89 results about "Residual solvent" patented technology

The invention discloses a preparation method and application of a polymer membrane based on solvent in-situ functionalization enhancement. The method comprises the following steps: dissolving a polymer raw material by adopting a polymerizable solvent to form a homogeneous membrane casting solution; then synchronously carrying out ultraviolet light induced polymerization on the residual solvent in the membrane in the membrane casting liquid phase separation forming process by utilizing a constant-temperature circulating coagulating bath carrying an ultraviolet light illumination system; performing drying treatment to obtain a flat plate / hollow fiber composite membrane; the method is applied to the aspects of seawater desalination, wastewater treatment, food processing, biological medicine, energy chemical industry and the like. By utilizing dual functions of the solvent, polymerized solvent molecules and macromolecular chains form a stable cross-linked interpenetrating network structure, functional design of the membrane is realized through customizability of the solvent, functionalization enhancement of the membrane is realized while the process is simplified, ultraviolet polymerization synchronously optimizes phase separation kinetics, and the performance of the membrane is improved. Uniform surface pore size distribution and efficient mass transfer channels are formed, and the advantages of high efficiency and customizability are shown.

The invention relates to the technical field of liquid chromatographic analysis, and discloses a data acquisition method and system of a liquid chromatograph. The method comprises the following steps: extracting chromatograms without solvent residues and with known solvent residues from a historical database, and training by using a self-encoding neural network and a convolutional neural network to generate a baseline reference model and a ghost peak early warning model; obtaining solvent parameters of the previous analysis method, and calculating the residual solvent concentration through residual solvent information; inputting the residual solvent concentration into the baseline reference model and the ghost peak early warning model, and calculating to obtain a baseline drift prediction correction value and a ghost peak prediction risk area; pre-correcting the chromatographic signal acquired in real time to obtain a purified chromatographic signal; performing qualitative and quantitative analysis on the purification signal according to dynamic allocation resources of the ghost peak risk area to generate final chromatographic data; the data interference of the mobile phase residue is effectively eliminated, and the accuracy of data acquisition is improved.

The invention belongs to the field of high polymer material synthesis, and provides a method for preparing polyphenylene sulfide from high-purity p-dichlorobenzene, which adopts the whole process design of pre-construction of a composite sulfur source intermediate, regulation and control of an end group controllable oligomerization polyphenylene sulfide intermediate, segmented polymerization of the high-purity p-dichlorobenzene and precise dehydration-washing-drying. The ultra-low impurity level of 0.05-0.25 wt% of burning residues of the polyphenylene sulfide product, the sodium ion content of 10-200 mg / kg and the chloride ion content of 10-500 mg / kg is achieved, and meanwhile the high-performance stability of the melting point of 270-300 DEG C, the gel fraction of 92-99 wt% and the water content of 0.01-0.20 wt% is kept. The problems of deep removal of inorganic ions and ash content, balance of gel fraction and processability and control of residual solvents in the traditional polyphenylene sulfide preparation process are solved, and the method has wide application value in the fields of high-performance engineering plastics, special fibers, electronic packaging materials and the like.

The objective is to provide 5-aminolevulinic acid or its salts and a method for producing the same, which have fewer impurities and residual solvents and suppressed discoloration compared to conventional methods. The objective is to provide 5-aminolevulinic acid or its salts, wherein, based on peak area obtained by HPLC analysis, the ratio of the content of individual impurities to the content of 5-aminolevulinic acid or its salt is 0.0007 or less, and the sum of the ratios of the content of individual impurities to the content of 5-aminolevulinic acid or its salt is 0.0016 or less.

The invention discloses a crystal form and a preparation method of Alalistrum hydrochloride, the crystal form comprises a crystal form Form3, a crystal form 4 and a crystal form Form11, Alalistrum hydrochloride solids Form3 (methanol-water composite solvate), Form4 (hydrate) and Form11 can be obtained by mixing and dissolving Alalistrum hydrochloride solids and an organic solvent, and then adopting the modes of crystallization, crystal mush and volatilizing, and the Alalistrum hydrochloride solids Form3 (methanol-water composite solvate), Form4 (hydrate) and Form11 can be obtained by using the crystal form of Alalistrum hydrochloride and the preparation method of the crystal form of Alalistrum hydrochloride and the preparation method of the crystal form of Alalistrum hydrochloride. The preparation method disclosed by the invention is simple in process, strong in operability, high in yield, high in purity and good in crystallinity, and the crystal form disclosed by the invention is high in solubility, few in residual solvent and good in solid property and meets the medicinal development standard.

The utility model discloses a polymerization system for dehydration condensation reaction, which belongs to the technical field of polymer production and comprises a polymerization reaction kettle, a through hole is arranged at the top of the polymerization reaction kettle, a tower column is vertically arranged on the through hole, the tower column comprises a plurality of tower sections which are sequentially communicated from top to bottom, and fillers are arranged in the tower sections. A tower cap is arranged at the top end of the tower section located at the uppermost end of the tower column, a cooling jacket and a thermometer are arranged on the tower cap, a gas phase outlet is formed in the upper portion of the tower cap and connected with a water removal tank, a gas outlet in the top of the water removal tank is connected with a recovery device, and a vacuum pump is connected to the tail end of the recovery device in the running direction of the recovery device; the vacuum pump is connected with a PLC. By utilizing the tower column, a solvent and a monomer with high boiling points are condensed, and water and impurities with lower boiling points leave the tower column, so that the raw material waste is reduced while the reaction is promoted; a water removal tank is arranged to absorb moisture in gas, so that the moisture in the gas is prevented from condensing when residual solvents and monomers are condensed in the recovery device, and the separation effect is not influenced.

This application discloses a novel tail gas absorption and desorption system for soybean oil extraction, comprising: an identification module, an absorption module, a magnetic field module, and a feeding module. The identification module is used to identify hazardous substances, and the specific identification steps are as follows: real-time acquisition of risk data, calculation of migration risk index based on risk data, and adjustment of absorption parameters according to migration risk index; acquisition of pressure data and valve status data of the absorption tower in the absorption module, calculation of escape risk index, and classification of escape risk level according to escape index; monitoring of residual solvent concentration in tail gas, adjustment of spray volume and centrifuge status according to residual solvent concentration, and automatic switching of treatment scheme according to the magnitude of migration risk index through a graded treatment mechanism, thereby achieving effective control and removal of hazardous substances in degummed oil, reducing hazardous substance residue, and improving the quality and safety of degummed oil.

The invention relates to the technical field of crystal structure prediction, and discloses a quantum algorithm-based energetic CxNyOz crystal structure prediction method, which comprises the following steps of: calculating an evaporation and diffusion dimensionless number and capillary pressure by obtaining surface tension, a contact angle, a geometric feature scale, temperature, partial pressure, a diffusion coefficient and an evaporation rate; establishing a residual solvent mole fraction and solvent chemical potential sequence; constructing a binary layer occupancy model Hamiltonian containing layer occupancy energy, adjacent layer action energy, a capillary pressure volume term and a molecular polarity action term, and obtaining a hierarchical occupancy number by using a quantum approximation optimization algorithm; calculating interlayer respiration and shear frequency and mode volume sensitivity based on a quantum variation algorithm; and finally, the lattice spacing and the prediction result are obtained through cost functional minimization, and accurate prediction and quantitative analysis of the structure of the energetic crystal under the unbalanced desolvation condition are realized.

This invention discloses a stirred synthesis method for the production of 5-methyluridine, comprising the following steps: S1. forming a homogeneous initial reaction system; S2. obtaining a uniformly mixed intermediate reaction system with consistent temperature distribution; S3. obtaining a final reaction system; S4. obtaining a crystallization-inducing system; S5. obtaining a crystal-mother liquor suspension system; S6. obtaining a mature suspension system with completed crystal growth; S7. stopping depressurized bubbling and gradually reducing the shear pulse amplitude while maintaining low-speed three-dimensional suspension flow field stirring to age the crystals, obtaining an aged crystal suspension system; S8. terminating stirring to obtain the target product, 5-methyluridine crystals. After drying, the residual solvent content of 5-methyluridine in this invention is less than 0.05%, and its color and melting point meet pharmaceutical-grade standards.

This invention relates to the field of glycerol purification technology, specifically to a multi-stage distillation purification method for pharmaceutical-grade glycerol. Using industrially synthesized crude glycerol as raw material, the pretreated material is obtained through heating and degassing. Then, a first-stage molecular distillation removes low-boiling-point impurities, yielding an intermediate product. A second-stage molecular distillation further refines the product, collecting the gaseous glycerol fraction. Finally, under nitrogen protection, trace colored substances and residual polar impurities are removed through an adsorbent bed. After cooling, pharmaceutical-grade glycerol is obtained. Finally, the product is filtered and aseptically filled. This invention effectively removes aldehydes and ketones, residual solvents, and trace impurities from synthetic glycerol through the coupling of two-stage molecular distillation and adsorption processes. The resulting product has a purity ≥99.7%, total aldehyde and ketone impurities ≤0.005%, residual solvent ≤0.001%, bacterial endotoxin <2.5 EU / g, and batch-to-batch RSD <1%, meeting the standards for injection and suitable as an excipient in high-end pharmaceutical preparations.

The object of the present invention is to provide a thin film for a solid-state battery which, due to its low residual solvent content, has a less detrimental effect on the performance of the solid-state battery and can be produced by a continuous roll-to-roll coating process. The present invention relates to a thin film for a solid-state battery 100, comprising solid electrolyte particles 110 and crystalline fluororesin 120 and 130, which binds the solid electrolyte particles 110 together, wherein at least a portion 130 of the crystalline fluororesin has a fibrous form and the content of volatile components, measured by a gas analyzer, is 10 ppm by mass or less.

The application discloses a preparation method of high-light water-based aluminum silver paste self-laminating paint, relates to the technical field of paint preparation, and comprises the following steps: adding water-based resin and modified silicon resin into a high-speed dispersion kettle, preliminarily mixing the water-based resin and the modified silicon resin after stirring to form a resin base, adding organic silicon additives, a thickening agent and a pH regulator into the resin base in sequence, stirring and adjusting the viscosity and the pH value of the system, immersing a substrate to be coated in an alkali solution of hydroxyl ions to remove surface grease and a loose layer, washing the substrate with water, immersing the substrate in an acid solution of hydrogen ions for treatment, finally washing the substrate with water and drying the substrate, removing residual solvents and moisture from the cooled reflection layer by soft drying, and obtaining the water-based aluminum silver paste paint with a self-laminating structure. According to the preparation method, the high-light water-based aluminum silver paste paint with the self-laminating structure is prepared by optimizing filler modification, resin proportioning, surface treatment and heating processes, and the paint can provide excellent reflection performance, and ensure the stability, uniformity and adhesion of the coating.

The application discloses a preparation method of a high-refractive spectral regulation type composite optical film, which comprises the following steps: adding organic solvent and deionized water into a reactor, then adding complex acid to adjust the pH value of the reaction solution, and obtaining a mixed solvent; adding organic resin into the mixed solvent and fully stirring to uniformly dissolve; then adding a silane coupling agent, and under the condition of continuous stirring, adding titanium acid tetraisopropyl ester, a titanium oxide precursor, into the reactor to perform a hydrolysis reaction, and obtaining a hybrid sol; performing rotary evaporation on the hybrid sol to remove the contained solvent; adding a photocuring agent and uniformly mixing, coating the mixture onto a PC substrate, removing the residual solvent, curing with an ultraviolet lamp, and obtaining a product. The composite optical film prepared by the preparation method has ultraviolet-blue selective blocking function, and the overall refractive index of the material is improved, the preparation process is simple, and the method is suitable for large-scale application.

The application discloses a kind of testing methods of residual solvent in chemical fiber, it is related to chemical fiber testing technical field, including reaction box, the top position of the reaction box is provided with cover plate, the side of the reaction box is fixedly connected with handle, the front and rear sides of the reaction box are fixedly connected with side plate, a pair of rod body is fixedly connected on the side plate;It also includes docking assembly, limiting component and shaking assembly, the docking assembly is arranged on the front and rear sides of the reaction box for fixing the use of the reaction box, the limiting component is arranged on the docking assembly and is used in cooperation, the shaking assembly is arranged on the bottom plate and is used in cooperation with the reaction box.The application has reasonable structure, the reaction box can be installed and disassembled by docking assembly, the limiting component is used in cooperation with docking assembly, finally the chemical fiber and methanol in the reaction box are fully mixed and reacted by shaking assembly, which facilitates extraction detection in later period.

The invention relates to the field of analytical chemistry, and particularly discloses a method for determining residual solvents N, N-dimethylformamide, dichloromethane, isopropanol, ethyl acetate, methyl tert-butyl ether, ethanol, acetone, tetrahydrofuran and ethylene glycol dimethyl ether in a litamilast raw material by adopting a headspace-gas chromatography method, and a method for determining residual solvents N, N-dimethylformamide, dichloromethane, isopropanol, ethyl acetate, methyl tert-butyl ether, ethanol, acetone, tetrahydrofuran and ethylene glycol dimethyl ether in a litamilast raw material by adopting a headspace-gas chromatography method. The method comprises the following steps of: detecting by using a capillary column with 6 percent of cyanopropyl phenyl-94 percent of dimethyl polysiloxane as a stationary liquid through headspace sample introduction gas chromatography and a flame ionization detector (FID). According to the method disclosed by the invention, nine residual solvents contained in the litamilast raw material can be completely separated in one system, the separation degree is greater than 1.5, the specificity is good, interference from blank solvents and other unknown impurities is avoided, the sensitivity is high, the detection accuracy is high, and the quality of litamilast can be effectively controlled.

The present application relates to a kind of powder configuration device in PAN-based carbon fiber production, including configuration kettle, the top of the configuration kettle is connected with solvent feed line, powder feeding pipeline, the bottom of the configuration kettle is connected with dissolving material discharge pipeline, cleaning fluid discharge pipeline, solvent feed line is also connected with gas replacement pipeline in parallel on it.This powder configuration device in PAN-based carbon fiber production when configuration mode, when solvent addition amount finally reaches preset total amount, solvent feed regulating valve is closed, while nitrogen regulating valve is opened, replacement regulating valve is opened, residual solvent in solvent pipeline is blown to configuration kettle, and stirring until configuration ends, can guarantee the dissolution of the used powder additive Precise, guarantee powder dissolution effect.

This application relates to the field of biomedical materials technology, specifically disclosing a method for preparing a thermosensitive biodegradable root canal suppository. The method includes the following steps: S1, dissolving a thermosensitive biodegradable polymer material in a solvent; S2, adding the active pharmaceutical ingredient and excipients to the polymer solution and stirring until homogeneous; S3, injecting the mixture into a mold and placing it under low-temperature conditions to solidify the mixture into a semi-solid suppository preform; S4, removing the suppository preform from the mold; S5, removing residual solvent from the semi-solid suppository intermediate; S6, heat-treating the dried suppository intermediate; and S7, sealing and storing the finished suppository in protective packaging. The root canal suppository of this application can be used for root canal medication during root canal treatment. It has the advantages of being solid at room temperature for precise implantation into the root canal, and rapidly softening upon contact with body temperature to adapt to irregular root canal walls, achieving complete root canal sealing.

The present application relates to the field of separation and purification, and discloses a method for extracting and purifying organic substances from a biological matrix sample, comprising the following steps: after adjusting the pH of the sample to 1-3, performing sample loading and adsorption; through magnetic force, transferring the adsorption material to perform cleaning; after cleaning, before elution, performing infrared or microwave heating on the adsorption material, aiming at evaporating residual solvent, and denaturing and coagulating co-adsorbed proteins to prevent them from being co-eluted, thereby significantly improving the purity of the final eluate; and finally, performing elution on the heated adsorption material. The present application combines special materials and innovative processes, realizes automatic sample pretreatment with high recovery rate and high purity, and can be applied to the extraction of oligonucleotides, peptides, small molecules and the like; and solves the problems of low recovery rate and poor reproducibility caused by non-specific adsorption of proteins in biological samples.

The application discloses a kind of fast screening method of solvent residual quantity in food contact packaging material, sample is sent into gas chromatograph by headspace sampler and separates out the gas to be measured, and the gas to be measured is detected using hydrogen flame ion detector, and the chromatogram of sample is obtained;Add mixed standard intermediate liquid of known content in blank matrix to obtain the standard reference sample of the limited concentration to be measured, and the peak area of methyl acetate, benzene, toluene, ethylbenzene, o-xylene, m-xylene, p-xylene is measured respectively;By comparing the sum of the peak area of all detected substances in sample chromatogram with the chromatographic peak area of methyl acetate in standard reference sample, judge whether the total amount of residual solvent meets the limit requirement, and by comparing the peak area of benzene, toluene, ethylbenzene, o-xylene, m-xylene, p-xylene in sample with the peak area of corresponding substance in standard reference sample, judge whether each benzene solvent meets the limit requirement.

The utility model discloses a kind of heterogeneous solution continuous refining systems. Heterogeneous solution continuous refining system includes: crude product liquid storage unit, crude product liquid storage unit is suitable for storing heterogeneous solution;Layering unit, layering unit is connected with crude product liquid storage unit, layering unit is at least provided with 3 layering tanks of consistent height, layering tank is suitable for the layering and separation of heterogeneous solution;Fine storage unit, fine storage unit is connected with the last layering tank in layering unit, fine storage unit is suitable for storing the solvent of large density in heterogeneous solution;Impurity storage unit, impurity storage unit is connected with the last layering tank in layering unit and the first layering tank in layering unit respectively, impurity storage unit is suitable for storing the solvent of small density in heterogeneous solution, and residual solvent of large density is returned to layering unit. The utility model's heterogeneous solution continuous refining system utilizes gravity natural flow, realizes the efficient refining of heterogeneous solution, and energy consumption is low.

The application discloses a surface treatment method for improving the printing property of a screen printing plate, and comprises the following steps: S1. nanoparticle preparation: the nanoparticles comprise one or a combination of more than two of aluminum oxide, silicon dioxide, indium oxide, tin oxide, zinc oxide, tantalum pentoxide and magnesium oxide; S2. hydrophobic modification of the nanoparticles: the nanoparticles are added into ethanol in a certain proportion, 0.67 g of octadecyl phosphoric acid is added into 50 mL of the ethanol, the mixture is shaken, the excess solvent is evaporated, and the remaining modified nanoparticles are dried; S3. preparation of a coating solution: the modified nanoparticles are configured into a solution with a concentration of 10-50 mg / mL, a solvent with a ratio of tetrahydrofuran to isopropyl alcohol being 1:1 is used for preparation, and organic silicon resin is added and uniformly mixed; and S4. coating preparation: the coating solution is sprayed onto the surface of the screen printing plate by using an airbrush, and then dried to volatilize the residual solvent and solidify the resin. The film layer prepared by the method has a better hydrophobic effect than that of a perfluoropolyether film system, and the printing property of the screen printing plate is greatly improved.

The invention discloses a washing drafting process and drafting device for high-performance carbon fiber precursors, and relates to the technical field of carbon fiber precursor spinning. The device comprises a washing mechanism, and a hot water drafting mechanism is arranged on one side of the washing mechanism; the washing mechanism comprises washing tanks, a connecting roller is rotationally mounted between the washing tanks, the connecting roller is an N-angle star-shaped roller, a driving roller is rotationally mounted between the washing tanks, the tension and the drafting process of tows can be accurately adjusted, the orientation and the structure of fibers are optimized, and the physical characteristics of the fibers are further improved; by increasing the temperature of the washing tank step by step, the diffusion speed of the solvent can be increased, the washing time can be shortened, the overall production efficiency can be improved, the production line can run more smoothly, the solvent in the tows is removed through washing, the concentration of the residual solvent in the protofilaments can be remarkably reduced, and the purity and the uniformity of the final product can be ensured. The method is crucial for improving the mechanical property and the chemical stability of the carbon fiber.

The application discloses a method for detecting residual solvents in daprodustex raw medicine, characterized in that the method quantitatively detects residual solvents in daprodustex raw medicine by high performance liquid chromatography; the high performance liquid chromatography conditions adopt mixed mobile phases of mobile phase A and mobile phase B to perform gradient elution on the daprodustex raw medicine to be measured; the mobile phase A is 10 mM potassium dihydrogen phosphate in 0.1% phosphoric acid aqueous solution; the mobile phase B is a methanol solution; the initial proportion of the mobile phase A and the mobile phase B in the elution process is 100% mobile phase A and 0% mobile phase B; after the gradient elution, the chromatogram of the daprodustex raw medicine to be measured is measured, and the content of the residual solvents in the daprodustex raw medicine to be measured is calculated by the peak area according to the external standard method with the chromatogram of a standard sample.

The invention discloses a preparation process of fatty alcohol polyoxyethylene ether sulfate with low residual organic solvent. The process comprises the following steps: cooling C12-C14 fatty alcohol-polyoxyethylene ether to 25 DEG C, introducing a polyol-monoterpene synergistic solvent, carrying out 7 kPa vacuum film evaporation at about 60 DEG C, blowing nitrogen microbubbles with the pressure of 0.2-0.4 MPa into a microwell plate with the pore diameter of 5-10 m, and carrying out enhanced desolvation according to a gas-liquid volume ratio of 0.6-1.0; sulfonating the obtained material with SO3 / air mixed gas subjected to graded cooling, neutralizing, continuously desolventizing through a thin-layer falling film (80-120 m) at the temperature of 45-50 DEG C, and scavenging with nitrogen; the whole process cooperates with mass transfer to drive 1, 4-dioxane and isopropanol to rapidly migrate, and the total residual solvent of the finished product is greatly reduced.

The application relates to the field of functional polymer film materials, and discloses a porous film and a preparation method and application thereof. Two surfaces of the porous film are a hydrophilic film surface and a hydrophobic film surface; wherein the pore diameter of the porous film is 0.05-20 mu m, the average pore diameter is 2-15 mu m, the porosity is 35-80 vol.%, and the porous film is distributed with micro-protrusion structures. The porous film can effectively reduce water evaporation, the surface energy of the hydrophobic layer is relatively high, is suitable for water or mist collection, has good stability, is easy to recycle, and can avoid water body pollution caused by residual solvents on the film surface.

The application discloses a preparation method of a triptolide sesquiterpene alkaloid purity standard sample, and belongs to the technical field of natural product separation and purification and standard substance preparation. The method comprises the following steps: obtaining total alkaloid crude products through ethanol extraction and acid-dissolution alkalinization extraction, enriching the total alkaloid crude products through methanol grading, pre-separating the total alkaloid crude products through a specific two-phase system of petroleum ether (60-90 DEG C)-ethyl acetate-isopropyl alcohol-water HSCCC, and finally obtaining monomer products with purity greater than or equal to 99.0% through reverse-phase preparation HPLC refining and low-temperature multiple recrystallization. The obtained standard sample has water content less than or equal to 0.5%, residual solvents meet the requirements of ICH Q3C and the Chinese Pharmacopoeia, and the impurity spectrum fingerprint similarity is greater than or equal to 0.98 under different raw material batches and amplification conditions, so that the batch consistency, traceability and storage stability are significantly improved, and the strict requirements of standard substances in quality control and analytical detection are met.

A cellulose ester fiber comprising cellulose ester wherein the fiber has a curvature factor of less than 3; a residual solvent concentration on the cellulose ester fiber of less than 5000 ppm by weight; and wherein the solvent comprises N, N-dimethylformamide, N, N-dimethylacetamide, or dimethyl sulfoxide, or mixtures.

The application belongs to the technical field of polymer materials, and discloses a method for preparing a polyamide nanofiltration membrane based on a non-reactive ionic liquid, which comprises the following steps: preparation of a substrate PES membrane: 16wt% of polyethersulfone PES, 16wt% of polyethylene glycol PEG, and 68wt% of N-N dimethylformamide DMF are weighed and placed in a round-bottom flask, stirred in a water bath, and left to stand at the same temperature to remove air bubbles, then, the casting solution is cast on a glass plate with a steel knife and immersed in ultrapure water to remove residual solvent; preparation of a polyamide PA membrane: interfacial polymerization is performed on the PES membrane by using an aqueous phase solution containing piperazine PIP and 1-butyl-3-methylimidazole chloride and an oil phase solution containing TMC to synthesize a polyamide active layer. The application provides a new perspective for the regulation of monomer diffusion and reaction in the interfacial polymerization process, and has important application potential in the preparation of high-performance polyamide composite membranes.