100 results about "Thiophenate" patented technology

The present invention discloses a sulfur-nitrogen co-doped graphene hollow nanosphere and its preparation and application, belonging to the technical field of graphene nanomaterials. During the preparation, a mixture of thiourea and zinc powder is first calcined under the protection of an inert gas, and then H2O and HCl are added to the calcined product and heated for reaction, followed by post-processing to obtain the target product. The resulting product is a sulfur-nitrogen co-doped graphene material, which presents a hollow spherical morphology. This material has a large specific surface area and pore volume, and both the nitrogen and sulfur doping amounts have reached a high level. It has been verified that the obtained high-sulfur-nitrogen co-doped graphene hollow nanospheres have unique graphite nitrogen-pyridine nitrogen-thiophene sulfur synergistic active sites, which have high atomic utilization and high stability, and exhibit the best performance of activating persulfate to degrade organic matter. It can continuously and rapidly separate organic pollutants in actual water bodies and exhibit excellent stability.

The invention relates to a method for preparing bio-based isosorbide dimethyl ether through resin catalysis, and belongs to the technical field of organic synthesis. Adding corn starch into a sulfuric acid solution, hydrolyzing into glucose, and filtering to obtain a glucose solution; adding a solid acid catalyst into the concentrated glucose solution, and filtering after reaction; carrying out reduced pressure distillation on the filtrate to obtain an isosorbide crude product, and purifying through recrystallization; the preparation method comprises the following steps: adding isosorbide, a methylation reagent and a basic catalyst into a reaction kettle, stirring for reaction, cooling and filtering; and distilling the filtrate, and collecting fractions to obtain high-purity isosorbide dimethyl ether. The solid acid catalyst is sorbic acid based styryl macroporous cation exchange resin; the styryl macroporous cation exchange resin is soaked in sulfuric acid to be activated and then is mixed with sorbic acid chloride, 2-thiophenecarbonyl chloride and zinc chloride to react, and then washing and drying are performed to prepare the solid acid catalyst; the isosorbide dimethyl ether prepared by the method disclosed by the invention is high in purity and relatively high in yield.

The invention discloses transparent resin as well as a preparation method and application thereof, and belongs to the technical field of polyester synthesis and application and development of polyester materials. The preparation method comprises the following steps: sequentially carrying out esterification reaction and polycondensation reaction on a mixture containing dibasic acid, dihydric alcohol, a catalyst and a stabilizer to obtain transparent resin; the binary acid is selected from at least one of terephthalic acid, 2, 5-furandicarboxylic acid and 2, 5-thiophenedicarboxylic acid; the dihydric alcohol is selected from at least two of ethylene glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, isosorbide and 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol, and the dihydric alcohol is selected from at least two of ethylene glycol, 1, 4-butanediol, 1, 4-cyclohexanedimethanol, isosorbide and 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol; the catalyst is selected from defect-state nano titanium dioxide; and the stabilizer is selected from triphenyl phosphate. By using the combination of the defect-state nano titanium dioxide catalyst and the triphenyl phosphate stabilizer, the polymerization reaction can be completed with high activity and low time consumption, and meanwhile, good transparency, excellent color, low ash content and excellent thermodynamic property of the product are kept.

Methods for controlling and / or suppressing Poa annua (annual bluegrass) in a stand of warm season turfgrass are provided. In certain aspects, the methods may include contacting a stand of warm season turfgrass comprising Poa annua with an herbicidally effective amount of thiencarbazone-methyl when the Poa annua is in an early post-emergence growth state or during an early post-emergence period of time.

The invention belongs to the technical field of biological medicine, and particularly discloses application of tea polyphenol combined with meropenem to preparation of a medicine for resisting carbapenem drug-resistant bacteria, and the carbapenem drug-resistant bacteria are animal source blaNDM-5 positive escherichia coli and / or klebsiella pneumoniae. A trace bouillon chessboard method, a cefoxitin hydrolysis test, a time-sterilization curve, a greater wax moth infection model and the like prove that the tea polyphenol and carbapenem antibiotic meropenem generate a good synergistic antibacterial effect, and the tea polyphenol can also inhibit the activity of NDM-5 enzyme; meanwhile, the treatment and protection effects of meropenem on a greater wax moth infection model are improved. It is found for the first time that tea polyphenol can reverse the drug resistance of carbapenem drug-resistant bacteria to meropenem and enhance the antibacterial activity of meropenem to carbapenem drug-resistant bacteria, the synergistic effect is remarkable, use is easy, popularization is easy, and good application value is achieved.

The present application provides a kind of herbicidal composition comprising trifluralin, acetochlor and thifensulfuron-methyl, active ingredients comprising trifluralin, acetochlor and thifensulfuron-methyl, and the mass ratio of trifluralin, acetochlor and thifensulfuron-methyl is 10-30:20-40:0.5-2.The herbicidal composition of the present application can be used for the control of annual weeds in crop fields, and has a significant synergistic effect.

The invention provides a photoactive layer conjugated polymer donor, a preparation method and application thereof, and a semitransparent solar cell device, and belongs to the technical field of organic synthesis. The invention provides a conjugated polymer donor for a photoactive layer, which takes thiophene as a skeleton, enhances the solubility by a long alkyl chain group, belongs to a narrow-band gap donor, is large in weight-average molecular weight, is high in viscosity of the conjugated polymer donor for the photoactive layer, and can be used for preparing an active layer with the same thickness. The conjugated polymer donor of the high-molecular-weight optical active layer can use a lower-concentration solution, so that the material loss of the active layer is reduced, the difficulty and time of proportioning are reduced, the process cost is reduced, the large-scale mass production and industrialization of OPV are facilitated, and the method has huge application potential in semitransparent organic solar cell devices.

The invention belongs to the technical field of environmental microorganisms, and provides Klebsiella capable of degrading thifensulfuron methyl and simultaneously promoting plant growth, the Latin of the Klebsiella is Klebsiella sp., the preservation name is Klebsiella sp. HDJY-1, the preservation place is China Center for Type Culture Collection, the preservation date is November 17, 2025, and the preservation number is CCTCC NO: M 20252578. The strain has excellent low temperature resistance and alkali resistance, not only can grow and propagate by taking thifensulfuron methyl as a unique carbon source and energy, but also can secrete plant growth-promoting substances such as indoleacetic acid and the like, and has a nitrogen fixation function. Therefore, the strain provided by the invention not only can remarkably promote plant growth and improve nutrient absorption efficiency so as to improve plant biomass and agricultural product quality, but also can provide an excellent strain resource for thifensulfuron methyl pollution remediation of farmland soil.

The present application provides a novel structure of thiophene compound, the compound has significant inhibitory effect on spore germination and appressorium formation of various plant pathogenic fungi and oomycetes (such as Pyricularia oryzae, Colletotrichum gloeosporioides, Gibberella, Phytophthora, Phytophthora capsici), which can be used for preventing and treating plant diseases caused by fungi and / or oomycetes.

The present invention relates to an emulsion formulation comprising thiencarbazone-methyl or a pesticide-acceptable salt thereof, one or more organic water-immiscible solvents, one or more organic water-miscible solvents selected from linear and cyclic carbamate esters, one or more emulsifiers, and one or more organic bases, wherein the formulation exhibits a pH of 5.5 to 9.

The invention relates to a metal anti-corrosion cleaning agent, a preparation method and application, and the metal anti-corrosion cleaning agent comprises the following components in parts by weight: 0.001-0.06 part of a composite functional agent; 0.1 to 3 parts of a pH regulator; 0.01 to 1 part of inorganic acid; 50-80 parts of an organic solvent; and 20-50 parts of ultrapure water. The thienyl carboxylic ester derivative and the alkanol derivative are combined, the thienyl carboxylic ester derivative removes metal ions (such as Cu < + > and Fe < + >) in a targeted mode by means of the strong chelating capacity of ester groups, and organic pollutants are stripped through the pi-pi effect; the alkanol derivative wraps non-polar residual gum by using a long-chain hydrophobic end, and a hydrophilic end enhances the wettability of a solution, so that full-coverage cleaning of a nano-scale structure is realized.

The application provides a fermented vegetable oil and a preparation method thereof. The preparation method comprises the following steps: crushing a vegetable oil raw material and mixing the same with water to obtain a raw material solution; adding a biological enzyme to the raw material solution to perform enzymolysis, and after enzyme inactivation, an enzymolysis product is obtained; then, a fermentation bacteria is added to perform fermentation, sterilization and centrifugation to obtain an oily liquid; the oily liquid, 1,2-dilauroylphosphatidyl ethanolamine, a self-assembled structure regulator and propylene glycol are uniformly mixed, and then added into water to obtain a liposome suspension of the fermented vegetable oil; 3-thiophene malonic acid and / or flower acid are first added into the liposome suspension of the fermented vegetable oil, and then heparan sulfate and calcium chloride are added, and after reaction, the fermented vegetable oil encapsulated in a carrier is obtained. The preparation method of the fermented vegetable oil has good long-term stability, and can also improve the poor compatibility of the fermented vegetable oil with a water-based system.

The application discloses a kind of heterogeneous methylation reagent and preparation method thereof, it is related to organic synthesis technical field.The preparation method of heterogeneous methylation reagent provided by the application, the heterogeneous methylation reagent is heterogeneous aryl sulfide type methylation reagent or heterogeneous aryl sulfide type deuteromethylation reagent, this preparation method is based on the synthesis method of superhigh crosslinking polymer, by aryl sulfide compound with thianthrene as representative is polymerized, the reactivity of material obtained after polymerization still retains monomer, can repeatedly cycle and carry out methylation or deuteromethylation, reach almost 100% atomic utilization efficiency.The traditional homogeneous sulfur methyl methylation reagent such as (DMTT) will produce dibenzothiophene by-product after reaction, and it is very difficult to separate and purify methylated product, and the methylation reagent of heterogeneous of the application only needs simple centrifugation or suction filtration step to realize the separation of product and methylation reagent, greatly improve synthesis efficiency.

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a pyrimidine and thienopyrimidine derivative, a preparation method and application thereof. The pyrimidine derivative in the application is a compound with the structure of formula I, and the thienopyrimidine derivative is a compound with the structure of formula II. The pyrimidine and thienopyrimidine derivative can be used as an AcrB efflux pump inhibitor, and can significantly enhance the antibacterial activity when combined with an antibacterial drug. The Nile red experiment shows that the compound 64c can completely inhibit the AcrB-mediated efflux at a concentration of 50 μM, and the effect is better than that of the positive control PA beta N. The compound in the application has novel structure and excellent activity, and can be used for preparing an AcrB efflux pump inhibitor for reversing bacterial drug resistance and an antibacterial sensitizing drug.

The application belongs to the technical field of near-infrared luminescence and ultrasonic treatment materials, discloses a kind of activatable acoustic power nano materials based on conjugated polymer and its preparation method and application, comprising the following steps: 2,6-di (trimethyl tin) -4,4-di (2-ethylhexyl) -dithiophene and cyclopentadiene, 4,7-dibromo-5,6-dinitrobenzo [c] [1,2,5] thiazole, catalyst tetra (triphenylphosphine) palladium are added into reaction tube, toluene is added, and the reaction product is settled with methanol under nitrogen protection, to obtain conjugated polymer;Degradable mesoporous silica is used to wrap to realize the water-soluble of molecule, and the corresponding activatable acoustic treatment reagent is obtained.The material disclosed in the application can be used for activatable acoustic dynamics treatment guided by near-infrared two-zone imaging, which helps to improve the specificity of tumor treatment, and mesoporous silica wrapping can also be used for drug loading and transport.

The invention discloses a degradable environment-friendly fiber and a preparation method thereof, and relates to the field of fibers. When the degradable environment-friendly fiber is prepared, triethyl phosphite firstly reacts with 3-(2-bromoethyl) thiophene and then reacts with dimethyl terephthalate and ethylene glycol, and modified polyester is prepared; the preparation method comprises the following steps: enabling chitosan oligosaccharide to react with 4-hydroxy-3-pyridylaldehyde, thionyl chloride and 2-(dimethylaminomethyl) thiophene in sequence, so as to prepare functionalized chitosan oligosaccharide; mixing the functionalized chitosan oligosaccharide, zinc acetate and modified polyester, and performing melt spinning to obtain composite fibers; mixing thiophene, ferric chloride and trichloromethane to prepare a thiophene solution; and immersing the composite fiber in a thiophene solution, and drying to obtain the degradable environment-friendly fiber. The degradable environment-friendly fiber prepared by the invention has excellent flame retardance, antibacterial property, antistatic property and light aging resistance.

The application provides a herbicide composition for preventing and treating cyperus iria, a preparation method and application thereof, and aims to solve the technical problem of lacking effective and controllable herbicide for cyperus iria and various monocotyledonous and dicotyledonous weeds in the field. The herbicide composition is composed of effective components and necessary adjuvants, wherein the effective components are composed of atrazine, halosulfuron, thifensulfuron-methyl and fluroxypyr according to a weight ratio of 9.0-54.0:0.75-3.0:0.75-3.8:1.5-6.5. The herbicide composition has rapid and effective prevention and control effects on common annual grass weeds and broadleaf weeds in the millet field, and can eradicate the malignant weed cyperus iria. The herbicide composition is safe to the millet, and can also play a certain role in controlling the growth of the millet, reduce the plant height of the millet, reduce the risk of lodging of the millet, and improve the yield of the millet.

The invention discloses an antibacterial and anti-static turnover tray which is formed by compounding a base layer, an antibacterial and anti-static functional layer and a surface protective coating, each layer is composed of the following materials in parts by mass; the base layer material is prepared from 80 to 100 parts of modified high-density polyethylene; the antibacterial and antistatic functional layer is prepared from the following materials in parts by weight: 30-40 parts of polystyrene-butadiene-styrene block copolymer, 10-15 parts of silver-loaded zeolite antibacterial agent, 5-8 parts of polythiophene conductive polymer, 5-8 parts of compatibilizer and 1-2 parts of calcium stearate lubricant; the surface protection coating material is prepared from 20 to 30 parts of waterborne polyurethane emulsion. The formula is improved, and the silver-loaded zeolite antibacterial agent and the polythiophene conductive polymer are introduced, so that the turnover tray is good in durability and has antibacterial and antistatic functions.

Disclosed herein are apyrase inhibitors of Formula (I): (I). Also disclosed herein are methods for using the disclosed inhibitors, including in methods for protecting crops from pests. In one aspect the apyrase inhibitors are useful for enhancing the activity of pesticides for the protection of crops from pathogens and to support crop yield.

The application relates to the technical field of platinum recovery, and particularly discloses a method for purifying and recovering platinum. The method for purifying and recovering platinum comprises the following steps: extracting chloroplatinate ions from a liquid to be purified by using an organic extractant, the liquid to be purified being an aqueous solution in which platinum exists in the form of chloroplatinate ions, and separating an organic phase; the organic extractant is obtained by dispersing 2-(thiophenylmethyl) diethyl phosphonate in methyltrioctylammonium chloride; reacting the chloroplatinate ions in the organic phase with an aqueous reagent, separating the organic phase and the aqueous phase, back-extracting platinum into the aqueous phase, and separating the aqueous phase; adding a reagent to the aqueous phase to convert the platinum into a precipitate; separating the precipitate, and calcining to obtain elemental platinum. The methyltrioctylammonium chloride and 2-(thiophenylmethyl) diethyl phosphonate synergistically extract the chloroplatinate ions with high selectivity, have extremely high extraction capacity, reduce the amount of the organic extractant, and reduce the pressure of subsequent treatment of the organic extractant.

The invention discloses a trithiophene type fluorescent probe for detecting total polar substances of edible oil as well as a preparation method and application of the trithiophene type fluorescent probe. The preparation method comprises the following steps: directly carrying out a coupling reaction on 4-bis (4-methoxyphenyl) amino] phenyl]-[2, 2 ': 5', 2 ''-trithiophene-5-formaldehyde and 4-bis (4-methoxyphenyl) aminophenylboronic acid to prepare 5''-[4-[bis (4-methoxyphenyl) amino] phenyl]-[2, 2 ': 5', 2 ''-trithiophene-5-formaldehyde, and reacting the compound with 4-methylquinoline to synthesize the probe (E)-4-methoxy-N-(4-methoxyphenyl)-N-[4-(5''-(2-(quinoline-4-yl) vinyl)-[2, 2 ': 5', 2 ''-trithiophene-5-formaldehyde. The compound can selectively detect the polarity of edible oil, yellow fluorescence is quenched after the polarity of the edible oil is increased, and the compound can be used as a fluorescent probe for detecting the polarity of the edible oil.

The application discloses a kind of twelve-hole polyester staple fiber and preparation method thereof, it is related to polyester technical field.The application first 3-thiophene isocyanate is reacted with phenol to obtain thiophene group blocked isocyanate;Carbon nanotube is carboxylated with sulfuric acid and nitric acid, then reacted with 3-aminothiophene to obtain thiophene group carbon nanotube, thiophene, thiophene group blocked isocyanate is oxidized and polymerized on the surface of thiophene group carbon nanotube to obtain polythiophene carbon nanotube;N, N-dimethyl-n-octylamine is reacted with epichlorohydrin to obtain functional diol;Ethylene glycol, terephthalic acid, 2-vinyl terephthalic acid and functional diol are prepared into pre-modified polyester by polycondensation;Pre-modified polyester is reacted with methoxypolyethylene glycol mercapto to obtain modified polyester;Modified polyester and polythiophene carbon nanotube are melt spun to obtain finished fiber.The twelve-hole polyester staple fiber prepared by the application has the effects of antibacterial, moisture absorption, antistatic and good mechanical properties.

The invention discloses a carbonyl reductase directional modification method for synthesis of atorvastatin intermediates, which belongs to the technical field of enzyme gene engineering, and is characterized in that carbonyl reductase genes are used as templates, mutation primer pairs are designed, double-site mutation is carried out by adopting an overlapping extension PCR (polymerase chain reaction) method, escherichia coli is transformed, IPTG (isopropyl-beta-d-thiogalactoside) is used for inducing expression, and mutant carbonyl reductase is prepared. The K205D / R237W double mutation modified carbonyl reductase improves the enzyme activity, combines the synergistic effect of the thiophene pyridine coenzyme analogue, improves the conversion rate of the atorvastatin intermediate and the product purity, is significantly superior to the traditional chemical reduction method, avoids the low-temperature and high-pressure conditions of the traditional chemical method, reduces the energy consumption, and is suitable for industrial production. The use amount of an organic solvent and the generation amount of byproducts are reduced, and the generation amount of wastewater is reduced.

This invention provides a cyan-transparent electrochromic polymer, its preparation method, and its applications, belonging to the field of electrochromic polymer technology. The invention uses 6,6'-(2,6-dibromo-4H-cyclopentano[2,1-b:3,4-b']dithiophene-4,4-diyl)bis(hexyl-1-ol), 2,6-di(trimethyltin)-4,4-di(2-ethylhexyl)-dithiophenecyclopentadiene, and 4,7-dibromobenzo[c][1,2,5]thiadiazole as main raw materials, reacting them under the action of a catalyst to obtain a cyan-transparent electrochromic polymer. The film made from the cyan-transparent electrochromic polymer of this invention has an optical contrast ratio of 47.01% in the 719 nm wavelength range, a coloring time of 0.81 s, and a fading time of 0.32 s.

The present application provides a method for electro-synthesis of a thiophene-based conductive polymer film in an aqueous solution and application of the film, which comprises electrochemical synthesis of a conductive polymer film in an aqueous solution and metallization of the film. Traditional preparation methods of a thiophene-based conductive polymer film have poor solubility of polymer monomers, and thus the monomers need to be modified or dissolved in special organic solvents. The use of organic solvents not only pollutes the environment, but also limits the universality of the preparation of the polymer film to some extent and affects its large-scale application. The present application provides a method for electro-synthesis of a thiophene-based conductive polymer film in an aqueous solution, which uses an aqueous electrolyte solution with low price and almost no pollution to the environment, and can quickly prepare a thiophene-based conductive polymer film with high quality and high stability. Further metallization modification of the film can be applied to various electronic product fields, especially flexible and wearable electronic information products.

The invention belongs to the technical field of medicines, and particularly relates to application of a tetrahydrothieno [2, 3-c] pyridine compound and a derivative of the tetrahydrothieno [2, 3-c] pyridine compound. The compound provided by the invention has a structure as shown in a formula I, wherein R1 and R2 are independently selected from hydrogen and substituted or unsubstituted C1-C4 alkyl; and R3 is independently selected from a substituted or unsubstituted five-membered aromatic heterocyclic ring. The anti-candida albicans activity of the tetrahydrothieno [2, 3-c] pyridine compound and the pharmaceutically available salt provided by the invention is found for the first time, and the tetrahydrothieno [2, 3-c] pyridine compound and the pharmaceutically available salt can be used for clinically treating fungi such as candida albicans, and can effectively solve the problem of fungus drug resistance.

The invention discloses a mattress material based on modified fibers and a preparation method of the mattress material. The mattress material comprises nylon 66 fibers, low-melting-point fibers and the modified fibers. The low-melting-point fiber is ES bi-component parallel composite fiber composed of polypropylene and polyethylene, and the modified fiber is prepared by mixing a modified polymer and a modified filler to prepare a spinning solution and then carrying out electrostatic spinning and ultraviolet irradiation. Molecular chains of the modified polymer contain rich furan rings and thiophene rings, synthesis of bacterial cell walls can be destroyed, the furan is grafted with oximido, and a formed furan oxime ester unit can generate highly unstable and reactive free radicals, so that metal ions in cells are unbalanced to cause change of cell metabolism homeostasis. The lysozyme fixed on the modified filler can be hydrolyzed to form peptidoglycan of bacterial cell walls, so that the cell walls are broken, and the material has good antibacterial performance.

The present invention discloses a nano-ceramic microsphere thermal insulation material and a preparation method thereof, which relates to the field of thermal insulation materials and includes the following raw materials: silicone-acrylic emulsion, styrene-acrylic emulsion, modified nano-ceramic microspheres, silica aerogel, talc powder, dispersant, thickener, flame retardant and water. Among the flame retardants used in the present invention, sodium lignosulfonate, phosphate ester and amino group with reduced hydrophilicity cooperate to provide flame retardancy, endowing the thermal insulation material with strong waterproof and fireproof properties. The modified nano-ceramic microspheres used in the present invention, in combination with talc powder, endow the thermal insulation material with strong thermal insulation properties by using nano-ceramic microspheres with improved agglomeration. At the same time, a large conjugated system formed by the reaction of 6-(thiophen-2-yl)-1H-indazole and 2-methoxy-5-nitro-2,4,6-cycloheptatriene-1-one endows the thermal insulation material with strong anti-aging properties.

The present invention relates to an herbicide tolerance protein, an encoding gene thereof and use thereof, the herbicide tolerance protein comprising: a protein (a) having an amino acid sequence as shown in SEQ ID NO: 1, and having an alanine substitution at least at position 176 and / or having a valine substitution at position 178 of SEQ ID NO: 1; or (b) having an amino acid sequence as shown in SEQ ID NO: 3; or (c) having an amino acid sequence as shown in SEQ ID NO: 5; or (d) having an amino acid sequence as shown in SEQ ID NO: 7; or (e) being derived from (a) by means of the amino acid sequence of (a) undergoing substitution and / or deletion and / or by added one or several amino acids, and having the activity of thifensulfuron hydrolase. The herbicide tolerance protein of the present invention has a broad application prospects in plants.

The invention provides an electrochromic polymer containing a thiophene embedded unit. The electrochromic polymer is prepared from the following components in parts by weight: 5 to 10 parts of 5-dibromo, 10 to 15 parts of 4-dialkoxy methyl propylene dioxythiophene, 5 to 10 parts of 4-dicyanothiophene and 3 to 5 parts of 0.006 mmol palladium acetate. The invention provides an electrochromic polymer containing a thiophene embedded unit and a preparation method of the electrochromic polymer. The electrochromic polymer is prepared from the following raw materials in parts by weight: 10-15 parts of 3, 4-dialkoxy methyl propylene dioxythiophene, 5-10 parts of 4-dicyanothiophene, 3-5 parts of 0.006 mmol of palladium acetate, 5-8 parts of 0.3 mmol of potassium carbonate, 15-30 parts of 0.03 mmol of pivalic acid, 1 part of hydrogen atom, 3 parts of halogen atom, 2 parts of hydroxyl, 2 parts of carboxyl, 1 part of ester group or linear or branched alkyl with 1-20 carbon atoms, so that the electrochromic polymer has the characteristics of low driving voltage, high optical contrast, high stability, low cost and the like. Meanwhile, two parts of precipitates are poured into a stirring device, an isopropanol solution is added into the stirring device to be stirred, filtering is conducted, and the production period is shortened.