33 results about "Acetonitrile" patented technology

The present invention relates to a hydroxyacetonitrile production method and production system based on a carbon fiber off-gas. The carbon fiber off-gas comprises a carbonization off-gas. The hydroxyacetonitrile production method comprises the following steps: subjecting the carbonization off-gas to de-tarring treatment and de-ammoniation treatment to obtain a treated off-gas; and performing a nucleophilic addition reaction between the treated off-gas and formaldehyde in the presence of a catalyst to obtain the hydroxyacetonitrile. By subjecting the carbonization off-gas to de-tarring treatment and de-ammoniation treatment and performing a nucleophilic addition reaction between the treated off-gas and formaldehyde in the presence of the catalyst to obtain the hydroxyacetonitrile, the present invention can significantly reduce the contents of hydrogen cyanide and ammonia gas in the off-gas, and the treated off-gas can meet emission standards. In addition, using the carbon fiber off-gas as a starting material to produce hydroxyacetonitrile can also be achieved, thereby leading to improved resource utilization rate and economic benefits.

The invention relates to a preparation method of aldehyde group functionalized halogen-containing helicene, which comprises the following steps: S1, dissolving terephthalaldehyde and p-halobenzyl cyanide in ethanol, adding sodium ethoxide into the solution for reaction, and washing, filtering and drying a reaction product to obtain a solid A; s2, dissolving the solid A in methylbenzene, then adding iodine and epoxypropane for reaction, and washing, filtering and drying a reaction product to obtain a solid B; s3, dissolving the solid B in dichloromethane, adding n-butyllithium into the dichloromethane, sequentially and slowly adding methanol, water and hydrochloric acid after the color of the solution is changed, extracting an organic filtrate after the reaction is completed, carrying out rotary evaporation on the organic filtrate, washing, filtering and drying to obtain aldehyde group functionalized halogen-containing helicene; the invention provides the aldehyde group functionalized halogen-containing helicene and the preparation method thereof, the method is simple to operate, the reaction is simple and convenient, the expansion is flexible, the aldehyde group is successfully introduced into the compound, the reaction steps are reduced, and the experiment complexity is reduced.

The invention belongs to the technical field of pharmaceutical analysis, and provides a method for detecting related impurities of EvoCASE, which comprises the following steps: precisely weighing EvoCASE, and diluting with a mobile phase A as a solvent to obtain a test solution; precisely measuring the test solution obtained in the step S1, and diluting with the mobile phase A as a solvent to obtain a contrast solution; weighing evocamide and various impurity reference substances, and diluting by taking the mobile phase A as a solvent to obtain a system applicable solution; carrying out liquid chromatography detection, and calculating the content of each impurity in the to-be-detected EvoCassette; chromatographic conditions are as follows: a chromatographic column adopts octadecylsilane chemically bonded silica as a filler; the mobile phase A and the mobile phase B are mixed liquid of buffer salt, methanol and acetonitrile. The method provided by the invention can be used for simultaneously separating and detecting various impurities in the Evocamide, has the characteristics of simplicity in operation and high sensitivity, is high in chromatographic peak separation degree, does not interfere with each other, is good in peak shape, can be used for detecting related impurities in the Evocamide and a preparation thereof, and ensures the medication safety of the Evocamide and the preparation thereof.

The invention provides a liquid chromatography detection method and a quantitative determination method for volatile carbonyl compounds in cigarette smoke. The liquid chromatography detection method is based on a DNPH compound special chromatographic column and gradient elution, adopts a mobile phase composed of water and acetonitrile in a volume ratio of 1: 1-1: 9, and realizes the determination of n-butyraldehyde and isobutyraldehyde in the cigarette smoke as well as the determination of n-butyraldehyde and isobutyraldehyde and other 7 carbonyl compounds required to be determined in ISO 21160 and YC / T 254-2008 standards for the first time. The volatile carbonyl compounds such as formaldehyde, acetaldehyde, acetone, acrolein, propionaldehyde, crotonaldehyde, 2-butanone and the like are effectively separated, and the effective separation of the volatile carbonyl compounds and other interferents in the smoke is further realized. The invention further provides a quantitative determination method for volatile carbonyl compounds in cigarette smoke, a liquid chromatography-ultraviolet analysis method is adopted, the liquid chromatography is the liquid chromatography detection method, and the accuracy and reliability of the quantitative determination result are remarkably improved.

The utility model discloses a reaction device which comprises a waste water tank, the output end of the wastewater tank is connected with the cyanogen breaking kettle and is used for conveying cyanogen-containing waste liquid; a first pump body is arranged at the output end of the cyanogen breaking kettle, and the output end of the first pump body is connected with the top of the cyanogen breaking kettle and a neutralization kettle; a second pump body is arranged at the output end of the neutralization kettle, and the output end of the second pump body is connected with the top of the neutralization kettle and a saline water tank; the cyanogen breaking kettle, the neutralization kettle and the wastewater tank are matched for use, a first pump body and a second pump body are utilized for circulation in the cyanogen breaking and neutralization process, full reaction is achieved, the total cyanogen content of cyanogen-containing wastewater obtained through cyanidation synthesis of o-chlorobenzyl cyanide can be reduced to 20 mg / kg, and meanwhile the pH value of saline water is close to alkalescence.

This invention relates to a method for synthesizing azoxystrobin, belonging to the field of organic synthesis technology. The method uses 2-(2-(chloromethyl)phenyl)-3-methoxyacrylonitrile and 2-hydroxy-6-trifluoromethylpyridine as raw materials, condensing them under alkaline conditions to obtain an etherified intermediate, which is then directly hydrolyzed and esterified with methanol under acidic conditions to obtain azoxystrobin. This method avoids the use of expensive 3-isochloroketone as a raw material, using inexpensive 2-(2-(chloromethyl)phenyl)-3-methoxyacrylonitrile prepared from o-methylphenylacetonitrile as the key fragment, further reducing the cost of azoxystrobin raw materials. Furthermore, the process route is simple, the yield is high, and it is suitable for industrial production.

This invention discloses a method for synthesizing organophosphonic fluoride compounds. The method involves fluorinating organophosphonic oxides with fluorinating agents such as copper tetraacetonitrile hexafluorophosphate or copper tetraacetonitrile tetrafluoroborate to obtain organophosphonic fluoride compounds. The fluorinating agents used in this synthesis method are inexpensive, readily available, and stable, avoiding the use of expensive and unstable fluorinating agents. Furthermore, it enables efficient and selective conversion of organophosphonic oxides to organophosphonic fluoride compounds under mild conditions, and exhibits a wide range of functional group tolerances.

The invention relates to a preparation method of ketoprofen, and belongs to the technical field of synthesis of drug intermediates. In order to solve the problems of low yield and difficulty in removing impurities in the prior art, the invention provides a preparation method of ketoprofen, which comprises the following steps: in the presence of alkali metal alkoxide, reacting 3-benzoylbenzyl cyanide with a methyl esterification reagent to obtain a compound as shown in a formula II; carrying out methylation reaction on the compound as shown in the formula II and dimethyl sulfate; carrying out selective ester hydrolysis reaction under the action of an ester hydrolysis catalyst to obtain salt of a compound as shown in a formula IV; after the reaction is finished, enabling a reaction solution to contain water and a water-insoluble organic solvent, standing for layering, collecting a water phase, and adding acid into the water phase for acidification to obtain a compound shown as a formula IV; and under acidic or alkaline conditions, carrying out cyano hydrolysis and decarboxylation reaction on the compound as shown in the formula IV to obtain ketoprofen. Through route improvement, the product purity is more effectively guaranteed, and the effects of high product purity and yield are achieved.

The invention discloses a high performance liquid detection method for purity of (1S, 4R)-4-amino-2-cyclopentene-1-methanol hydrochloride, which comprises the following steps of: preparing a solution sample by adopting a chromatographic column taking octadecylsilane chemically bonded silica as a filling agent and taking acetonitrile-a buffer solution containing 50mmoL / L sodium dihydrogen phosphate and 10mmoL / L sodium octanesulfonate in a volume ratio of (13: 87)-(17: 83) as a mobile phase; and calculating the purity of the sample according to a peak area normalization method. The method can effectively separate each component in a short time, and has the characteristics of simplicity and convenience in operation, high analysis efficiency and stable result.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of triazolone-14C. Comprising the following steps: synthesizing phenol-14C: preparing a system A: adding water and concentrated sulfuric acid into a single-mouth bottle and stirring; performing liquid separation on aniline hydrochloride-14C and a saturated sodium bicarbonate solution, performing extraction, adding an organic phase into the system A, performing reaction concentration, dropwise adding sodium nitrite, adding methylbenzene, and performing reaction at 100 DEG C; extracting, drying, filtering, concentrating, and passing through a chromatographic column; the preparation method comprises the following steps: synthesizing 4-chlorophenol-14C, namely dropwise adding N-chlorosuccinimide into 4-chlorophenol-14C, p-toluenesulfonic acid and acetonitrile, and reacting completely; extracting, drying, filtering, concentrating, and passing through a chromatographic column; 4-chlorophenol-14C, ethyl acetate, 1, 2, 4-triazole, potassium carbonate and 600 polyethylene glycol are synthesized, 1, 1-dichloropinacolone is dropwise added, and a reaction is conducted at the temperature of 85 DEG C; after the reaction is finished, cooling to room temperature, extracting, drying, filtering, concentrating, and passing through a chromatographic column; the total yield of the three steps is basically maintained between 60% and 85%, the synthetic reaction conditions are simple, and the yield is high.

The invention discloses a method for determining the content of formaldehyde in a hydrochlorothiazide bulk drug, which comprises the following steps: precisely weighing a formaldehyde solution, adding acetonitrile, an acetonitrile solution of 2, 4-dinitrophenylhydrazine and a phosphoric acid solution, and diluting to prepare a reference substance solution; the method comprises the following steps: precisely weighing a hydrochlorothiazide bulk drug, adding acetonitrile, an acetonitrile solution of 2, 4-dinitrophenylhydrazine and a phosphoric acid solution, and diluting to prepare a test solution; the method comprises the following steps: precisely measuring an acetonitrile solution of 2, 4-dinitrophenylhydrazine, a phosphoric acid solution and 1ml of acetonitrile, and diluting with acetonitrile to prepare a blank solution; analyzing by adopting high performance liquid chromatography, precisely measuring the blank solution, the test solution and the reference substance solution, respectively injecting into a liquid chromatograph, recording chromatograms, and calculating by peak area according to an external standard method to obtain the content of formaldehyde in the hydrochlorothiazide bulk drug. The method has the remarkable effects that the method has the characteristics of simple process, low use cost, good precision, high accuracy and the like, and the content of formaldehyde in the hydrochlorothiazide bulk drug can be rapidly measured.

The invention discloses a high performance liquid chromatography method for detecting related substances in a tandospirone citrate bulk drug. According to the method, a chromatographic column is an octadecyl silane bonded silica gel packed column; the mobile phase A is a mixed solution of a buffer system with the pH value of 2.5-4.5 and acetonitrile, the mobile phase B is a mixed solution of a buffer system with the pH value of 1.5-3.0 and acetonitrile, gradient elution is adopted, dual-wavelength detection can be adopted, the first detection wavelength is 220-250 nm, and the second detection wavelength is 190-215 nm. The method can simultaneously separate and detect various related substances in the bulk drug, has the characteristics of strong specificity, high sensitivity, good repeatability, simplicity and convenience in operation and the like, and can be used for quality control of the tandospirone citrate bulk drug.

The application provides a synthesis method of p-chlorophenylglycine, which comprises the following steps: (1) dissolving p-chlorophenylacetonitrile in an alcohol solvent, and reacting by introducing hydrogen chloride gas to obtain 2-(4-chlorophenyl)-1-imino-ethyl methyl ether hydrochloride; (2) oxidizing the 2-(4-chlorophenyl)-1-imino-ethyl methyl ether hydrochloride by an oxidizing agent to obtain an oxidation intermediate; (3) under alkaline conditions, the oxidation intermediate is subjected to Neber rearrangement and hydrolysis to generate p-chlorophenylglycine sodium salt; and after the reaction is completed, the p-chlorophenylglycine is precipitated after the acid is adjusted to the isoelectric point. The method provided by the application has the advantages that raw materials are easy to obtain, the synthesis process is simple, the reaction is more mild, the toxicity and pollution of cyanide are avoided, the yield of p-chlorophenylglycine is high, and the method is suitable for industrialized scale production.

The invention relates to application of a metal catalyst in catalytic hydrolysis of o-chlorophenylacetonitrile or phenylacetic acid, and the metal catalyst is a metal oxide of a manganese element and / or a cerium element, and / or a solid composite metal oxide containing a rare earth element and at least one of the manganese element, the cerium element, an alkali metal element and an alkaline earth metal element, and / or a solid composite oxide containing at least two rare earth elements. The metal catalyst provided by the invention has an efficient catalytic hydrolysis effect on chlorophenylacetonitrile or phenylacetic acid, and can achieve the purpose of efficient and environment-friendly preparation of chlorophenylacetic acid or phenylacetic acid.

The present application relates to a kind of methods for preparing hydrogen cyanide by methanol ammoxidation, the method is that methanol is mixed with ammonia, air is preheated and then enters the reactor containing catalyst to carry out ammoxidation reaction, and generates the reaction gas containing hydrogen cyanide, the reaction gas is sequentially subjected to cooling, ammonia neutralization, hydrogen cyanide absorption and rectification process to obtain high-purity hydrogen cyanide, wherein, the absolute humidity in the mixed gas of gaseous methanol, ammonia and air is controlled to be 0.5-5.0g / m 3 The present application effectively reduces the generation of by-products such as formaldehyde and hydroxyacetonitrile during the reaction, improves the yield and purity of hydrogen cyanide, and reduces the problem of pipeline blockage caused by by-products.

The invention relates to the technical field of liquid crystal materials, and discloses 3, 3 '-biphenol-thiadiazolyl diurea as well as a preparation method and application thereof. Aminoacetonitrile hydrochloride and sodium nitrite react to generate aminoacetonitrile diazonium salt; reacting the aminoacetonitrile diazonium salt with hydrogen sulfide to generate 5-aminothiadiazole; the preparation method comprises the following steps: reacting 5-aminothiadiazole with 3-chloro-6-methoxy phenyl isocyanate to generate thiadiazolyl-3-chloroanisole-2-ylurea, and recording the thiadiazolyl-3-chloroanisole-2-ylurea as BP010-3; and reacting the BP010 <-3 > with sodium hydroxide to generate BP010 <-4 >, and reacting the BP010 <-4 > with hydrochloric acid to generate the 3, 3 '-biphenol-thiadiazolyl diurea. According to the liquid crystal material 3, 3 '-biphenol-thiadiazolyl diurea, different functional groups are introduced into biphenol to achieve different application scenes, compared with a traditional material, the material has better electrical conductivity, abrasion resistance, moisture resistance, cold resistance and the like, and the technical barrier of liquid crystal material application in the market is broken through.

The invention provides a method for detecting the content of ethanol and residual solvents in fluorine [18F] tosipir injection, and relates to the technical field of drug analysis and detection.The method comprises the steps that gas chromatography is adopted for detection, the residual solvents comprise acetonitrile and dimethyl sulfoxide, and the conditions of the gas chromatography are as follows: a chromatographic column is SH-PolarWax; the diluent is N, N-dimethyl formamide; the column temperature is programmed, the initial temperature is 35-45 DEG C, and the temperature is kept for 4-8 minutes; raising the temperature to 160 DEG C at the speed of 35-45 DEG C / min, and keeping the temperature for 1 Heating to 200 DEG C at the speed of 6-14 DEG C / min, and keeping for 4-10 minutes; according to the chromatographic conditions disclosed by the invention, the ethanol and the residual solvent in the fluorine [18F] tolcipir injection can be well separated, and the method can be used for determining and controlling the ethanol and the residual solvent in the fluorine [18F] tolcipir injection in the fluorine [18F] tolcipir injection.

The application discloses a synthetic method of flonicamid, and belongs to the technical field of organic synthesis. 4-trifluoromethyl nicotinic acid and aminoacetonitrile hydrochloride are reacted in the presence of a mixed catalytic system, a dichloromethane and water mixed system is used for refluxing, water is added for crystallization, and then filtering and drying are carried out to obtain white crystal flonicamid product, the purity of which can reach more than 99.0%, and the product is stored in a dry and sealed manner. The method has the advantages of simple operation, less reaction by-products, high product purity and low cost, and has great competitiveness in the market.

The invention discloses a near-infrared luminous gold-copper doped nano-cluster material as well as a synthesis method and application thereof, and belongs to the crossing field of coordination chemistry and nano materials. Thioether gold and copper hexafluorophosphate tetraacetonitrile serve as raw materials, binaphthyl dithiophosphate (R / S-PS) is used for coordination protection, a reducing agent diphenyl silane (Ph2SiH2) is added, the gold-copper-doped nano-cluster material with the near-infrared light emitting function is obtained through a one-pot reduction method, the molecular formula of an enantiomer cluster is Au13Cu4 (C20H12O2PS2) 12 (C7H17NCl) 3, the abbreviation is R / S-Au13Cu4, the enantiomer cluster belongs to an orthorhombic system, and the molecular formula of the enantiomer cluster is shown in the description. And the space group is a chiral space group C222. The material shows a remarkable aggregation-induced emission (AIE) characteristic in a dichloromethane / cyclohexane system. The compound shows strong near-infrared emission at 725 nm in an aggregation state, the photoluminescence quantum yield is as high as 35%, and the compound has a remarkable two-photon excitation luminescence characteristic. The excellent optical properties lay a foundation for realizing high-quality cell imaging application under 740 nm exciting light.

This invention relates to a simple method for preparing photochromic triphenylacrylonitrile compounds. The readily synthesizable 2-(4-bromophenyl)-3,3-diphenylacetonitrile acrylonitrile is reacted with diphenyl disulfide to obtain a sulfide fluorescent compound, which is then oxidized using different oxidants to obtain sulfoxide or sulfone fluorescent compounds. All synthesized fluorescent compounds exhibit photochromic properties in solution. The sulfoxide-containing triphenylacrylonitrile compounds can be recrystallized using different methods to obtain crystals with two conformations, only one of which exhibits photochromic properties. This method is simple to operate and has high yield. The crystal structure of the compounds prepared by this method is beneficial for studying the relationship between solid conformation and photostimulation, and can be applied to memory storage materials.

This invention discloses a method for preparing a polymer electrolyte and its application. The polymer solid-state electrolyte is prepared by free radical thermal polymerization after adding a low-solventization-energy, low-melting-point small-size co-solvent, polymer monomer, and initiator to a deep eutectic electrolyte. The deep eutectic electrolyte is prepared through a eutectic reaction of a hydrogen bond donor and a lithium salt. The low-solventization-energy, low-melting-point small-size co-solvent is one or more of acetonitrile, fluoroacetonitrile, difluoroacetonitrile, and trifluoroacetonitrile. The polymer electrolyte for solid-state batteries provided by this invention has high conductivity, a simple preparation method, good flexibility, and is easy to process. It exhibits good stability to the lithium metal anode while also accommodating the rapid desolvation process of lithium ions, and can be applied in wide-temperature-range solid-state batteries operating at -80 to 120°C.

The invention belongs to the field of analytical chemistry detection, and particularly relates to a method for detecting radiochemical purity of actinide [225Ac] conjugates. According to the method, high performance liquid chromatography is adopted to be connected with a gamma counter in series, a mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is a mixed solution of buffer salt and a cation pair reagent, and the mobile phase B is acetonitrile. The detection method can accurately detect the radiochemical purity of the 225Ac conjugate, is stable, reliable and high in sensitivity, and has important significance on quality control and research of actinide [225Ac] conjugate products.

The invention relates to a perfluorocyclopentane oxide continuous epoxidation reaction and centrifugal separation integrated process system and a method thereof.According to the system, secondary salt-containing wastewater discharged by a centrifugal separator is directly fed into a sodium hypochlorite preparation kettle and mixed with solid sodium hypochlorite fed by a solid sodium hypochlorite closed feeding device; preparing a 15-20% high-concentration sodium hypochlorite solution and recycling the sodium hypochlorite solution to a reaction system; according to the system, a high-concentration sodium hypochlorite solution, an acetonitrile solvent and D2 are mixed according to an accurate ratio at 10-20 DEG C through a two-stage mixer, the mixture enters a micro-channel tubular reactor, and reaction is performed for 4-9 seconds at 10-30 DEG C to complete epoxidation reaction; and carrying out stage treatment on the product through a serial centrifugal separator to quickly separate out a crude perfluorocyclopentane oxide product, a circulating solvent and salt-containing wastewater. Low-temperature rapid reaction is achieved through the microchannel reactor, the sodium hypochlorite decomposition risk is eliminated through two-stage centrifugal separation, and the device has the advantages of being high in raw material utilization rate, low in energy consumption, good in safety, capable of achieving continuous and automatic operation in the whole process and the like.

The invention discloses a method for determining the content of NBPT in urea. The method comprises the following steps: S1, preparing a detection reagent; s2, sample pretreatment; s3, carrying out chromatography-mass spectrometry detection; and S4, quantitative analysis. According to the method, a 0.1% formic acid aqueous solution-acetonitrile mobile phase system is directly injected into an LC-MS / MS system, formic acid serves as an ionization accelerant to remarkably improve the protonation efficiency of NBPT under an ESI < + > source, the [M + H] < + > response strength is larger than 105 cps, and the derivatization step necessary for a traditional HPLC-UV method is thoroughly omitted; secondly, a blank matrix extracting solution is introduced to match a standard curve, a urea / fertilizer matrix extracting solution homologous with a to-be-detected sample is used for diluting a standard substance, the ion inhibition effect of high-concentration ammonium salt larger than 5000mg / kg in urea on a target substance is accurately counteracted, the standard addition recovery rate of a complex matrix sample is stabilized to be 85%-99.5%, and the quantitative deviation is smaller than 5%.

This invention discloses a method for preparing methylglycine-N,N-diacetic acid trialkali metal salt. The method involves preparing a methylglycine-N,N-diacetic acid (MGDN) solution using solid iminodiacetonitrile (IDAN) and liquid hydrogen cyanide and acetaldehyde solutions. This is followed by a two-step alkaline hydrolysis to prepare the methylglycine-N,N-diacetic acid trialkali metal salt solution. The optimized post-treatment improves the overall product yield, reduces byproduct formation, and enhances product quality and stability. The methylglycine-N,N-diacetic acid trialkali metal salt product prepared by this method has a yield >97%, an NTA.3Na content <0.08%, a Hazen color number of 20–280, and a total aldehyde residue of 5–20 ppm, including formaldehyde, acetaldehyde, and formaldehyde releasers.

The application discloses a process for preparing HCN by methanol ammonia oxidation. The process is characterized by using ammonia, methanol and air as raw materials to prepare HCN in a reactor loaded with catalyst A and catalyst B; the catalyst A and the catalyst B are loaded in the upper part and the lower part of the reactor in sections. The application is applied to the preparation of HCN by methanol ammonia oxidation, and the bed temperature under high load is controllable, the activity and HCN selectivity are excellent, the preparation cost is low, and the selectivity of by-products formaldehyde and hydroxyacetonitrile is low.

This invention belongs to the field of analytical chemistry detection, specifically relating to a lutetium [ 177 A method for detecting the radiochemical purity of lutetium [Lu] conjugates. The method employs high-performance liquid chromatography (HPLC) with a tandem radioactive detector. The mobile phase comprises mobile phase A and mobile phase B, wherein mobile phase A is phosphoric acid and a phosphate buffer, and mobile phase B is selected as acetonitrile and / or methanol. This invention's detection method can accurately detect lutetium [Lu]. 177 The radiochemical purity of the Lu conjugate is high, and it is stable, reliable, and highly sensitive, especially for lutetium [ 177 The quality control and research of Lu conjugate products are of great significance.