23 results about "Formic acid" patented technology

The invention discloses a new method for formic acid purifying, which comprises the following steps: the aqueous solution of dilute formic acid with the mass concentration of more than 30 percent and anhydrous calcium chloride are mixed, heated to 80 to 95 DEG C so as to lead the anhydrous calcium chloride to be dissolved, and then formic acid with high concentration is obtained through atmospheric distillation; and the mass ratio of the water in the aqueous solution of calcium chloride anhydrous and the aqueous solution of dilute formic acid is 1: 1.5 to 1.8. The purifying method of formic acid is a process which has the advantages of simple and convenient operation, fastness, low cost and cleanness, thus being suitable for industrial production.

The invention provides a preparation method for preparing a nylon porous material on a large scale. The preparation method is characterized in that the selected raw material is nylon, the preparation process is simple and efficient, water in the production process can be repeatedly utilized, and the preparation method conforms to the environment-friendly concept. The nylon is dissolved by using anhydrous formic acid, and a sodium bicarbonate solution is added for foaming to obtain the porous material which is of a three-dimensional porous structure and has excellent performance. The prepared nylon porous material has the advantages of being low in density, high in porosity, low in heat conductivity, high in specific surface area and the like. Compared with aerogel and other porous materials, the preparation method for preparing the porous material is simple, and low-cost large-scale production can be achieved. The method can be used in heat preservation, heat insulation, marine petroleum pollution treatment, catalyst carriers, sound absorption and shock absorption buffer materials and other fields, and has wide application prospects.

The invention relates to the field of active dye in the novel technology and especially relates to low-alkali or alkali-free active bright-blue dye and a preparation method thereof. The invention provides the low-alkali or alkali-free active bright-blue dye shown in the formula (1), and in the formula (1), M represents hydrogen or alkali metal. In dyeing, the low-alkali or alkali-free active bright-blue dye can be crosslinked and fixed to cotton fibers only by use of 1-3g/l of an alkali agent and even, the low-alkali or alkali-free active bright-blue dye can be crosslinked and fixed to the cotton fibers under the condition of dyeing bath pH of 7 and no alkali agent. The preparation method is a novel technology completely different from the traditional technology and is especially suitable for blended fabric dyeing. The low-alkali or alkali-free active bright-blue dye and the cotton fibers are bonded by covalent bonds and thus dry and wet fastness, solarization fastness and washing fastness are stable and good. Separated picolinic acid is a vitamin and has small influence on the environment.

The invention discloses non-toxic anti-crack putty.The non-toxic anti-crack putty mainly comprises, by weight, 18-24 parts of calcite powder, 35-45 parts of shell powder, 25-32 parts of perlite, 3-6 parts of hydroxypropyl methyl celluloses, 7-13 parts of starch ether, 6-10 parts of modified seaweed, 6-12 parts of calcium carbonate, 3-4 parts of ethylenediamine, 4-7 parts of formic acid, 18-23 parts of diatomaceous earth, 7-15 parts of latex powder, 6-9 parts of sodium silicate, 4-6 parts of rosin, 3-5 parts of methyl silicone oil and 22-26 parts of water.The non-toxic anti-crack putty has the advantages that good anti-crack effects can be realized by the non-toxic anti-crack putty, the non-toxic anti-crack putty is good in adhesion, water resistance and glossiness and high in strength and is non-toxic and odorless, processes for manufacturing the non-toxic anti-crack putty are simple and are convenient to implement and suitable for factory mass production, and the like.

The invention provides a method for detecting the content of ergothioneine in edible mushrooms, and belongs to the technical field of analytical chemistry. According to the present invention, an edible mushroom to be detected comprises a fresh sample or a dry sample, an extraction solvent is specifically selected according to the fresh sample and the dry sample, the extraction solvent adopted by the fresh sample is a formic acid-methanol solution, the formic acid-aqueous solution or the formic acid- methanol-aqueous solution, the extraction solvent adopted by the dry sample is the methanol-aqueous solution, and the ultrasonic or oscillation extraction method is adopted; the operation is simple; the extraction effect is good, and then the content of ergothioneine in the extracting solutionis analyzed by utilizing a hydrophilic interaction chromatography ultra-high performance liquid chromatography (HILIC-UPLC), so that the content of ergothioneine in the edible mushroom to be detectedcan be accurately and rapidly determined. In addition, the method provided by the invention is good in repeatability and high in separation degree.

The invention discloses a preparation method of indole-3-carboxylic acid. The preparation method is implemented by the following steps: (1) adding a catalyst into an organic solvent prepared from indole; (2) adding solid phosgene into an indole solution containing the catalyst, so as to generate acylation reaction; (3) carrying out basic hydrolysis on a product generated in the step (2) by virtueof an alkaline solution; (4) carrying out acidization on a product generated in the step (3) by virtue of inorganic acid; and (5) carrying out recrystallization on a product generated in the step (4),so as to obtain indole-3-carboxylic acid. The preparation method is simple and convenient in operation and high in product purity and yield and can meet chemical and medicine production requirements.

Provided are a preparation method for synthesizing a pyrazolecarboxylic acid derivative of the following formula (I), which is suitable for industrial production, and an intermediate as shown by the following formula (II). The method is high in reaction yield in each step, low in waste gas and waste water and low in cost, and requires no special reaction equipment.

The invention discloses a method for synthesizing 2,5-furandicarboxylic acid by catalyzing carbon dioxide with N-heterocyclic carbene. The method comprises the following steps: (1) dissolving furoate, N-heterocyclic carbene (NHC) and a metal compound catalyst in a first solvent, and introducing CO2 for a reaction to obtain 2,5-furandicarboxylic acid 2-formate; (2) dissolving 2,5-furandicarboxylic acid 2-formate and alkali in a second solvent for a reaction to obtain 2,5-furandicarboxylic acid salt; and (3) dissolving the 2,5-furandicarboxylic acid salt in deionized water, and conducting acidifying with an acid to obtain 2, 5-furandicarboxylic acid. Compared with the prior art, the method has the advantages that a reaction system is simple, intermediate oxidation products are not accumulated, the yield and the yield of FDCA are high, and the method has industrial application potential; and meanwhile, CO2 is a carbon resource which is rich in reserves, low in price and easy to obtain, and CO2 is efficiently converted into a product with a high economic added value through catalytic conversion, so a way for reducing CO2 emission is achieved.

The invention relates to a preparation method of a tobacco precursor-aroma monomer pyrazine-2-formate. The method includes the steps of: dissolving pyrazine-2-formic acid and beta-ionol in dry dichloromethane, performing stirring for 10min-30min, adding 4-dimethylamino pyridine and 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride, conducting stirring at room temperature for 4-12h, carrying out TLC monitoring reaction, and tracking the reaction end point, adding water into an organic phase for washing, separating liquid, then using a saturated sodium chloride solution to perform washing, and separating liquid, drying the organic phase with anhydrous Na2SO4, and performing concentration to obtain a crude product, and carrying out column chromatographic separation so as to obtain the product. Compared with geraniol and beta-ionol precursors, the pyrazine-2-geranyl formate and pyrazine-2-formic acid-beta-ionol ester prepared by the method provided by the invention can significantly increase the adding amount in cigarettes, are applied as a tobacco fragrance enhancer in cigarettes, can reduce cigarette irritation and miscellaneous gas, and can improve the mellow sense and comfort of cigarette smoke.

The invention discloses an oil washing agent for carbon dioxide displacement as well as a preparation method and application thereof, and belongs to the field of carbon dioxide displacement oil extraction. The preparation method of the oil washing agent comprises the following steps: reacting a first monomer with formaldehyde in formic acid to obtain a first reactant; reacting the first reactant with borane, adding an oxidizing agent, and reacting under an alkaline condition to generate a second reactant; and reacting the aromatic hydrocarbon and a second monomer to obtain a third reactant, and reacting the second reactant and the third reactant under the heating condition to obtain the oil washing agent, wherein the first monomer is selected from at least one of 3-phenyl-4-pentene-1-amine, 4-pentene-1-amine, 4-methyl-pentene-1-amine and 2-amino-4-pentenoic acid; the second monomer is selected from at least one of succinic anhydride, 2,3-dimethyl succinic anhydride, glutaric anhydride and adipic anhydride; and the aromatic hydrocarbon is selected from at least one of benzene, methylbenzene and ethylbenzene.

The invention provides a continuous hydrogenation method of ethyl pyrazine-2-carboxylate. The continuous hydrogenation method comprises the following steps: dispersing a mixture of ethyl pyrazine-2-carboxylate and hydrogen to form a gas-liquid mixture containing small liquid drops with sizes of 50 nm-5 mm, wherein the gas-liquid mixture is used as a reaction raw material; and continuously inputting the reaction raw material into a fixed bed reactor, carrying out a catalytic hydrogenation reaction, and continuously discharging ethyl pyrazine-2-carboxylate, wherein the fixed bed reactor is divided into at least two temperature control sections along the flowing direction of the material, and the temperature of the latter temperature control section is controlled to be lower than the temperature of the former temperature control section. According to the above forced dispersion process, the reaction raw material can be subjected to high-performance mass transfer in the catalytic hydrogenation reaction process, so the sufficient reaction degree of the reaction raw material is improved, and reaction time is shortened. The fixed bed reactor is subjected to sectional temperature controlalong the flowing direction of the material, so heat accumulation can be effectively removed, a reaction state in the reactor can be effectively controlled, and the yield, purity and product performance stability of a target product, namely ethyl pyrazine-2-carboxylate are improved.

The invention relates to the technical field of dyeing auxiliaries and particularly relates to a preparation method of a color fixing agent for mercerized wool deep green dyeing. The preparation method comprises the following steps: preparing the following raw materials in parts by mass: 20-25 parts of polydimethylsiloxane, 7-12 parts of ethanol, 5-8 parts of triethanolamine, 1-2 parts of polypropylene glycol, 3-6 parts of triethylene triamine, 2-8 parts of fatty alcohol-polyoxyethylene ether, 2-4 parts of formic acid and 100-200 parts of water; putting the raw materials into a stirring tank,and continuously stirring for 20-30 min at 120 rpm at 45 DEG C to obtain the color fixing agent for mercerized wool deep green dyeing. According to the preparation method of the color fixing agent formercerized wool deep green dyeing provided by the invention, the obtained color fixing agent can effectively improve the color fastness of the mercerized wool dyed by the deep green dye while effectively avoiding the phenomena such as color fading after the mercerized wool dyeing.

The invention discloses a new way for synthesizing formaldehyde and/or methanol from formic acid. Efficient synthesis from the formic acid to the formaldehyde and/or the methanol is realized through combination of different chemical reactions. According to the new way for synthesizing the formaldehyde and/or the methanol from the formic acid, the new way needs less energy (1 mole of ATP to ADP needs to be consumed for producing 1 mole of formaldehyde), the efficiency is higher, and 2 mM of formaldehyde or 4.83 mM of methanol can be produced within 1 hour. The new way can be integrated with existing approaches to realize the purpose of synthesizing complex compounds and liquid fuels by using raw materials such as carbon dioxide, biomass, natural gas and the like.

The invention belongs to the technical field of catalytic synthesis, and particularly relates to a manganese oxide supported catalyst, a preparation method thereof and a preparation method of formic acid. The manganese oxide supported catalyst provided by the invention comprises a carrier, and a manganese oxide and a metal oxide auxiliary agent which are supported on the surface of the carrier. The invention also provides a preparation method of formic acid by using the manganese oxide supported catalyst, and the preparation method comprises the following steps: mixing cellulose, the catalyst and water under the condition of oxygen, and carrying out hydrolytic oxidation reaction to obtain formic acid, the catalyst is the manganese oxide supported catalyst in the scheme. Results of the embodiment show that the formic acid is prepared from the widely sourced and renewable cellulose biomass as the raw material, the formic acid can be prepared by a one-pot method, the preparation steps are simple, the yield and selectivity of the formic acid are high, the yield is 58% or above, the selectivity is 79% or above, and the catalyst can be recycled and is environmentally friendly.

The invention discloses a determining pretreatment method for a leek sample containing 3,5,6-trichloro-2-pyridinol pesticide residue. The method comprises: accurately weighing 10-20 g of a crushed sample in a 250 mL conical flask with a stopper, adding an acidified mixed solution of ethyl acetate and water, performing vibrating extraction, then collecting the organic phase, concentrating to almost dry, eluting with acidified acetonitrile, purifying by using a graphitized carbon amino column, using methanol and formic acid water with the concentration of 0.1% according to the volume ratio of 50:50 for dissolving, and filtering by a 0.22 mu m filter film for determining. The disclosed processing method is capable of processing 3,5,6-trichloro-2-pyridinol in leek, does not need derivatization, and is fast in determining speed, low in cost, and high in sensitivity, accuracy, stability and reliability.

The present invention is hygroplasm combining detection method for detecting several kinds of drugs in urine. The present invention features that based on practical sample condition and required detection sensitivity, the sample is first pre-treated via solid phase extraction, direct deposition or direct sample feeding, and then gradient eluted in linked chromatographic column with SKF525A as internal reference and water or methanol containing formic acid as flow phase. The method is simple and reliable in the quantitative detection of 19 kinds of drugs and has its methodologic indexes meeting the practical requirement.

The invention relates to a method for identifying bamboo shavings in gingered bamboo shavings traditional Chinese medicine formula granules. The method comprises the following steps: respectively taking gingered bamboo shavings traditional Chinese medicine formula granules and bamboo shavings reference medicinal materials, and preparing a test solution and a reference medicinal material solution; and spotting the test solution and the reference medicinal material solution on a thin layer chromatography plate, developing by using toluene-trichloromethane-acetone-formic acid as a developing solvent, and inspecting. According to the method, a thin-layer chromatography process, especially a developing solvent formula, is adjusted, the developing solvent can specifically dissolve the bamboo shavings components so as to separate the bamboo shavings components from the test solution and then develop the bamboo shavings components on the chromatography plate, the influence of other interference components is effectively removed, the color development of spots is clear, and the separation degree is good.

The invention belongs to the technical field of optical adhesives, and particularly relates to a hot-melt optical adhesive with an ultraviolet blocking function and a preparation method thereof, and the hot-melt optical adhesive comprises the following components in parts by weight: 100 parts of a mixed copolymer; 1-5 parts of a coupling agent; 0.2-0.6 part of an antioxidant; 0.1-0.6 part of a light stabilizer; 5-10 parts of a water blocking agent; the mixed copolymer is obtained by reacting an ethylene-vinyl acetate copolymer, a cross-linking agent, an anti-ultraviolet agent, an initiator and a polymerization initiator in a weight part ratio of 100: (5-10): (0.5-1): (1-3): (0.5-1); the anti-ultraviolet agent is composed of 4-methacrylamido salicylic acid and thiazolyl-2 (1H)-pyridone-4-methallyl formate, and the thiazolyl-2 (1H)-pyridone-4-methallyl formate is obtained in the mode that citric acid and 2-aminoethanethiol are subjected to a reaction to obtain an intermediate product, and then the intermediate product is subjected to methallyl alcohol esterification to obtain the thiazolyl-2 (1H)-pyridone-4-methallyl formate. According to the optical adhesive, the optical adhesive has a shielding effect on ultraviolet rays with the wavelength of 320-400 nm in sunlight, so that the damage of most ultraviolet rays to the optical cement is reduced, and the service life of the optical cement is prolonged.

The invention relates to a preparation method of a varenicline tartrate intermediate, which comprises the following steps: reducing an initial raw material 2, 3, 4, 5-tetrahydro-7, 8-dinitro-3-(trifluoroacetyl)-1, 5-methylene-1H-3-benzo aza through a Pd/C formate system to prepare the varenicline tartrate intermediate 2, 3, 4, 5-tetrahydro-7, 8-diamino-3-(trifluoroacetyl)-1, 5-methylene-1H-3-benzo aza, and further preparing the varenicline tartrate intermediate from the initial raw material 2, 3, 4, 5-tetrahydro-7, 8-dinitro-3-(trifluoroacetyl)-1, 5-methylene-1H-3-benzo aza. The 1, 5-methylene-1H-3-benzo aza is a compound shown in a formula I in the specification. The method has the advantages of mild and safe reaction conditions, low cost and good yield, is more beneficial to industrial production of varenicline tartrate, and is suitable for industrial production of varenicline tartrate.

The invention relates to refining methods of polymer materials and in particular relates to a method for refining a poly(ether-ketone-ketone) crude product by using a hydrochloric acid water solution of oxalic acid. The refining method comprises the following steps: firstly carrying out reflux stirring on a certain amount of poly(ether-ketone-ketone) crude product in a water solution containing dimethyl sulfoxide; and then adding the hydrochloric acid water solution of oxalic acid, carrying out reflux stirring and carrying out filtration after cooling; then carrying out reflux washing with a mixed water solution of glycolic acid and formic acid and carrying out filtration and drying, thus obtaining the poly(ether-ketone-ketone) pure product. Poly(ether-ketone-ketone) molecular chains tightly wrapping catalyst impurities can be unfurled by utilizing the poly(ether-ketone-ketone) swelling characteristic of the water solution containing dimethyl sulfoxide, so that impurity ions are exposed and diffused into media, and meanwhile, metal ions are continuously trapped by utilizing the metal ion chelating characteristic of oxalic acid under acidic conditions, thus achieving efficient removal of Al<3+> in the poly(ether-ketone-ketone) crude product.

The invention provides a 3, 3 ', 4, 4'-biphenyltetracarboxylic acid reaction crystallization method, and belongs to the field of chemical reaction. Mixing water with first hydrochloric acid, and preheating to obtain a preheated hydrochloric acid solution; a 3, 3 ', 4, 4'-biphenyl sodium tetraformate solution and second hydrochloric acid are dropwise added into the preheated hydrochloric acid solution at the same time, an obtained reaction solution is subjected to a double decomposition reaction, a double decomposition product is obtained, and the content of hydrochloric acid in the reaction solution is kept to be 1-10 wt% in the dropwise adding process; and continuously discharging the double decomposition product, and sequentially carrying out cooling and solid-liquid separation. According to the invention, the content of hydrochloric acid in the reaction liquid is ensured to be constant, and simultaneous dropwise addition of the 3, 3 ', 4, 4'-biphenyltetracarboxylic acid sodium solution and hydrochloric acid is limited, so that the crystalline state of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid is improved, crystalline particles of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid are more suitable for solid-liquid separation, and the quality level of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid is improved.