1020results about "Carboxylic compound separation/purification" patented technology

The invention discloses a method for preparing high-purity nickel acetate from crude nickel carbonate in the technical field of nickel compound purification, which comprises the following steps: mixing the crude nickel carbonate with deionized water to obtain a suspension, and adding glacial acetic acid to react to obtain a nickel acetate solution; then a specially-made hierarchical-pore titanium silicalite molecular sieve loaded bimetallic nanocluster material is added for purification treatment, the material is obtained through precise preparation, the method comprises the steps of carrier modification, bimetallic loading, hydrophobic modification, activation balance and the like, and the material has excellent impurity adsorption capacity and chemical stability; carrying out concentration crystallization and solid-liquid separation on the purified solution to obtain wet nickel acetate crystals; the mother liquor is subjected to adsorption treatment again, crystals in the mother liquor are recycled, and finally all the crystals are combined and dried to obtain a high-purity nickel acetate product. The process is simple and efficient, the purity of the prepared nickel acetate exceeds 98.5%, the content of each impurity is superior to the industrial standard, and the mother liquor can be recycled, is environment-friendly and is suitable for industrial production.

The invention discloses a hydrofining method for optimizing the chromatic value of a bio-based terephthalic acid product, and belongs to the technical field of terephthalic acid hydrofining. The special refining process suitable for the bio-based CTA is formed by optimizing the whole process of pretreatment, hydrogenation reaction and post-treatment. The process not only solves the problem that the bio-based raw material has many impurities, but also realizes the balance of environmental protection and economy through the green solvent (water), the efficient catalyst (Pd / C) and controllable parameter design, provides a feasible path for the industrial production of bio-based PTA, and promotes the transformation of the polyester industry to sustainable development. The method provided by the invention is high in impurity removal rate, can efficiently purify the bio-based CTA to obtain a product meeting the PTA standard, is mild in reaction condition, realizes low-energy-consumption and high-stability operation under efficient catalysis, is small in process pollution, and reduces the environmental load.

The invention provides a betaine succinate eutectic crystal as well as a preparation method and application thereof, and belongs to the technical field of eutectic crystal manufacturing. The structural formula of the succinic acid betaine eutectic crystal is shown as a formula I, the molecular formula of the succinic acid betaine eutectic crystal is C28H56N4O16, in the succinic acid betaine eutectic crystal, the molar ratio of succinic acid to betaine is 1: 2, and the succinic acid betaine eutectic crystal has low irritation and excellent effects.

The invention belongs to the technical field of impurity separation, and particularly discloses a method for separating and purifying impurities in a process for preparing glyoxylic acid through oxalic acid electrolysis, a crystallization kettle is included, an isolation device is arranged in the crystallization kettle, and the isolation device comprises a conical top cover, a conveying pipe, an annular filter screen, a directional conveying assembly and a sealing assembly; the conical top cover is arranged at the axis of the crystallization kettle, an opening of the conical top cover faces downwards, and a plurality of fixing rods are fixedly connected between the top of the conical top cover and the inner wall of the side face of the crystallization kettle. According to the method, glyoxylic acid product solutions with different concentration specifications and the high-purity glyoxylic acid crystal can be obtained after the electrolyte is sequentially subjected to pre-evaporation, electrodialysis, secondary evaporation, cooling crystallization, solid-liquid separation, washing and drying and other procedures, so that the prepared high-purity glyoxylic acid crystal can be popularized and applied in the field of high-end medicine.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of butynedioic acid. The preparation method of the butynedioic acid comprises the following steps that butynediol is oxidized into the butynedioic acid through pypocholoride and a catalyst, and the catalyst comprises carbon black and a metal compound loaded on the carbon black. According to the invention, butynediol is used as a raw material, and butynediol is oxidized by using pypocholoride and a catalyst to prepare butynedioic acid. Wherein butynediol is easy to obtain, and the raw material cost is low. In addition, the catalyst uses carbon black to immobilize a metal compound, conversion of pypocholoride into a large number of reactive oxygen free radicals can be accelerated, butynediol can be efficiently oxidized under the action of pypocholoride and the catalyst, and the whole synthesis route is safe and green, simple and feasible in process, low in equipment requirement, low in operation cost, free of secondary pollution and low in production cost.

The invention discloses a potassium propionate continuous synthesis process, and relates to the technical field of potassium propionate synthesis, the process comprises the following steps: S1, raw material pretreatment: selecting fermentation waste liquid containing propionic acid and acetic acid and potassium ore leaching liquid containing potassium hydroxide and potassium carbonate as composite raw materials, adding a composite chelating agent into the potassium ore leaching liquid, and uniformly stirring; according to the method, the composite raw material system composed of the fermentation waste liquid and the potassium ore leaching liquid is adopted, and the composite chelating agent is added, so that resource utilization of industrial waste is achieved, the raw material cost is reduced, meanwhile, impurities are prevented from interfering with continuous reaction, and through gradient temperature control-pressure cooperative regulation and linkage regulation of the PLC system, the yield is increased. The problem of product deliquescence caused by local overheating is solved, volatilization loss of propionic acid is reduced, the adaptability of the technology to raw material batch fluctuation is improved through raw material concentration online detection and dynamic parameter adaptation, the continuous production stability is guaranteed, and finally synchronous improvement of the potassium propionate synthesis efficiency and the product quality is achieved.

The invention provides a method for separating and extracting bio-based succinic acid from fermentation liquor, which comprises the following steps: (1) enabling the fermentation liquor to sequentially pass through a ceramic membrane and a nanofiltration membrane, and decoloring to obtain bio-based succinic acid decolored liquor; (2) sequentially carrying out ion exchange impurity removal and concentration treatment on the bio-based succinic acid decoloring solution to obtain a bio-based succinic acid concentrated solution; and (3) carrying out multi-stage cooling crystallization on the bio-based succinic acid concentrated solution to obtain the bio-based succinic acid, the multi-stage cooling crystallization comprises first-stage crystallization, second-stage crystallization and third-stage crystallization which are carried out in sequence. Through the steps of integrated membrane filtration, decoloration, ion exchange, concentration, multi-stage crystallization and the like, thalli, proteins, pigments, inorganic ions and other impurities in fermentation liquor can be efficiently removed, so that a high-purity bio-based succinic acid product is obtained, meanwhile, the product yield is increased, and energy consumption and waste discharge are reduced.

The invention belongs to the technical field of automatic control, and discloses a cyclopropylamine (R)-mandelate crystallization process feedback control method, which comprises the following steps: acquiring the concentration, solvent temperature, stirring speed and pH value of cyclopropylamine (R)-mandelate in a solvent in real time, and forming a state parameter set reflecting the real-time state of a cyclopropylamine (R)-mandelate crystallization system; based on the state parameter set, deriving a solute supersaturation degree change rate, a nucleation rate and a crystal growth rate by adopting an explicit kinetic relationship to obtain a kinetic feature set of the cyclopropylamine (R)-mandelate; collecting the grain size, the shape and the crystallization uniformity of the crystal, and constructing a corresponding crystal quality prediction function in combination with the kinetic feature set of the cyclopropylamine (R)-mandelate to obtain a predicted crystal quality index; comparing the actually detected crystal morphology index with the predicted crystal quality index, and calculating to obtain a deviation value; the crystal quality of the cyclopropylamine (R)-mandelate is improved.

The invention relates to the technical field of separation and purification, in particular to a method for recovering cis-15-tetracosenoic acid from an acer truncatum seed oil byproduct, which comprises the following steps: selecting the acer truncatum seed oil byproduct, crushing, sieving, washing, adding modified attapulgite and beta-cyclodextrin, stirring and adsorbing at constant temperature, and filtering; preparing the modified attapulgite; adding a KOH-EtOH solution containing lipase and polyethylene glycol into a pretreated product for refluxing, and adding a saturated saline solution for refluxing; standing and layering the reaction liquid, and extracting, acidifying, washing, drying and distilling an organic phase to obtain mixed fatty acid; and carrying out composite purification to obtain a pure cis-15-tetracosenoic acid product. According to the method, the purity and the extraction rate of the cis-15-tetracosenoic acid are remarkably improved, the oxidation, heat and storage stability of the product is enhanced, the color is improved, and the comprehensive application performance is better.

The invention provides bio-based succinic acid and a preparation method and application thereof, the median particle size of the bio-based succinic acid is 300-500 [mu] m, and the bio-based succinic acid comprises the following particles in percentage by mass: 0-10% of particles with the particle size of d1, 30-40% of particles with the particle size of d2, 40-50% of particles with the particle size of d3 and 8-18% of particles with the particle size of d4, d1 is less than 150 [mu] m, 150 [mu] m < = d2 < 300 [mu] m, 300 [mu] m < = d3 < 500 [mu] m, and d4 > = 500 [mu] m. The bio-based succinic acid is large in particle size, controllable in particle size distribution and good in uniformity, not only solves the problem of dust raising in succinic acid application, but also can reduce the adhesive force among particles and avoid the problems of agglomeration and caking, so that the storage time of the bio-based succinic acid is prolonged, the succinic acid has proper friction force, and the service life of the bio-based succinic acid is prolonged. The storage performance and the downstream application performance are improved, and the application requirements of various scenes are met.

The invention belongs to the technical field of chemical production, and particularly relates to a novel process for separating pentaerythritol by a membrane method and application of the novel process. The membrane separation comprises the steps of separating sodium formate by using an ion exchange membrane and separating pentaerythritol by using a low-pressure nanofiltration membrane device. The dealdehyding liquid is separated through different membranes, and formic acid, pentaerythritol, dipentaerythritol and other substances can be effectively separated. The process greatly shortens the process flow and saves the cost. According to the technical scheme, the quality and performance of the pentaerythritol product are remarkably improved, the added value of the product is increased, and a new technical scheme is provided for industrial production of pentaerythritol.

The invention belongs to the technical field of medical analysis, and particularly relates to a method for separating chemical components in hemsley rockvine root. According to the present invention, various chromatography methods are adopted to carry out separation and purification, such that sitroside (I), vanillyl glycolII (II), 5-hydroxymaltol (III), vanillic acid (IV), afzelin (V), 2, 3-dihydroxypyrazole (9E, 11E)-13-hydroxypyrazole (9, 11-dienoate), and 2, 3-dihydroxypyrazole (10E, 12E)-9-hydroxypyrazole (10, 12-dienoate) are obtained from hemsley rockvine root. Wherein the compounds II, III, VI and VII are separated from the hemsley rockvine root for the first time, and development and quality control of the hemsley rockvine root medicinal material are facilitated.

The invention provides an energy-saving method and device for producing feed-grade propionic acid by using methanol carbonylation acetic acid waste liquid. The methanol carbonylation acetic acid waste liquid comprises the following components in percentage by mass: 40-80% of acetic acid, 20-60% of propionic acid and the balance of high-boiling residues, the method comprises the following steps: (1) evaporating the waste liquid by adopting a film evaporator with a scraper conical structure at the bottom to obtain a first gas phase and first kettle residues, controlling the evaporation rate to be 50-85% in the evaporation process, and keeping the first kettle residues in a flowing state; 2) directly feeding the first gas phase obtained in the step 1) into a recovery rectifying tower to obtain a second gas phase and crude propionic acid, and condensing the second gas phase to obtain acetic acid; 3, the crude propionic acid obtained in the step 2 passes through a resin tower, trace impurity metal ions are removed, and then the feed-grade propionic acid product is obtained.The method is simple in technological process, low in energy consumption and capable of running continuously, the content of the recycled propionic acid is larger than or equal to 99.5%, and the concentration of the impurity metal ions reaches the feed-grade standard.

The present invention provides a method for efficiently producing a nucleic acid oligomer. Specifically, the present invention provides a method for producing a nucleic acid oligomer represented by Formula (2), the method including a step of reacting a nucleic acid oligomer represented by Formula (1) with a dichloroacetic acid solution having a molar ratio of formaldehyde to dichloroacetic acid (formaldehyde mol / dichloroacetic acid mol) of 90×10−6 or less:wherein symbols have the meanings given in the description;wherein symbols have the meanings given in the description.

The application discloses a rapid evaporation separation process of m-toluic acid, mainly including five steps of MX removal rapid evaporation, IPA removal rapid evaporation, MTA removal rapid evaporation, IPA refining and MTA refining. The process has the characteristics of short operation period, good separation effect and high MTA yield, and can recover IPA as a by-product, thereby avoiding generation of a large amount of residues.

The invention provides a fleroxacin salicylic acid drug salt single crystal prepared from acetylsalicylic acid and a preparation method thereof. The preparation method comprises the following steps: dissolving acetylsalicylic acid and fleroxacin in 8-15 mL of a solution formed by mixing one, two or more than two solvents of water, ethanol and methanol according to a certain molar ratio; and putting the mixed solution in a constant-temperature water bath at 40-80 DEG C, and stirring for 1-5 hours. And after full reaction, volatilizing the mixed solution in a suitable environment to obtain colorless blocky crystals after 1-30 days, namely the fleroxacin salicylic acid drug salt single crystals. The crystal can effectively improve the solubility, moisture absorption stability and permeability of fleroxacin. Compared with fleroxacin, the fleroxacin salicylic acid drug salt single crystal has the advantages that the bacteriostatic effect and the inflammatory factor level reducing effect are improved, and the fleroxacin salicylic acid drug salt single crystal has good antibacterial and anti-inflammatory effects.

This application relates to the field of functional crystalline material preparation and microfluidic application technology, specifically disclosing a method and product for preparing formate crystals using core-shell microcapsules, including the following steps: (1) dissolving a solid alkaline raw material in a formic acid solution to prepare reaction solution a; (2) separately conveying polymer solution A and polymer solution B with phase separation characteristics, and reaction solution a, so that they are mixed at the intersection of microchannels to prepare dispersed phase b, which is then introduced into the assembly zone for phase separation assembly to form core-shell microcapsules; (3) the core-shell microcapsules are crystallized in a continuous temperature-changing crystallization zone to form formate solid; (4) the formate solid is collected, washed and dried sequentially to obtain the target product; (5) the oil layer is continuously extracted and returned to the assembly zone for recycling. The formate crystals prepared in this application not only have a large particle size, but also exhibit good size uniformity and morphological repeatability, and have the advantages of high throughput, green environmental protection, and simple operation.

A process for production of both purified recycled aromatic dicarboxylic acid (rCA) and purified aromatic dicarboxylic acid (vCA), said process comprising:Producing a first stream comprising a recycled aromatic dicarboxylic acid by a first process, wherein the first process comprises the depolymerisation of a polymer feedstock comprising a polymer of said aromatic dicarboxylic acid in a first reaction system;Producing a second stream comprising the aromatic dicarboxylic acid by a second process wherein the second process comprises the oxidation of an aromatic hydrocarbon in a second reaction system;Purifying both the first stream and the second stream in a common purification system to thereby produce both purified recycled aromatic dicarboxylic acid (rCA) and purified aromatic dicarboxylic acid (vCA).The present invention also provides an apparatus for the production of both purified recycled aromatic dicarboxylic acid (rCA) and purified aromatic dicarboxylic acid (vCA),

This invention belongs to the technical field of medicinal chemistry and provides a milrinone-tartaric acid cocrystal. Using Cu-Kα radiation, its X-ray diffraction pattern (expressed as 2θ) exhibits characteristic peaks at at least 10.0±0.2°, 13.2±0.2°, 20.4±0.2°, 24.7±0.2°, 26.2±0.2°, 26.7±0.2°, and 34.3±0.2°. The cocrystal of this invention has high solubility and good stability. Using this cocrystal to prepare formulations avoids the use of large amounts of excipients and auxiliaries in existing technologies, reducing both production costs and clinical safety risks. The preparation method of the milrinone-tartaric acid cocrystal provided by this invention is simple to operate, the crystallization process is easy to control, and it has good reproducibility.

This invention belongs to the technical field of medicinal chemistry, specifically relating to a novel crystal form of cariprazine, specifically the cariprazine-4-hydroxybenzoic acid-methanol-hemihydrate crystal form and its preparation method. The novel cariprazine-fumaric acid crystal form provided by this invention comprises a basic unit of one molecule of cariprazine, one molecule of 4-hydroxybenzoic acid, one molecule of methanol, and 0.5 molecules of water. Its preparation method is simple to operate, the crystallization process is easy to control, and it has good reproducibility. The formation of a eutectic significantly enhances the solubility of cariprazine, exhibiting strong pharmaceutical value.

The invention discloses 10-hydroxydecanoic acid as well as a preparation method and application thereof, and belongs to the technical field of cosmetics, Candida lipolytica is taken as a fermentation thallus, the Candida lipolytica contains alkane monooxygenase (CYP450), alcohol dehydrogenase (ADH), fatty alcohol oxidase (FAO) and fatty aldehyde dehydrogenase (FALDH), amplification and activation are performed on the Candida lipolytica in a seed culture medium, and the Candida lipolytica is obtained. The method comprises the following steps: inoculating a seed solution into a liquid culture medium, enabling a strain to adapt to a culture environment in advance, reducing strain death caused by environmental mutation after inoculation, inoculating the seed solution into the liquid culture medium, culturing until OD600 is 45-55, realizing high-density enrichment of the strain, being beneficial to increasing the content of CYP450, ADH, FAO and FALDH, adding decane and Tween 80, and enabling the Tween 80 to be capable of increasing the permeability of a cell membrane and increasing the reaction rate, the CYP450 is used for catalyzing decane to carry out hydroxylation, and ADH, FAO and FALDH are used for carrying out oxidation, so that the high-purity 10-hydroxydecanoic acid is obtained.

The invention provides a resource recovery system and method for wastewater containing sodium citrate and sodium sulfate, and the system comprises a buffer mixing unit which is used for collecting wastewater and multiple paths of reflux liquid; the first nanofiltration assembly is used for preliminarily separating the mixed solution into a first concentrated solution enriched with sodium citrate and a first permeate enriched with sodium sulfate; the sodium citrate recovery branch is used for carrying out secondary concentration and evaporative crystallization on the first concentrated solution through a second nanofiltration assembly and a first crystallization unit so as to recover sodium citrate crystals or a high-concentration sodium citrate solution; the sodium sulfate recovery branch is used for carrying out concentration and freezing crystallization on the first permeate through a desalination concentration assembly and a second crystallization unit so as to recover sodium sulfate or mirabilite; and permeate liquid of the second nanofiltration assembly, mother liquid of the first crystallization unit and mother liquid of the second crystallization unit flow back to the buffer mixing unit. According to the invention, high-efficiency separation and high-purity recovery of two salt resources are realized, and the energy consumption is obviously reduced.

The invention discloses an androdenafil citrate crystal form and a preparation method thereof, and particularly provides a crystal form A to a crystal form H of androdenafil citrate, and X-ray powder diffraction analysis spectrums respectively correspond to a figure 1 to a figure 8. Compared with amorphous androdenafil citrate, the androdenafil citrate with the crystal structure obtained by the invention has higher purity, better stability and dissolution performance while ensuring the effect of inhibiting the activity of PDE5 enzyme, so that higher bioavailability can be obtained, the safety of clinical application is improved, and the androdenafil citrate is more suitable for medicine application.

This invention discloses a yam oxylipoic acid compound with aromatase inhibitory activity, its application, and analytical identification methods, belonging to the field of medicinal chemistry. The yam oxylipoic acid compound is (Z)-9-ethoxy-6,10-dihydroxyoctadec-7-enoic acid, a novel compound. This compound can significantly inhibit aromatase activity and possesses the ability to inhibit excessive estrogen production, thus showing promising application prospects and value in diseases related to estrogen imbalance regulation.

The invention discloses a use method of 2, 4-dihydroxybenzoic acid dissolving and recrystallizing equipment, the 2, 4-dihydroxybenzoic acid dissolving and recrystallizing equipment comprises a closed dissolving kettle, a crystallization kettle and a mother liquor storage tank, the closed dissolving kettle, a first separator, a first filtrate storage tank and the crystallization kettle are connected in sequence, and the mother liquor storage tank is connected with a second separator. A discharge port of the crystallization kettle is connected with a feed port of a second separator, a filtrate discharge port of the second separator is connected with a liquid inlet of a second filtrate storage tank, and a liquid outlet of the second filtrate storage tank is communicated with a liquid inlet of the mother liquid storage tank through a third pipeline; the second pipeline between the first separation column and the second pump body is communicated with a liquid outlet of the mother liquid storage tank through a fourth pipeline; the second pipeline between the second pump body and the fourth pipeline is communicated with one end of a backflow pipeline, and the other end of the backflow pipeline is communicated with the first pipeline. The 2, 4-dihydroxy benzoic acid dissolving and recrystallizing equipment disclosed by the invention can be used for preparing 2, 4-dihydroxy benzoic acid with the purity of 99.68%, and the content of metal ions is reduced to 0.15 ppm.

The invention relates to the technical field of preparation of sodium phenylacetate, and provides a preparation method of high-clarity sodium phenylacetate, which comprises the following steps: dissolving a sodium phenylacetate crude product, decolorizing, concentrating, crystallizing, separating and drying to obtain the high-clarity sodium phenylacetate, a crystallization solvent adopted during crystallization is composed of water and an organic solvent; the water accounts for 0.2%-0.8% of the volume of the devitrification solvent. Through the technical scheme, the problems of low clarity, low yield and low purity of sodium phenylacetate in the prior art are solved.

The application relates to a concentration device for methoxyacetic acid preparation and relates to the technical field of methoxyacetic acid preparation, which comprises a concentration barrel, a spraying assembly, a collecting assembly, an evaporation assembly and a detection assembly. One side top of the concentration barrel is communicated with a liquid inlet pipe, the spraying assembly is arranged in the concentration barrel, the liquid inlet pipe is communicated with the spraying assembly, and the spraying assembly is used for spraying a solution needing to be concentrated into the concentration barrel. The collecting assembly is arranged at the bottom of the concentration barrel and is used for collecting the concentrated solution. A lead screw is fixedly arranged at the center of the bottom in the concentration barrel, the lead screw is a reciprocating lead screw, the lead screw is vertically arranged and coaxially arranged with the concentration barrel. A rotating block is spirally transmission-connected with the lead screw in the vertical direction. The evaporation assembly is used for contacting steam with the sprayed solution, so that the solvent in the solution is evaporated together. The detection assembly can assist in detecting the concentrated solution. The concentration device for methoxyacetic acid preparation can realize an efficient evaporation and concentration process.

The application discloses a new ganbaxin-succinic acid co-crystal and a preparation method thereof. The method comprises the following steps: step 1, dissolving ganbaxin solid in solvent I; step 2, adding succinic acid solid into the solution obtained in step 1; step 3, heating the solution obtained in step 2 and keeping the temperature, and continuously stirring; step 4, filtering the clear solution obtained in step 3, and evaporating the filtrate; and step 5, drying the crystal obtained in step 5, and obtaining the ganbaxin-succinic acid co-crystal after drying. The solubility of the ganbaxin-succinic acid co-crystal obtained in water is 0.487 mg / mL, which is 10 times of that of the raw material medicine, and the water solubility of the ganbaxin-succinic acid co-crystal is much better than that of the original crystal.

The present invention is directed to tall oil rosin in solid, crystalline form. The tall oil rosin according to the present invention has a very low color, i.e. it is essentially color-less. The present invention is also directed to a process for producing the tall oil rosin and to the use of the tall oil rosin according to the present invention.