation method comprises the steps that 2, 4, 5, 6-tetra (9-carbazolyl)-isophthalonitrile serves as a photocatalyst, 1-azabicyclo [2.2. 2] octane serves as a hydrogen atom transfer catalyst, a biphenyl isocyanide compound, the photocatalyst, the hydrogen atom transfer catalyst and an alkali additive are jointly dissolved in 1, 3-dioxolane, the mixture is stirred to be uniform, and the phenanthridine-6-formaldehyde derivative is obtained. And carrying out free radical tandem cyclization and acid-catalyzed hydrolysis reaction to obtain the phenanthridine-6-formaldehyde derivative. The invention also provides a specific reaction equation. According to the developed synthesis method of the phenanthridine-6-formaldehyde derivative, the compound can be efficiently and conveniently prepared, the technical bottlenecks of harsh reaction conditions and tedious steps in a traditional process are successfully overcome, raw materials which are low in price and easy to obtain are adopted, operation is carried out under mild conditions, the synthesis method has the outstanding advantages of being high in yield, safe and simple to operate, environmentally friendly and the like, and the method is suitable for industrial production. Good industrial application potential is shown.

The invention relates to preparation of a crystalline allyl covalent organic framework material and application research of the crystalline allyl covalent organic framework material in benzamide cyclization green photocatalytic conversion. The SF-COF material is prepared by adopting a step-by-step synthesis method. The preparation method comprises the following steps: synthesizing a COF precursor by taking 1, 3-benzenetricarboxaldehyde and p-aminophenylacetonitrile as raw materials, and preparing the allylation covalent organic framework material with the electronic push-pull effect from the COF precursor and 5, 5 ', 5'-(benzene-1, 3, 5-triyl) tri (thiophene-2-formaldehyde) through a solvothermal method. The material is applied to the field of photocatalytic organic conversion, and benzamide cyclization and conversion of derivatives of benzamide are achieved under irradiation of a blue light LED. The prepared SF-COF has the advantages of efficient charge separation and electron conduction performance, good structural stability and chemical stability and the like. And a catalyzed organic reaction substrate has the advantages of wide universality range, good cycle stability and the like, and shows excellent photocatalytic conversion capability.

The invention belongs to the technical field of epoxy resin, and particularly relates to double-dynamic-bond synergistic exchange epoxy resin as well as a preparation method and application thereof. The preparation method of the double dynamic bond synergistic exchange epoxy resin comprises the following steps: adding aromatic dialdehyde and amino-containing disulfide into a solvent for condensation reaction, and filtering and drying to obtain a double dynamic bond curing agent; the preparation method comprises the following steps: adding the double-dynamic-bond curing agent into epoxy resin, carrying out ring-opening addition reaction, carrying out gradient heating curing, and cooling to room temperature, the aromatic dialdehyde is terephthalaldehyde, isophthalaldehyde or o-phthalaldehyde, and the amino-containing disulfide is 2, 2 '-diaminodiphenyl disulfide or 4, 4'-diaminodiphenyl disulfide. The invention designs and synthesizes a double-dynamic covalent bond curing agent containing an imine bond and a disulfide bond, and is used for constructing a novel degradable and self-healing epoxy resin. The material maintains good thermal stability and insulation performance, and realizes degradation and self-healing functions at the same time.

The invention discloses a carbamoyl-substituted diarylethene derivative as well as a preparation method and application thereof, and the preparation method comprises the following steps: reacting R-substituted 3-bromo-2-hydroxybenzaldehyde with an arylmethyl triphenylphosphonium bromide compound or an aryl acetic acid compound to obtain an intermediate A; then the intermediate A and cuprous cyanide are subjected to a heating reaction in N, N-dimethylformamide and nitrogen atmosphere, and an intermediate B is obtained; and finally, heating the intermediate B, acetaldoxime and indium trichloride in toluene for reaction to obtain the carbamoyl-substituted diarylethene derivative. The carbamoyl-substituted diarylethene derivative disclosed by the invention has a remarkable effect in an in-vitro anti-tumor activity test, particularly has excellent anti-proliferation ability to human BRCA mutant tumor cells, and can be used for preparing medicines for treating PARP-1 activity abnormity related diseases. The synthesis route is simple, the cost is low, and large-scale implementation is facilitated.

The invention belongs to the technical field of microbial fermentation and insect pest prevention and control, and particularly relates to endogenous bacillus velezensis and application of fermentation liquor of the endogenous bacillus velezensis in prevention and control of bemisia tabaci. The invention discloses bacillus velezensis NM153 which is preserved in the China Center for Type Culture Collection on March 27, 2025, and the preservation number of the bacillus velezensis NM153 is CCTCC (China Center for Type Culture Collection) M 2025605. A stock solution of the bacillus velezensis NM153 supernate and the bacterial suspension is diluted by 300 times and 500 times to treat the bemisia tabaci, and the result shows that the death rate of the bemisia tabaci treated by the bacillus velezensis NM153 supernate is obviously higher than that of a bacterial suspension treatment group, and the death rate of the bemisia tabaci treated by the bacterial suspension treatment group is obviously higher than that of the bemisia tabaci treated by the bacillus velezensis NM153. In addition, the bacillus velezensis NM153 metabolite is further verified and explained to have a remarkable technical effect on preventing and treating bemisia tabaci in o-carboxybenzaldehyde, tenuitoxin and micronomicin in the bacillus velezensis NM153 metabolite.

The invention provides a preparation method of an omariglitazone intermediate, which comprises the following steps: by taking p-halogenated benzaldehyde as a raw material, carrying out aldol condensation reaction, hydrolysis, decarboxylation, reduction, ring closing and the like to obtain an intermediate as shown in a formula 9, carrying out catalytic reaction, reduction reaction, ring closing and the like to obtain an intermediate as shown in a formula 13, and finally hydrolyzing to obtain a target product omariglitazone intermediate A. According to the invention, links of precious metal use and chiral resolution (key steps influencing cost and yield) in the prior art are avoided, and a method for synthesizing a single configuration through a chemical method is adopted, so that the yield is greatly improved, and the production cost is greatly reduced; meanwhile, a synthesis route is broken through, a target product is synthesized through cheap initial materials, and post-treatment is simpler and more controllable.

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.

The invention discloses a flame-retardant corrosion-resistant coating and a preparation method thereof, and relates to the technical field of fluorocarbon resin powder coatings. The flame-retardant corrosion-resistant coating comprises the following raw materials in parts by weight: 15-25 parts of fluorocarbon resin, 40-50 parts of epoxy resin, 3-5 parts of a curing agent, 5-7 parts of a reinforcing agent, 4-6 parts of a corrosion inhibitor, 6-8 parts of filler, 1-2 parts of a flatting agent and 0.5-1 part of benzoin. The preparation method comprises the following steps: reacting phosphonitrilic chloride trimer with p-hydroxybenzaldehyde to generate an intermediate 1, reacting the intermediate 1 with p-aminobenzoic acid to generate an intermediate 2, and reacting the intermediate 2 with 2-heptyl ethylene oxide to generate the reinforcing agent. The flame-retardant corrosion-resistant coating prepared by the invention has excellent mechanical properties, corrosion resistance, aging resistance and flame retardance.

The invention provides a chemical or enzymic method regenerated PET and PTA screening method, which comprises the following steps: pretreating a PET or PTA sample 1, and measuring the content of p-toluic acid, the content of p-carboxybenzaldehyde and the content of m-terephthalic acid by using high performance liquid chromatography; the method comprises the following steps: pretreating a PET or PTA sample 2, pretreating by using a high-temperature pyrolysis method, and measuring an isotope ratio of oxygen-18 to oxygen-16 by using an isotope ratio mass spectrometer; the method comprises the following steps: calculating a cleanliness index, an oxy-18 index and a bottle flake index by using a formula based on a test result, and classifying PET and PTA samples through a decision tree according to the indexes; combining and mixing the PET and PTA products based on the classification result and the requirements of downstream customers on the regeneration method and the regenerated material content; the method is convenient, accurate and reliable, the classification result is objective, the screening efficiency of PET and PTA regenerated by a chemical or enzyme method can be improved, and the economic cost is saved.

The invention relates to the field of pipes, and discloses a heat-resistant high-strength MPP cable protection pipe and a preparation method thereof.The cable protection pipe comprises polypropylene resin, composite filler, modified layered lanthanum phenylphosphonate and auxiliaries; the composite filler is prepared by carrying out amino functional covalent modification on halloysite nanotubes by using a modified silane coupling agent, then carrying out protonation treatment and carrying out cation exchange on nano montmorillonite grafted with the modified silane coupling agent, and the modified silane coupling agent is prepared by reacting gamma-methacryloxypropyltrimethoxysilane with polyether amine; the modified layered lanthanum phenylphosphonate is prepared by grafting and modifying the surface of the layered lanthanum phenylphosphonate by using a cyclotriphosphazene substitute, the cyclotriphosphazene substitute is prepared by reacting 4-amino-1, 2, 4-triazole with p-hydroxybenzaldehyde and then substituting with phosphonitrilic chloride trimer, and the prepared MPP cable protection tube has the advantages of good tensile property, high impact resistance, high heat resistance, good flame retardancy, good flame retardancy and good flame retardancy. Meanwhile, excellent flame retardance and antibacterial effect are achieved.

The invention discloses long-acting high-dynamic hydrazone bond hydrogel as well as a preparation method and application thereof, and particularly relates to the technical field of biomedical materials. The preparation method comprises the following steps: taking 1-adamantane acetic acid and adipic dihydrazide modified sodium hyaluronate and benzaldehyde-terminated eight-arm polyethylene glycol as carrier raw materials; the hydrazone bond hydrogel with relatively high stability is prepared through a coupling reaction of an aldehyde group of benzaldehyde-terminated eight-arm polyethylene glycol and a hydrazide group of 1-adamantane acetic acid and adipic dihydrazide modified sodium hyaluronate. The beta-cyclodextrin modified m-phenylenediamine catalyst is dynamically combined into the carrier through reversible host-guest complexation between beta-cyclodextrin and 1-adamantane acetic acid, so that the long-acting high-dynamic hydrazone bond hydrogel is obtained, and the requirement of three-dimensional culture of stem cells on mechanical properties can be met; and network dynamics can be maintained for a long time, so that stem cell spreading is supported, mechanical signal transduction is activated, osteogenesis-related gene expression is promoted, and stem cell osteogenesis differentiation capability is enhanced.

The invention discloses a phototherapy reagent and a preparation method and application thereof. The preparation method comprises the following steps: 1-[4-(diethylamino) phenyl]-ethane-1-ketone and 4-methoxybenzaldehyde are subjected to a condensation reaction in a NaOH ethanol solution, and a product and nitromethane are subjected to addition; performing condensation and addition on the other groups of raw materials by the same method; cyclizing the two addition products with ammonium acetate, and coordinating with boron trifluoride diethyl etherate to obtain NHM; carrying out substitution reaction on the NHM and sodium nitrite to obtain NOO; and oxidizing NOO by m-chloroperoxybenzoic acid to obtain NNOO. The reagent can target a tumor hypoxia microenvironment, hypoxia monitoring is achieved, NO is released through photostimulation for tumor gas therapy, meanwhile, the secondary amplification photo-thermal therapy effect is achieved, preparation is controllable, diagnosis and treatment are integrated, and the reagent is sensitive, safe and suitable for biomedical research and clinical diagnosis.

The invention belongs to the technical field of organic synthesis and separation, and particularly relates to a method for synthesizing phenolic resin from 2, 4 / 2, 5-methyl ethyl phenol. The invention provides a method for synthesizing phenolic resin from 2, 4 / 2, 5-methyl-ethyl phenol, which comprises the following steps: adding 2, 4 / 2, 5-methyl-ethyl phenol, aldehydes and a catalyst into a reactor, carrying out an anti-thermal insulation reaction, sampling and analyzing until the content of 2, 5-methyl-ethyl phenol is less than or equal to 0.5% and is qualified, heating, decompressing and dehydrating, steaming out unreacted 2, 4-methyl-ethyl phenol and water, and dehydrating to 100-200 DEG C to obtain linear 2, 5-methyl-ethyl phenolic resin; adding a catalyst into the steamed material, heating to completely react the reacted 2, 5-methyl ethyl phenol (when formaldehyde in the steamed material is insufficient, a small amount of formaldehyde can be supplemented), adding a non-water-soluble solvent for extraction and layering, and treating a water layer in a wastewater treatment workshop; and rectifying the oil layer to obtain 99% 2, 4-methyl ethyl phenol or pesticide intermediate 4-ethyl-2-cresol.

The invention relates to the technical field of p-fluorobenzaldehyde production, and particularly discloses a production process of high-purity p-fluorobenzaldehyde. The invention relates to a production process of high-purity p-fluorobenzaldehyde. The production process comprises the following steps: S1, carrying out a chlorination reaction by taking p-fluorotoluene and chlorine as raw materials to prepare a mixed chlorination solution of p-fluoromethyl benzyl monochloride, p-fluoromethyl benzyl dichloride and p-fluoromethyl benzyl trichloride; s2, adding an organic complexing agent, which is a water-soluble aprotic solvent, into the mixed chlorinated liquid prepared in the step S1, and then performing vacuum rectification to obtain distillate and residual liquid; rectifying by taking the residual liquid as a raw material to obtain kettle liquid and rectified liquid; and S3, carrying out hydrolysis reaction by taking the rectification liquid and water as raw materials, separating, and drying to obtain the product. The production process of the high-purity p-fluorobenzaldehyde has the advantages of high raw material conversion rate, high product purity and few three-waste products.

The present invention proposes a method and use for stabilizing a simple agglomerate for pH and salt and with adjustable size. In phosphoric acid buffer solutions with different salt concentrations and pH values, the polyacrylic acid hydroxypropyl group condensation body has specific stability; hydrophobic thermal response blocks are introduced into a hydroxypropyl acrylate monomer through reversible addition-fragmentation chain transfer polymerization to regulate and control the size of a condensation body, and a phase separation behavior is shown at different temperatures; a hydrophobic block without thermal response is introduced to regulate and control the size of the aggregate, and no thermal response behavior is shown. Continuous regulation and control of the size of the aggregate from the micron level to the nano level are achieved, and the requirements of different application scenes are met. The hydroxypropyl polyacrylate condensation body can be used for packaging various dyes and drugs; high-efficiency enzyme protection is achieved, formed aggregates can protect glucose oxidase, and the retention rate of enzyme activity reaches 85% or above after treatment is conducted for 3 hours at 60 DEG C; as a micro-reactor for the reaction of generating p-nitrobenzaldehyde phenylhydrazone from p-nitrobenzaldehyde and phenylhydrazine, the reaction rate is greatly improved.

This invention relates to a trifluoromethyl-substituted pyrene-phenylacetonitrile derivative, its preparation method, and its application. A trifluoromethyl-substituted pyrene-phenylacetonitrile derivative has the structural formula: [formula omitted]. The preparation method involves dissolving 1-pyrene formaldehyde, the corresponding trifluoromethylphenylacetonitrile, and an alkaline catalyst in an organic solvent, and carrying out a Knoevenagel condensation reaction under heating conditions. The reaction product is then post-treated to obtain the pyrene-phenylacetonitrile derivative. The application of a trifluoromethyl-substituted pyrene-phenylacetonitrile derivative in electrical storage devices is also discussed. This invention achieves precise control of storage performance by introducing trifluoromethyl groups at different positions on the benzene ring of the pyrene-phenylacetonitrile backbone, providing a novel design approach for developing new multi-level electrical storage materials. The synthesis route is concise and has broad application prospects in the field of high-density non-volatile memory.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of topiromilast. The preparation method comprises the following steps: taking a compound 1, namely 4-(1H-1, 2, 4-triazole-5-yl)-pyridine, and a compound 2, namely 2-cyanopyridine-4-formaldehyde as raw materials, and reacting under the action of a free radical initiator and a catalyst; and performing post-treatment to obtain the target compound topiromilast. According to the invention, the problems of low yield, use of a highly toxic cyaniding reagent and the like caused by construction of a triazole ring or introduction of a cyano group are avoided; the yield and the purity of the product are improved, the post-treatment operation is simple, and the method is suitable for industrial production.

The invention relates to a water-soluble ultraviolet absorbent 4-disubstituted aminobenzyl subunit camphorsulfonic acid and a synthesis method and application thereof, and the synthesis method comprises the following steps: in a toluene-methanol mixed solvent, carrying out heating reflux reaction on camphorsulfonic acid and 2 equivalent weight of sodium methoxide, and after enolation conversion is completed, carrying out reduced pressure distillation to obtain the 4-disubstituted aminobenzyl subunit camphorsulfonic acid. Slowly dropwise adding a corresponding 4-disubstituted aminobenzaldehyde solution with the molar weight equal to that of camphorsulfonic acid, continuously heating and stirring to react for 6-12 hours, adding water to terminate the reaction, acidifying the reaction solution by using hydrochloric acid or sulfonic acid type cation exchange resin, separating to remove methylbenzene, adjusting the pH value of a water phase to about 6.5, performing rotary evaporation dehydration under reduced pressure, and extracting a crude product by using a conventional method; a target product can be obtained through column chromatography purification, and the target product not only has water solubility, but also has the characteristic of absorbing UVA and UVB ultraviolet light at the same time; the composition can be applied to sun-screening agent products, cosmetics or home care products, and also can be applied to various industrial products such as paint, varnish, plastics, textiles and rubber to improve the light resistance of the industrial products.

The invention relates to the technical field, in particular to an amino resin composite material for a mulching film and a preparation process of the amino resin composite material. The method comprises the following steps: firstly, preparing a melamine-urea-formaldehyde prepolymer; the preparation method comprises the following steps: sequentially adding hydroxymethylated lignin, polydopamine nanoparticles synergistically grafted with furandialdehyde and lignin through a triazine structure, aminated carboxyl nano-cellulose and 2, 5-diformyl furan, and mixing; and adding a latent acid source to carry out acidic polycondensation, terminating the reaction, adding urea, and filtering. According to the invention, through component design and process control, stable chemical crosslinking and interface bonding are formed among the components, and the obtained composite material has high strength, high toughness, excellent tear resistance and puncture resistance, and excellent ultraviolet aging resistance and damp-heat stability, and can realize the balance between the service life of the mulching film and controllable degradability.

The invention relates to the technical field of oilfield chemistry, in particular to a self-crosslinking thickening agent and a preparation method thereof, the self-crosslinking thickening agent is obtained by copolymerization of acrylamide, acrylic acid, a physical crosslinking monomer and a chemical crosslinking monomer; the physical crosslinking monomer is N-cinnamyl-N, N-dimethyl hexadecyl ammonium chloride; the chemical cross-linking monomer is N-allyl-N, N-dimethyl p-benzaldehyde ammonium bromide, and the chemical cross-linking monomer is N-allyl-N, N-dimethyl p-benzaldehyde ammonium bromide; the molar ratio of the acrylamide to the acrylic acid to the physical crosslinking monomer to the chemical crosslinking monomer is (70-80): (15-25): (0.1-0.5): (0.1-0.5). According to the self-crosslinking thickening agent and the preparation method thereof, the thickening agent has good temperature resistance and salt resistance, meets the current oil and gas field development requirements, is reliable in method principle, easy and convenient to operate and mild in reaction condition, has wide market application prospects and can be widely applied to oil and gas resource development of high-temperature and ultrahigh-temperature reservoirs.

The invention relates to the technical field of chemical synthesis, and particularly discloses a compound with a peculiar smell removing function as well as a preparation method and application thereof. The chemical name of the compound is 2-ethoxy-3-((E)-methoxy-3-oxopropyl-1-alkene-1-yl) phenyl cinnamate, the smell of the compound is extremely light, sulfur-containing and nitrogen-containing compounds causing stink can be captured through a Michael addition reaction, and efficient peculiar smell removal is achieved. The preparation method comprises the following steps: (1) taking cinnamic acid as an initial raw material, and reacting with diethylamino sulfur trifluoride to prepare cinnamic acid acyl fluoride; (2) carrying out an esterification reaction on the cinnamic acid acyl fluoride and 2-methoxy-3-hydroxybenzaldehyde in the presence of 4-dimethylaminopyridine, so as to obtain 2-methoxy-3-formyl phenyl cinnamate; and (3) carrying out Wittig reaction on the 2-methoxy-3-formyl phenyl cinnamate and a phosphorus ylide reagent, so as to obtain the target compound.

This application relates to a terphenylamine skeleton compound, its preparation method, and its application, belonging to the field of chemical synthesis technology. The preparation method of the terphenylamine skeleton compound of this application includes the following steps: dissolving 2,4,6-triphenylaniline with thiazole-4-carboxaldehyde or thiophene-3-carboxaldehyde in a solvent, conducting a reductive amination reaction under reducing agent conditions, quenching, extraction, washing, concentration to remove solvent, and purification to obtain the terphenylamine skeleton compound. This application provides a simple and mild synthetic method for the natural active products 5'-phenyl-N-(thiazol-4-ylmethyl)-[1,1':3',1''-terphenyl]-2'-amine and 5'-phenyl-N-(thiophene-3-ylmethyl)-[1,1':3',1''-terphenyl]-2'-amine, which can only be extracted from the secondary metabolites of the marine fungus Aspergillus sp. Furthermore, this method utilizes widely available raw materials, which is beneficial for large-scale industrial production of these natural active products.

This disclosure relates to the field of chemical production technology, and in particular to a production apparatus and method for trioxymethylene. The trioxymethylene production apparatus includes: a reaction unit, a separation unit, a first formic acid absorption unit, and a product distillation unit. The outlet of the reaction unit is connected to the inlet of the separation unit; the gas phase outlet of the separation unit is connected to the inlet of the first formic acid absorption unit; the outlet of the first formic acid absorption unit is connected to the inlet of the product distillation unit; and the liquid phase outlet of the separation unit is connected to the inlet of the reaction unit. The reaction unit is used to convert formaldehyde into trioxymethylene under the action of a catalyst. The separation unit is used to separate the gas phase product from the reaction unit into a liquid stream containing recycled formaldehyde and a gas phase stream containing trioxymethylene. The trioxymethylene production apparatus and method provided by this disclosure are used to remove formic acid, a byproduct in the trioxymethylene production process, and reduce equipment corrosion.

The application provides a preparation method of a rare earth metal adsorption and separation resin and a resin extraction column. The preparation method comprises the following steps: adding an oil phase composed of styrene, divinylbenzene, a pore former and an initiator into an aqueous phase containing a dispersant and an inorganic salt to perform suspension polymerization, so as to obtain a white ball resin; performing phthalimide and hydrolysis on the white ball resin, so as to obtain a primary amine resin; performing reaction on the primary amine resin with chloroacetic acid and an alkaline medium, so as to perform carboxymethylation on part of the primary amine sites; and performing reaction on the obtained intermediate resin with phosphorous acid, formaldehyde and an acidic medium, so as to perform phosphonic acid methylation on the remaining part of the primary amine sites. The white ball resin is first subjected to amination, and then part of the carboxymethylation and part of the phosphonic acid methylation are sequentially performed, so that the carboxyl type chelation sites and the phosphonic acid type chelation sites are simultaneously reserved in the same resin bead, thereby being beneficial to improving the comprehensive adsorption performance and separation performance of the resin on the rare earth metal.

The invention discloses an intermediate for preparing optically pure berbamine and spirosine and a preparation method of the intermediate. The intermediate is a compound (S)-1-(4-(5-(((R)-8-bromo-6, 7-dimethoxy-2-methyl-1, 2, 3, 4-tetrahydroisoquinoline-1-yl) methyl)-2-hydroxyphenoxy) benzyl)-6-methoxy-2-methyl-1, 2, 3, 4-tetrahydroisoquinoline-7-alcohol (20a) or a compound (S)-1-(3-(4-(((R)-8-bromo-6, 7-dimethoxy-2-methyl-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1, 2, 3, 4-tetrahydroisoquinoline-1 The preparation method comprises the following steps: firstly, carrying out a multi-step reaction on 5-bromovanillin, 4-hydroxyphenylacetic acid and 4-benzyloxy-3-methoxybenzaldehyde which are used as initial raw materials to obtain optical pure berbamine and spirosine, and then, carrying out a multi-step reaction on the optical pure berbamine and spirosine to obtain the optical pure berbamine and spirosine, and carrying out a reaction on the optical pure berbamine and spirosine to obtain the optical pure berbamine and spirosine. The synthesis route adopts a convergent synthesis mode, the synthesis efficiency is high, the reaction condition is mild, the safety is high, and the operation is simple and convenient.

The invention relates to a synthesis method of low-cost environment-friendly dioscorea element I. The synthesis method comprises the following steps: by taking 3, 5-dimethoxybenzyl alcohol as a raw material, brominating, reacting with triethyl phosphite and 4-benzyloxy-3-methoxybenzaldehyde to generate 3, 4 ', 5-trimethoxy-3'-benzyloxy stilbene, carrying out ultraviolet cyclization reaction, reacting with palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon, palladium-carbon and debenzylating with hydrogen to obtain the Chinese yam element I. The potassium iodide is used as the catalyst in the ultraviolet lamp irradiation catalytic ring closing reaction, the pure water is used as the detergent, compared with the method adopting iodine as the catalyst and adopting a sodium thiosulfate aqueous solution as the detergent, the product yield of the compound 33-4 is 75%, the yield of the compound 33-5 is 16.6%, the purity is 98.7%, and the method has the advantages of low cost, high yield, few impurities and the like.

The present invention relates to the technical field of organic synthesis. Provided is a method for preparing 2,6-bis(4-azidobenzylidene)-4-methylcyclohexanone, comprising the following steps: S1, subjecting 4-nitrobenzaldehyde and trimethylsilyl azide to a nucleophilic aromatic substitution reaction to obtain 4-azidobenzaldehyde; S2, subjecting 4-azidobenzaldehyde and 4-methylcyclohexanone to an aldol condensation reaction, so as to obtain 2,6-bis(4-azidobenzylidene)-4-methylcyclohexanone. The described technical solution addresses the problems in the related art where the process for synthesizing 2,6-bis(4-azidobenzylidene)-4-methylcyclohexanone has low product yield, high costs and high energy consumption, and is not conducive to large-scale industrial production.

The invention discloses a high-load cobalt monatomic catalyst with a three-dimensional confinement structure as well as a preparation method and application of the high-load cobalt monatomic catalyst. A three-dimensional cyclodextrin-based covalent organic framework 3D-CD-COF, which is constructed by seven-(6-amino-6-deoxy)-beta-cyclodextrin (7ACD) and aromatic dicarboxaldehyde (terephthalaldehyde or 4, 4 '-biphenyl dicarboxaldehyde), is used as a carrier, multiple coordination sites are constructed through salicylaldehyde grafting, and high-loading anchoring of cobalt single atoms is realized; cobalt single atoms are uniformly dispersed in a three-dimensional intercommunicated pore channel in a CoN1O3 coordination form, the loading capacity reaches 13.0-14.0%, and a three-dimensional confinement structure can inhibit four-electron oxygen evolution side reaction. The catalyst has high hydrogen peroxide Faraday efficiency and high yield, compared with Co-CD without a three-dimensional confinement structure, the activity and selectivity are remarkably improved, and an efficient technical scheme is provided for electrochemical preparation of hydrogen peroxide.

The invention discloses a preparation method and application of a pyrenyl imine covalent organic framework material, and belongs to the technical field of materials. The preparation method comprises the following steps: dissolving 4, 4 ', 4', 4 ''-(pyrene-1, 3, 6, 8-tetrayl) tetraphenylamine and 3, 3 '-dimethoxy-[1, 1'-biphenyl]-4, 4 '-diformaldehyde in an organic solvent, fully mixing, and adding a catalyst to obtain a mixed solution; and freezing the mixed solution with liquid nitrogen, exhausting air, removing oxygen, carrying out a heating reaction, obtaining a yellow precipitate after the reaction is finished, and carrying out filtering, washing and vacuum drying treatment to obtain the pyrenyl imine covalent organic framework material. Pyrenyl and imine bonds on the pyrenyl imine covalent organic framework material structure prepared by the invention can provide a large number of binding sites bound with iodine, and the pyrenyl imine covalent organic framework material has the advantages of high crystallinity, large specific surface area, strong stability and the like, and can be used as a solid adsorption material for effective iodine vapor adsorption.