485results about "Sulfide preparation" patented technology

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is as follows: R1, R2 and R3 are respectively selected from one of hydrogen and C1-C4 alkyl, A1 is selected from one of hydrogen and C1-C4 alkyl, and A2 is C1-C4 alkyl; r4 is selected from one of H, phenyl and C1-C4 alkyl, and A2 is C1-C4 alkyl; and R5 is hydrogen or methyl. The optical monomer provided by the invention contains a (methyl) acrylate group, and has the properties of high refractive index and low volume shrinkage; and a plurality of aromatic rings with high molar refractive index and low molar volume are contained, so that the whole molecule of the whole monomer is extremely high in refractive index. The monomer structure provided by the invention has a plurality of branched chains, the overall molecular weight is small, and the molecules are not easy to agglomerate.

The invention discloses a (methyl) acrylate monomer, a holographic recording medium, a preparation method and a related device.The structural formula of the (methyl) acrylate monomer is as shown in G1-G5. The preparation method is easy to operate and high in synthesis yield, and further, the holographic recording medium can be applied to holographic recording. The (methyl) acrylate monomer with the structure is introduced into the photopolymer type holographic recording medium, reverse migration of a short polymer chain can be effectively inhibited, and therefore the holographic recording medium with high sensitivity and high diffraction efficiency is obtained, and the invention further provides a preparation method of the holographic recording medium. The invention also provides a volume holographic grating, a holographic optical element and an optical device comprising the holographic recording medium.

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is shown as G1, G2, G3 and G4, R1 and R2 are respectively selected from one of H, C1-C10 alkyl and halogen, A1 is C1-C10 alkyl, R3 is hydrogen or methyl, and n is a positive integer selected from 1-10. The optical monomer provided by the invention has a (methyl) acrylate group with high refractive index and low volume shrinkage property, contains a plurality of aromatic rings with high molar refractive index and low molar volume, and also has sulfur atoms with relatively high molar refractive index, so that the whole molecule of the whole monomer has extremely high refractive index. The whole monomer structure in the invention has at least two functionalities, and can realize fast reaction; the monomer structure also contains more branched chains and carbon chains, and molecules are not easy to agglomerate and have a certain migration rate.

The invention relates to an optical monomer and a preparation method and application thereof, the structural general formula of the optical monomer is shown as G1, G2, G3, G4, G5 and G6, R1 represents hydrogen, phenyl, halogen and C1-C4 alkyl, and A1 represents C1-C4 alkyl or phenyl; r2 represents hydrogen or methyl; n is a positive integer selected from 1-10. The optical monomer provided by the invention contains a plurality of aromatic rings with high molar refractive index and low molar volume, and also contains sulfur atoms with relatively high molar refractive index, so that the whole molecule of the whole monomer is extremely high in refractive index. The monomer structure provided by the invention has a plurality of branched chains, the overall molecular weight is small, and the molecules are not easy to agglomerate.

The invention discloses an optical monomer and a preparation method thereof, a composition, a resin material and a preparation method thereof. The optical monomer provided by the invention comprises a quaternary carbon structure and a side chain connected with the quaternary carbon structure through an ester bond. The side chain comprises a thioether chain segment connected with an ester bond, an aromatic group connected with the thioether chain segment and an epoxy group connected with the thioether chain segment. The optical monomer provided by the embodiment of the invention takes a quaternary carbon structure as a core skeleton, and a side chain sequentially comprises an aromatic group, a thioether chain segment and a terminal epoxy group. A thioether structure with high polarizability and an aromatic group are introduced into the molecular design of the optical monomer, so that the refractive index and the optical transparency of a resin material are remarkably improved. And the rigidity of the epoxy aromatic ring is beneficial to improving the thermal stability and mechanical strength of the resin material. The epoxy group at the tail end can react with conventional epoxy resin to form a compact network structure, so that the stability of the resin material is improved, and the yellowing tendency is reduced.

This invention belongs to the field of chemical synthesis and relates to a method for achieving deuterated methylation of a nucleophile. The invention provides a deuterated methylating reagent, which is obtained by reacting formic acid with deuterated methanol under acidic conditions, followed by a second reaction with thiaanthracite and trifluoromethanesulfonic acid. The nucleophile is then reacted with the deuterated methylating reagent described in claim 1, a base, and a solvent to obtain the deuterated methylated product. This invention also provides a method for achieving deuterated methylation of a nucleophile, which involves dissolving the nucleophile and 5-deuterated methyl-5H-thiophene-5-onium trifluoromethanesulfonate in a suitable solvent, adding a base, and then performing the deuterated methylation reaction at room temperature. In the method provided by this invention, the yield of the product after nucleophile methylation can reach 52% to 95%.

The invention belongs to the technical field of synthesis and preparation of high-molecular optical materials, and particularly relates to a multi-mercaptothiol composition as well as a preparation method and application thereof. According to the present invention, the three-step synthesis route of the tetrahydroxymethylation reaction, the thiol precursor introduction and the deprotection is adopted, the reaction conditions are mild, the steps are clear, the yield is high, the complexity of the traditional synthesis route is avoided, the production cost is reduced, and the industrial production is easily achieved. In the aspect of refractive index regulation and control, the compound contains a plurality of sulfur atoms, the coating is endowed with the characteristic of high refractive index, accurate regulation of the refractive index can be realized by adjusting the formula of the composition, the requirements of different optical applications are met, and the application range of the material is widened. The prepared optical coating has excellent light transmittance, light loss can be reduced to the maximum extent, and the efficient performance of an optical device is ensured; meanwhile, the haze value of the coating is low, the light scattering phenomenon is effectively avoided, and the imaging definition and the precision of an optical system are guaranteed.

The invention discloses an optical monomer, a holographic recording medium, a preparation method and a related device, the structural general formula of the optical monomer is as shown in G1-G6, the monomer is high in refractive index, the preparation method is simple, and further, the optical monomer with the structure is introduced into the photopolymer type holographic recording medium, so that the photopolymer type holographic recording medium is prepared. The invention further provides a preparation method of the holographic recording medium, a volume holographic grating containing the holographic recording medium, a holographic optical element containing the holographic recording medium and an optical device containing the holographic recording medium.

The invention discloses a modified polymer cement-based normal-temperature foaming fireproof coating and a preparation method thereof, and relates to the technical field of fireproof coatings. The modified polymer cement-based normal-temperature foaming fireproof coating comprises a component A and a component B, the component A is prepared from the following raw materials in parts by weight: 15 to 20 parts of cement, 10 to 12 parts of calcium carbonate, 0.3 to 0.9 part of nano titanium dioxide, 30 to 35 parts of polyurethane emulsion, 1 to 2 parts of cross-linking agent, 8 to 12 parts of flame retardant, 1 to 3 parts of foaming agent, 0.5 to 1.5 parts of dispersing agent and 10 to 20 parts of deionized water; the component B comprises the following raw materials in parts by weight: 20-25 parts of a curing agent, 0.1-0.5 part of an organic zinc catalyst and 0.5-1.2 parts of a foam stabilizer; the prepared modified polymer cement-based normal-temperature foaming fireproof coating has excellent fireproof performance, bonding strength and compressive strength.

The application discloses a preparation method of perfluoroalkyl aryl sulfide, and a structural formula of the perfluoroalkyl aryl sulfide is shown as formula (I); the method comprises the following steps: firstly, obtaining corresponding aryl sulphenyl chloride by chlorination of thiophenol; under the condition that fluoride and crown ether exist, obtaining perfluoro-1,1-dimethylbutyl negative ion by addition of D-2 ‑ And the aryl sulphenyl chloride added is subjected to a nucleophilic substitution reaction to synthesize a product (1,1,1,3,3,4,4,5,5,5-decafluoro-2-trifluoromethylpent-2-yl)(aryl)sulfide. The application adopts a reaction strategy of efficient coupling of thiophenol and perfluoroalkyl, and can be used for preparing various fluorine-containing benzene sulfide compounds.

The invention provides a synthesis method of a thioether ligand and a palladium-catalyzed 2-aryl indole compound, and designs an application of the biphenyl thioether ligand and a palladium catalyst in preparation of the 2-aryl indole compound. Indole and arylboronic acid are subjected to a reaction under the action of a palladium catalyst and a biphenyl sulfide ligand, and the structural formula of the biphenyl sulfide ligand is shown in the specification. Ar is phenyl, furyl, thienyl, naphthyl or phenyl substituted by one or more substituent groups; r1 is methyl, methoxyl, fluorine atom, chlorine atom, bromine atom or methyl ester group; r2 is the same or different and is methyl, ethyl, isopropyl, isobutyl, cyclohexyl, benzyl, n-butyl or n-hexyl; r3 is alkoxy, alkylthio, substituted amino or halogen; the palladium catalyst is a divalent palladium compound.

The present application relates to a kind of preparation method of vicinal diol compound, which comprises the following steps: in non-aqueous solvent, formula (I) compound and reducing agent are reacted under light condition, to obtain the vicinal diol compound shown in formula (II);The reducing agent is formic acid or formate;The wavelength of the light is less than 390nm;Its reaction formula is as follows.The preparation method of the present application does not need transition metal catalyst, also does not need other special catalyst and special additive, and the aldehyde ketone substrate can be reacted with formic acid or formate in solvent by specific wavelength of light, to obtain corresponding vicinal diol compound with high yield, its reaction condition is mild, has wide substrate applicability, and green and environmental protection, simple and practical operation method, provides an effective synthesis strategy for the synthesis of shikimic alcohol compound.

The invention discloses a polyfunctional rosin-based reactive diluent. The structural formula of the polyfunctional rosin-based reactive diluent is shown as a formula (I) or a formula (II). The polyfunctional rosin-based reactive diluent has a rigid tricyclic diterpenoid structure of rosin, is small in molecular weight and low in viscosity, can be used for preparing an ultraviolet curing material, has excellent hardness and scratch resistance after light curing and film forming, and is simple in preparation method, low in cost and suitable for industrial production. And a polycarboxylic acid functional group is efficiently constructed under a mild condition.

The invention discloses a photocatalytic synthesis method of diethyl disulfide, and relates to the technical field of organic synthesis. The preparation method specifically comprises the following steps: mixing Co (NO3) 2.6 H2O and Ni (NO3) 2.6 H2O, and adding methanol to obtain a solution A; 2-methylimidazole and methyl alcohol are mixed, and a solution B is obtained; mixing the solution A and the solution B to obtain a zeolite imidazole framework material; selenium powder and the zeolite imidazole framework material are mixed and calcined, and a NiCoSe2 material is obtained; the preparation method comprises the following steps: mixing a NiCoSe2 material, ZnCl2, InCl3 and C2H5NS, adding an ethanol water solution, and carrying out microwave hydrothermal synthesis to obtain a NiCoSe2-coated ZnIn2S4 photocatalyst; the NiCoSe2-coated ZnIn2S4 photocatalyst and ethanethiol are subjected to a photocatalytic reaction under N2 atmosphere protection and visible light irradiation, and diethyl disulfide and hydrogen are generated. The method is mild in reaction condition and high in product stability.

The present application provides a method for preparing a deuterated chemical by means of a deuteration reaction of a carbon-hydrogen bond with a deuterium gas under the catalysis of an alkali, wherein in the presence of a catalyst, a deuterium gas is added into a compound containing a carbon-hydrogen bond for a deuteration reaction so as to generate a deuterated compound. A deuterium gas is used as a deuterium source, such that multiple water separation operations, tedious steps and the wasting of energy caused by usage of a large amount of deuterium oxide as a deuterium source are avoided. Moreover, a cheap and easily available alkali metal compound is used for replacing an expensive transition metal catalyst and a complex-structure ligand as a catalyst for a deuteration reaction, and the alkali metal compound has the advantages of a low cost, a good compatibility with functional groups of a substrate and a high deuteration rate. The present application provides a new, low-cost, green and efficient deuteration method, which has a high application value.

The application provides a Pd6(SR) 12 cluster with an octahedral structure, the Pd6(SR) 12 cluster is a cyclohexanethiol ligand-protected palladium cluster, contains 6 Pd atoms, 12 cyclohexanethiol ligands, the 6 Pd atoms form an octahedral core, and the sulfur atoms in the cyclohexanethiol ligands are connected with the Pd atoms peripherally, and each sulfur atom is connected with two Pd atoms. The application further discloses a preparation method of the Pd6(SR) 12 cluster, and the application fills the technical vacancy of synthesizing Pd clusters with structures other than a ring structure, and has high popularization value.

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The application discloses a full synthesis method of clethodim, and the method is characterized by reasonable selection / design of a process route, simplified process flow, reduced separation and purification operation, effectively reduced production cost and improved production efficiency, further improved yield of a key intermediate through research and screening of process conditions of the key step, reduced generation of impurities, and improved product quality and yield of the target product.

The present invention concerns the recovery of methionylmethionine from aqueous alkali ions containing media by intermediate formation of Bis(methionyl)-diketopiperazine.

The invention belongs to the technical field of organic synthesis. The invention particularly relates to a synthesis method of chiral beta-diaryl ethanol. The physiological activity, the pharmacological action and the material performance of the chiral molecule are directly determined by the spatial configuration of the chiral molecule. Therefore, efficient construction of chiral compounds is always the core research direction of organic synthesis and medicinal chemistry. Wherein the chiral beta-diaryl ethanol is a kind of key intermediates with irreplaceable application value. According to the invention, the Suzuki-Miyaura type asymmetric ring-opening coupling reaction of nickel catalyzed aryl epoxy and aryl boric acid with high stereoselectivity is realized, and the asymmetric ring-opening coupling reaction is used for synthesizing chiral beta-diaryl alcohol compounds. The method is wide in substrate compatibility and raw material source, mild in reaction condition, free of exogenous alkali and convenient to operate. An aryl epoxy compound and arylboronic acid are used as raw materials, diethylene glycol dimethyl ether nickel bromide is used as a catalyst, chiral biimidazoline is used as a ligand, under the promotion of sodium iodide, reaction is performed in an ethanol solvent according to the following reaction formula at the temperature of 50 DEG C for 10 hours, and the chiral beta-diaryl ethanol compound with the high ee value is obtained.

The application belongs to the technical field of electrolyte solvent synthesis and application, and discloses a fluorosulfone ether compound, a preparation method thereof and a sodium ion battery electrolyte. The structural general formula of the fluorosulfone ether compound is R'-O-L-SO2-R; wherein R' and R are respectively selected from C1-C6 alkyl; and L is a fluorinated alkylene group with a carbon atom number greater than or equal to 2. The fluorosulfone ether compound of the application can be applied to the sodium ion battery electrolyte, so that the high-voltage stability, low-temperature stability and interface stability of the electrolyte can be significantly improved.

The present application belongs to the technical field of condensate, and particularly relates to a non-peptide small molecule condensate and preparation and application thereof. The present application provides a non-peptide small molecule condensate which is prepared by taking a small molecule shown in formula I as a precursor, wherein Y and Z are each independently NH, O or S, R = or X = O or S; R1 and R2 are each independently selected from H, C 3‑20 alkyl, -C 1‑8 alkylene-phenyl, -C 1‑8 alkylene-5-10-membered heteroaryl, -C 1‑8 alkylene-S-C 1‑8 alkyl, -C 1‑8 alkylene-SH, -C 1‑8 alkylene-O-C 1‑8 alkyl or -C 1‑8 alkylene-NH-C 1‑8 alkyl; and R1 and R2 are not H at the same time. The obtained condensate not only has good spontaneous non-classical fluorescence characteristics, but also has the abilities of drug loading and controllable release, and shows excellent resistance to enzymatic hydrolysis and good biocompatibility. Formula I

The invention relates to a process for preparing 1,2′-benzisothiazoline-3-one according to formula (I), comprising the following steps: (a) reacting a 2-halogenbenzonitrile compound of general formula (II) with a reaction mixture, containing: (i) alkaline sulphide and / or alkaline hydrogen sulphide and (ii) an alkyl halide compound, represented by general formula (III): R1X (III) for producing an intermediate product of general formula (IV), and (b) reacting the intermediate product of general formula (V) obtained in step (a) with a halogenating agent or an oxidant and subsequent reaction of the 2-(alkylsulfoxy)benzonitrile with an acid to form 1,2-benzisothiazoline-3-one as well as a halide compound of general formula (V) R1X (V).

The invention discloses a preparation method of trifluoromethyl sulfide, which comprises the step of reacting a trifluoromethyl reagent with sulfur in a polar aprotic solvent in the presence of fluoride to obtain the trifluoromethyl sulfide. The reaction conditions are mild, and trifluoromethyl sulfide can be prepared through one-step reaction.

The invention provides a preparation method of 2-acrylic acid 2-(2-naphthalenethio) ethyl ester, which comprises the following steps: (1) adding 2-thionaphthol, a first reactant and a catalyst into a first solvent, reacting at 110-140 DEG C for 4-10 hours, and washing with water to obtain 2-naphthyl sulfide ethanol; and (2) adding 2-naphthyl sulfide ethanol and a reaction aid into a second solvent, dropwise adding a second reactant, and reacting at 0-30 DEG C for 2-10 hours to obtain the 2-naphthyl sulfide ethanol, wherein the first reactant is 2-halogenated ethanol, ethylene oxide or ethylene carbonate and derivatives thereof; the second reactant is acryloyl chloride, alpha-methacryloyl chloride or a mixture of acrylic acid and phosphorus oxychloride. The preparation process is safe and simple, the cost is low, the reaction conditions are mild, the reaction polymerization can be effectively controlled, the post-treatment flow is simple, and industrialization is easy.

This invention belongs to the field of fluorochemical technology, specifically relating to a method for the photocatalytic synthesis of trifluoromethanesulfonic acid. The method for photocatalytic synthesis of trifluoromethanesulfonic acid described in this invention involves: firstly, dissolving 4-fluorothiophenol, a trifluoromethyl source, and a photocatalyst in a solvent, and catalyzing the reaction under visible light at room temperature. The reaction solution is then treated to obtain the intermediate 4-fluorotrifluoromethylthiobenzene. Next, the intermediate 4-fluorotrifluoromethylthiobenzene is mixed with formic acid and hydrogen peroxide, and oxidized at 40°C. After quenching, extraction, and purification, solid 4-fluorotrifluoromethyl sulfone is obtained. Finally, 4-fluorotrifluoromethyl sulfone is mixed with concentrated sulfuric acid for hydrolysis. The resulting reaction solution is quenched and then treated to obtain trifluoromethanesulfonic acid. The photocatalytic synthesis method for trifluoromethanesulfonic acid provided by this invention uses safe raw materials, operates under mild reaction conditions, has simple steps, and is environmentally friendly.

The polythiol composition according to an exemplary embodiment includes a tetrafunctional polythiol compound and a parapolythiol compound, the parapolythiol compound comprising C 13 H 28 S9 represents compounds and compounds derived from C 15 H 32 S 10 The compounds are indicated. The proportion of parapolythiol compounds, as measured by high-performance liquid chromatography (HPLC), ranges from 1% to 5%. By adjusting the content of parapolythiol compounds, optical products with excellent transmittance and optical properties can be manufactured.

To provide a method of treating a hydrocarbon-containing reservoir and a surfactant composition used for the treatment.SOLUTION: The method involves introducing a surfactant composition into a hydrocarbon-containing reservoir. The surfactant composition includes an alpha olefin sulfonate or an isomerized olefin sulfonate. The alpha olefin sulfonate or the isomerized olefin sulfonate is synthesized by i) oligomerizing a monomer comprising a C3 to C6 mono-olefin to form an oligomerization product and ii) sulfonating the oligomerization product.SELECTED DRAWING: None

The utility model relates to vulcanized isobutene production technical field, specifically is a kind of vulcanized isobutene production sulfur-containing wastewater recycling system, the bottom of high-pressure reaction kettle is connected with first conveying pipe respectively by tee joint, the first conveying pipe is connected with first dechlorination kettle, the first dechlorination kettle bottom discharge end is connected with second conveying pipe respectively by tee joint, the second conveying pipe is connected with second dechlorination kettle, the second dechlorination kettle bottom is connected with third conveying pipe respectively by tee joint, the third conveying pipe is connected with wastewater transfer tank, the wastewater transfer tank discharge end is connected with the first dechlorination kettle by circulation pipe.The utility model is dechlorinated by setting two dechlorination kettle, sodium sulfide can replace the chlorine that is not replaced in primary dechlorination reaction when secondary dechlorination, sulfur-containing wastewater is collected using wastewater transfer tank, then it is recycled to the next batch primary dechlorination reaction, realize the recycling of sulfur-containing wastewater, can reduce the wastewater treatment pressure of producer.

This disclosure provides a method for preparing sulfidated alkylphenol salt products to achieve a high sulfidation ratio of sulfidated alkylphenol salt to unsulfidated alkylphenol salt / phenol in the context of neutralization and optional over-alkaliening additives. The sulfidated alkylphenol salt products are obtained by sulfidating alkylphenols with a sulfur chloride blend comprising about 40% to about 75% by weight of sulfur dichloride.