325 results about "Separatory funnel" patented technology

This invention discloses method and apparatus for preparing polycarbosilane ceramic precursor containing Zr. The method comprises: utilizing low molecular weight polymer with S-H bonds (polysilane, polycarbosilane or poly(dimethyl silane)) as the raw material, organic metallic compound containing Zr as the additive, and Ar, N2 or their mixture as the protective atmosphere, and pyrolyzing at high temperatures and normal pressure to obtain Zr-containing SiC ceramic precursor PZCS. The pyrolysis apparatus comprises a three-necked flask in the heater, a pyrolysis column in the electric heating jacket, a condensing tube, a separatory funnel, and a vacuum system seam. The method is simple, and can control the content and properties of Zr in the precursor and the ceramic. The product has such advantages as high purity, high remoldability, and high heat resistance.

The invention discloses a preparation method of polyvinyl alcohol embedded spherical alta-mud, which characterized in the steps: (1) dissolving the quaternary ammonium salt cationic surface active agent into water, adding natural alta-mud, stirring, scrubbing, filtering, drying, activating, grinding by 100 mesh sieve and obtaining organobentonite; (2) mixing the said organobentonite and polyvinyl alcohol solution of 10 % containing sodium alginate of 0.02-0.2 % and stirring; (3) dripping the said mixture by separatory funnel with liquid-transfer head to crosslinking agent, after crosslinking reaction, rinsing with distilled water and drying. The excellence of the invention is: not needing filtration, centrifugation or sedimentation after adsorbing contaminant in water; having equivalent effect of removing organics to powder state alta-mud, having better effect of removing heavy metal than powder state alta-mud, capable of realizing simultaneously removing organic contaminant and heavy metal in waste-water, and capable of repetitious using after simple processing.

A process for separating Cr from the tanning sewage by emulsion membrane method includes such steps as proportionally mixing Span 80, flowing carrier TOA and kerosene, adding the mixture to NaOH solution, high-speed stirring to obtain emulsion, proportionally mixing it with K2Cr2O7 solution to be treated, low-speed stirring, laying aside for layering, discharging the lower layer of colorless water phase, and high-voltage electrostatic or microwave demulsifying to obtain Cr salt in the form of water phase.

The invention discloses a method for detecting vitamin A, D and E content in infant food and dairy products, comprising the following steps: accurately weighing a sample, adding a pyrogallic acid ethanol solution, adding a KOH aqueous solution for complete saponification, then rapidly cooling, and then placing the sample in a brown separating funnel, and irrigating an iodine flask by using an ethereal solution having a volume ratio of petroleum ether to ether being 2:1, putting the washing liquor in the brown separating funnel, shaking and standing until completely layering, carrying out extraction on the water layer by using another brown separating funnel filled with the ethereal solution, and combining the organic layers; washing the organic layers by using deionized water repeatedly until the organic layers are not alkaline, dewatering and filtering the organic layers, drying under nitrogen until nearly dried and then dissolving with methanol, blowing with a pressure blowing concentrator to 1 ml, bringing to volume by methanol, filtering through a filter membrane, and separating through a chromatographic column; separating by using 10% acetonitrile:methanol mobile phase with a flow rate of 0.3 mL/min; using three wavelengths of 296 nm, 264 nm, and 325 nm to simultaneously detect vitamin A, D and E, wherein, the detection concentrations respectively are 1.0-100.0 mu g/L, 1.0-100.0 mu g/L, and 0.50-50.0 mu g/L.

The invention belongs to the field of oil product sulfide removal, and in particular relates to a method for removing sulfide from an oil product by using a choline chloride/oxalic acid type eutectic solvent by virtue of an oxidation-extraction integrated process. The method is implemented according to the following steps: (1) synthesis of the choline chloride/oxalic acid eutectic solvent: weighing choline chloride and oxalic acid, and stirring until a transparent solution is formed to obtain the choline chloride/oxalic acid eutectic solvent; (2) a desulfurization process: weighing dibenzothiophene, and dissolving into normal octane to prepare simulated oil; weighing the simulated oil and the choline chloride/oxalic acid eutectic solvent; adding hydrogen peroxide, stirring, and cooling to room temperature; performing static lamination in a separating funnel, and absorbing a sample in an upper-layer oil phase; and measuring the sulfur content, and calculating the desulfurization rate. According to the method disclosed by the invention, in the preparation process, an adopted catalyst serves as both the catalyst and an extraction agent, thus the production cost is reduced, and the desulfurization process is simplified.

The invention discloses a method for separating and purifying microcystin by utilizing series-connected solid phase extraction columns. The method comprises the following steps of: A, preparing an algae powder material, namely harvesting wild bloom-forming cyanobacteria or microcystis aeruginosa cultured indoors, cooling and drying to prepare dried algae powder; B, preparing the solid phase extraction columns, namely putting C18 fillers into Solid Phase Extraction (SPE) columns; C, extracting algae toxin, namely weighing the dried algae powder, adding methanol according to a proportion, putting on a shaking table and oscillating at room temperature; D, removing impurities, namely adding a supernatant and an organic extractant into a separating funnel according to a proportion, mixing and uniformly shaking, standing, and after delamination, removing the organic extractant; E, separating and purifying the algae toxin, namely after pretreatment, enriching sample solution by using pre-activated series-connected SPE columns, and eluting the toxin by using 20 to 50 percent methanol aqueous solution; and F, performing Methyl Cellulose (MC) detection. The method has good separation effect, large loading amount, is easy and convenient to operate and low in cost, can obtain two microcystins with the weight of more than or equal to 10 mg and higher purity each time, and the High Performance Liquid Chromatography-Ultra Violet/Diode Array Detector (HPLC-UV/DAD) detection can reach 85 to 90 percent.

The invention relates to a gillyflower extract and a preparation method and applications thereof, belonging to the technical field of cigarette processing. The preparation method comprises the following steps: drying fresh gillyflower in the shade; smashing the dried gillyflower and sieving by a sieve with 20 meshes to obtain gillyflower powder; carrying out distillation extraction by adopting a device for distilling and extracting at the same time; continuously extracting 50g of gillyflower powder and 20ml of dichloromethane for 1-5 hours at the temperature of 50 DEG C; transferring a distillation extraction liquid to a liquid separating funnel; collecting a dichloromethane layer; and utilizing the dichloromethane rotatably recovered by a rotary evaporator at constant pressure of 40 DEG C to obtain a concentrated solution which is gillyflower extract. With adoption of 0.005-0.1% of gillyflower extract used as a spice additive in flavoring of cut tobacco of cigarette, the flavor of the cigarette can be obviously improved and modified; the fresh and sweet flavor can be enhanced, the stimulation is reduced, the miscellaneous flavors can be removed and the smoke is soft and delicate.

The invention discloses a method for extracting tea essential oil from oolong tea stalks. The method comprises the following steps of: putting the oolong tea stalks serving as raw materials into a tea stalk distillation device, adding distilled water, and distilling; measuring petroleum ether, adding into a petroleum ether distillation device, and distilling; connecting the tea stalk distillation device and the petroleum ether distillation device through a glass guide pipe, fully mixing volatile gas distilled from the tea stalks and petroleum ether steam in a gas storage bag, introducing mixed steam into a condensation pipe, condensing to form oil-water mixed liquid, and refluxing the mixed liquid to a separating funnel; refluxing a water phase and an oil phase in the separating funnel to a first flask and a second flask respectively, so that the circular extraction process is finished once; repeating the process to fully extract the essential oil from the tea stalks; and taking the second flask with the petroleum ether out, concentrating a solution in the second flask, and collecting to obtain tea essential oil paste. By the method, the extraction cost of the tea essential oil can be reduced, and the economic benefit of tea processing is improved.

The invention discloses a method for processing an onion sample containing organophosphorus and synthetic pyrethroid pesticide residues before determination, comprising the following steps: processing the onion in a microwave oven for 40 seconds; stirring, mixing and obtaining an even sample; then adding 30ml of acetonitrile and 10ml of distilled water; after oscillating and extracting for 30 minutes, filtering into a separating funnel of which the volume is 500ml; washing residues by 20ml of acetonitrile; filtering a washing liquid into the separating funnel; adding 8g of sodium chloride; oscillating for 1 minute; standing and layering; abandoning a lower-layer aqueous phase; taking an upper-layer organic phase, and processing the upper-layer organic phase by anhydrous sodium sulfate; washing the anhydrous sodium sulfate for several times by 20ml of acetonitrile; combining the acetonitrile phases; reducing pressure and concentrating to be dry; adding 2ml of acetone/ normal hexane (V/V, 1/1); eddying for 10 seconds; transferring to a sample introduction flasket; and determining by a gas chromatography and mass spectrometry. With the method for processing an onion sample before determination in the invention, impurity interference can be greatly lowered, and the method has high sensitivity.

The invention relates to a full automatic extraction device, which is used for extraction experiment in a chemical laboratory. The device comprises a shell, a getter device, an extraction container and a tap funnel which are fixedly arranged on the shell, wherein the tap funnel is positioned on the upper part of the extraction container; the extraction container is communicated with the getter device through an air duct and connected positions are all closed; the bottom end of the extraction container is provided with an imbibition long tube; the imbibition long tube passes through an opening on the top part of the tap funnel to the bottom of the tap funnel; the bottom of the tap funnel is provided with a drain pipe; the drain pipe is provided with a control valve; and the getter device is arranged in the shell, an outlet of the getter device is connected with a vent pipe, and the vent pipe extends outside the shell. The device adopts batch type vacuumizing principle, guides organic phase and aqueous phase to come and go rapidly in the extraction container and the tap funnel so as to make a target compound sufficiently transfer from the aqueous phase to the organic phase, thereby realizing liquid-liquid extraction and separation. The device can replace manual operation and save time and labor, and has good uniformity, an experimenter cannot breathe harmful gas, so the device is favorable for protecting human body from harm.

The invention discloses a preparation method for synthesizing vanillin by using natural eugenol as raw material. The preparation method comprises the following steps: adding potassium hydroxide and n-amyl alcohol into a three-neck round bottom flask with volume of 250 ml and equipped with a backflow condensation tube, a magnetic stirring device and a constant-pressure dropping funnel through isomerization, dropwise adding the natural eugenol after stirring for dissolution, heating for backflow, then transferring a reaction solution into water for dilution, transferring lower-layer liquid to a separatory funnel in several times, and washing with a NaOH solution until the color of upper-layer liquid does not become light; combining all alkali liquors, and extracting with acetone, acidating and evaporating rotatably to obtain isoeugenol; adding a certain amount of nitrobenzene into the isoeugeno to oxidize double bond of propenyl of the isoeugeno, and then purifying a vanillin crude product, wherein the vanillin productivity can reach above 95.0%. The method has the advantages that the adoption of highly-toxic catalysts of carbonyl iron and the like in the isomerization process is avoided, the after-treatment technology is relatively simple, and the operation is convenient. An extraction agent can be recycled to lower the cost.

The invention discloses a device for circularly separating soil microplastics based on a sodium bromide solution. The device comprises a separation system, a vacuum filtration system and a solution recovery system, wherein the separation system comprises a separator, an aeration disc, a tray and an adjustable aeration pump; the vacuum filtration system comprises a filtration bottle, a vacuum filtration pump and a sand core filter; and the solution recovery system comprises a separating funnel and a circulating pump. The invention also discloses a method for circularly separating the soil microplastics based on the sodium bromide solution. According to the invention, saturated sodium bromide is selected as a separation reagent of the soil microplastics; with combination with an aeration process, the microplastics float on the upper layer of a soil mixed solution, after the solution stands still and is layered, the microplastics overflow from pores of a container through aeration and solution adding power, the microplastics are collected through the vacuum filtration device, the sodium bromide solution is recycled through the recovery system, cost is greatly saved, low emission of sodium bromide is achieved, and environment protection is facilitated.

The invention provides a measuring method for monitoring the content of siloxane in hydrochloride acid during the organosilicone production process, and aims to provide a method which is simple to operate, is convenient and fast, and can accurately acquire the data about the content of siloxane in hydrochloride acid. The measuring method is realized through the technical scheme as follows: taking a clean reagent bottle, sampling from a production line a liquid phase sample with the sample amount between 100g and 1000g, and recording the total weight m2 of the sample and the reagent bottle; after taking back the sample, adding siloxane-soluble extraction agent 10 ml to 200 ml into a ventilation cabinet, oscillating violently for 5 min to 60 min, and weighing a constant weight beaker; taking lower level oil phase from a dryer into the beaker, placing oil phase in a water bath for evaporating to dryness, transferring oil phase into an oven under constant temperature at least for 1 hour and taking out oil phase, and then cooling oil phase in the dryer to the room temperature; and quantitatively calculating the content X of siloxane in the hydrochloride acid. The measuring method solves the problem that siloxane is separated out from the hydrochloride acid and accumulates to block the production device.

The invention discloses a separating funnel used in the extraction process, and belongs to the technical field of experimental vessels. According to the technical scheme, the separating funnel used in the extraction process is characterized in that the separating funnel comprises a bottle body, a bottle opening formed in neck of the bottle body and a drainpipe arranged at the bottom of the bottle body; a bottle stopper is installed on the bottle opening, the drainpipe is provided with a plug cock cavity, a polytef plug cock is installed in the plug cock cavity, multiple glass bases are evenly distributed on the portions, two-fifths away from the bottom end of the bottle opening, inside the bottle body and on the portions, one-second away from the bottom end of the bottle opening, inside the bottle body, and a hollow demulsification rod with a hole is arranged in each glass base. According to the separating funnel used in the extraction process, the structure is reasonable, the construction is simple, the liquid separation efficiency is improved, the emulsion phenomenon produced by an ordinary separating funnel in the separation process is reduced, and the problems that for the ordinary separating funnel, the flow velocity of the separating funnel is not smooth, and product loss exists under the emulsification condition are solved.

This invention incorporates barrel-shaped polymer-structured separatory funnels. The separatory funnels are made from an injection molding machine using cheaper plastic resins such as polypropylene, or polyethylene instead of glass in order to lower costs, so they are ready-to-use and disposable. The innovative separatory funnels have multi-functional features, which can be used as regular separatory funnels for liquid-liquid phase separation and extraction, as receiving receptacles to take the filtrate in a solid-liquid filtration apparatus, and also as flasks hooked in a rotary evaporator to evaporate solvents.

The invention relates to an instrument for extraction. The instrument comprises a separating funnel, wherein the bottom of the separating funnel is provided with a liquid outlet pipe; and the liquid outlet pipe is provided with a liquid outlet valve. The instrument is characterized in that the top of the separating funnel is provided with an air inlet end and an air outlet end; the air inlet end is communicated with an air inlet pipe; the air inlet pipe is arranged in the separating funnel; the bottom end of the air inlet pipe is positioned at the bottom in the separating funnel, and a vent gap is arranged between the bottom end of the air inlet pipe and the bottom in the separating funnel; at least one liquid inlet is communicated with the interior of the separating funnel; the instrument also comprises an air pump, a liquid supply device and an electric control device, wherein the air pump is at least communicated with the air inlet end of the separating funnel by an air delivery pipe; and the liquid supply device is communicated with the liquid inlet of the separating funnel by a liquid delivery pipe. The instrument is simple and compact in structure as well as simple and convenient to install and use.

The invention discloses a separating and purifying method of Metarrhizium anisopliae, which comprises the following steps: (1) adsorbing fungal ferment liquid to remove partial impurity; removing adsorbent through centrifuging; obtaining supernatant layer of ferment liquid; (2) extracting supernatant layer under ultrasound; separating organic phase and water phase through separatory funnel; reserving organic phase to condense into rough extract of Metarrhizium anisopliae; (3) decompressing rough extract of Metarrhizium anisopliae; condensing and drying fraction; dissolving and filtering; (4) making spectrum; separating and purifying the rough product in the high-effective liquid phased chromatograph to produce high-purity product.

The invention relates to a fluorescent molecular probe for detecting Cu<2+> in the field of fine chemical engineering, in particular to a preparation method of a Cu<2+> fluorescent molecular probe based on rhodamine dyes and an application of the fluorescent molecular probe to biocellular imaging and water system copper ion detection. A preparation method of a compound I includes the steps: adding 1 part of (E)-2-((3', 6'-bis (diethylamino)-3-oxaspiro [isoindazole-1, 9'-xanthene]-2-alkene) imine) ethylal and 6 parts of hydrazine hydrate into a reaction vessel, heating and stirring mixture, performing rotary evaporation to remove ethyl alcohol after reaction, and adding 50 parts of methylene dichloride and 150 parts of saturated sodium chloride solution; separating mixture by the aid of a separating funnel, drying a organic phase by the aid of anhydrous sodium sulfate, performing spin drying on solvents, and separating coarse products by a column chromatography to obtain the compound I. The preparation method is mild in reaction condition, less in synthesis step and high in product yield, and raw materials are low in cost and easily acquired.

The invention discloses a separation method of a water-soluble polymer with tetrahydrofuran as an extracting agent. The preparation method comprises the following steps: firstly, at temperature of 20-30 DEG C, adjusting a pH value of a reaction solution containing a water-soluble polymer, obtained through a polymerization reaction, to be neutral, adding sulfate to the reaction solution to form a sulfate solution; adding tetrahydrofuran to the obtained sulfate solution, calculating according to a volume ratio, i.e. a ratio of the sulfate solution to the tetrahydrofuran of 1:(0.25-2); standing and demixing after oscillating, wherein the upper layer is an organic-phase tetrahydrofuran phase, the lower layer is a water phase-phase sulfate solution; then separating the obtained tetrahydrofuran by using a separating funnel to obtain a tetrahydrofuran solution rich in water-soluble polymer, performing reduced pressure distillation in a water bath with temperature of 50-70 DEG C by using a rotary evaporator, and evaporating a tetrahydrofuran solvent to obtain the water-soluble polymer, thus realizing the separation of the water-soluble polymer with the tetrahydrofuran as the extracting agent.

The invention relates to a preparation method for a high-purity glabridin monomer, and relates to the preparation method for the high-purity glabridin monomer by separation from licorice. The preparation method mainly solves the problems of complicated preparation process, low separation efficiency, long separation time, and large consumption amount of a solvent. The method provided by the invention is characterized by comprising the following steps: preparation of a glabridin extract; concentration of glabridin by using a reversed-phase C18 column chromatography: successively eluting the extract with alcohols respectively with a concentration of 50%, 70% and 95%, respectively collecting eluents, and subjecting the collected eluent of the alcohol with the concentration of 70% to vacuum concentration until the eluent is dried so as to obtain crude glabridin; and separation of the above-mentioned crude glabridin with a high-speed countercurrent chromatographic technology: placing a separating solvent in a separatory funnel and carrying out complete shaking, then carrying out standing and layering, dissolving the above-mentioned crude glabridin in the separating solvent, and respectively measuring the concentrations of supernatant and subnatant solutions containing the glabridin with a highly-efficient liquid-phase chromatographic method. The preparation method for the high-purity glabridin monomer provided by the invention has short separation time and high recovery rate, is free of pollution, and saves the solvent.

The present invention discloses a method for concurrently determining the vitamin A content and the vitamin E content in a health product. The method comprises: (1) saponifying: weighing a sample to be detected, adding dehydrated alcohol, adding an aqueous solution of ascorbic acid, adding a dehydrated alcohol solution of benzo[e]pyrene as an internal standard solution, uniformly mixing, adding a potassium hydroxide aqueous solution, uniformly mixing, refluxing to obtain a saponifying solution, and cooling; (2) extracting: transferring the saponifying solution into a tap funnel, washing with ether, mixing the ether washing liquid into the tap funnel, shaking, carrying out standing layering, and removing the aqueous layer; (3) washing: washing with water until the aqueous layer does not present the alkaline state; (4) concentrating: loading the ether extraction solution into anhydrous sodium sulfate, filtering into a rotary evaporation flask, rinsing the tap funnel and the anhydrous sodium sulfate with ether, mixing the washing liquids, adding to the rotary evaporation flask, carrying out pressure reducing distillation, carrying out blow-drying with nitrogen gas, and immediately adding an ethanol aqueous solution to dissolve; and (5) using an ultra high-performance liquid chromatograph to determine.

A recovery process of phenylacetic acid belongs to the field of chemical technology, and more particularly, relates to a recovery process of phenylacetic acid. The invention provides a recovery process of phenylacetic acid, which has simple operations, low equipment requirements, and a high recovery rate. The process steps of the invention are that: adding 1000 ml of waste liquid into a three-mouth flask, adjusting the pH value to 2.0-3.0 with 20% hydrochloric acid, adding an extractant, controlling the temperature at 5-80 DEG C, stirring for 20-30 min, stopping stirring, transferring the mixed liquid into a separating funnel, allowing the liquid to stand for stratification; taking out the organic phase, adjusting the pH value to 9.0-9.5 with sodium hydroxide, transferring into a separating funnel, allowing the liquid to stand for stratification so as to remove the organic phase; heating the water phase to 50-60 DEG C, adding 5-25 g of active carbon for decoloration, filtering; cooling the filtrate, dropwisely adding 20% hydrochloric acid under stirring so as to adjust the pH to 2.0-3.0, performing crystal growing; performing suction filtration to obtain white sheet crystals, drying and weighing, calculating the yield, detecting the phenylacetic acid content.

The invention relates to a preparation method of a thickened oil aqua-thermolysis catalysis viscosity reducer with double structures of hydrogen supply and catalytic activity center. The preparation method is characterized by comprising the following steps of: 1) selecting raw materials, namely according to the mole ratio of dimethylbenzene to concentrated sulphuric acid to metal oxide to water of (1.5-2.5):(1.0-1.8): (0.3-0.6): (6-8), weighing the dimethylbenzene, the concentrated sulphuric acid, the metal oxide and the water; heating the dimethylbenzene to 100-120 DEG C, dropwise adding the concentrated sulphuric acid, and dripping off for 30-45 minutes; increasing the temperature to 130-150 DEG C, and continuing reaction for 2-3 hours; finishing the reaction and cooling to the room temperature, pouring the mixture solution into a liquid separation hopper, separating out the lower-layer solution to obtain a desired intermediate; and (3) mixing the metal oxide and water, adding the intermediate at 70-80 DEG C and stirring for 0.5-1h, filtering while being hot, drying the filtrate in a drying oven at 60-80 DEG C for 10-14 hours to obtain the product. The viscosity reducer prepared by adopting the method has a good viscosity reduction effect and is simple in preparation technique, and convenient and safe in site construction.

The invention relates to a separating funnel for extraction and an extraction instrument based on the separating funnel. The separating funnel comprises a funnel body, wherein a bottle hole is formed in the top end of the funnel body, and a bottle plug assembly is arranged on the bottle hole. The separating funnel is characterized by further comprising a venting pipe, wherein a venting hole is formed in the bottom end of the venting pipe and is located in the inner bottom of the funnel body, and a venting hole is formed in the top end of the venting pipe and is formed outside the funnel body. According to the separating funnel, the extraction can be realized by adding a small amount of solution, and in a similar way, the extraction instrument based on the separating funnel has the extraction function.