2082 results about "Distillation" patented technology

The invention relates to a continuous production method of high-purity tetraethoxysilane, and belongs to the technical field of tetraethoxysilane preparation. The method comprises a raw material pretreatment stage and a purification and rectification stage: in the pretreatment stage, silicon tetrachloride and ethanol are subjected to an esterification reaction in a molar ratio of 1: (3-4) under the protection of nitrogen, the pH is adjusted to be neutral through triethylamine, and triethylamine hydrochloride is removed through reduced pressure distillation; then, a cerium oxide-molecular sieve composite adsorbent with the specific surface area larger than or equal to 800 m / g and the pore diameter of 2-5 nm is adopted for dehydration under the pressure of 0.8-1.2 MPa till the water content is smaller than or equal to 5 ppm, and volatile impurities are removed through high-purity nitrogen purging; in the purification stage, metal ions and Cl are synergistically removed through a titanate modified resin layer and a nano TiOtube layer, and then step-by-step separation is performed through a four-stage differential pressure rectifying tower. Through collaborative optimization of structural design of the composite adsorbent, construction of an organic-inorganic hybrid interface of the resin layer and pressure gradient rectification, 72-hour continuous production is achieved, the single-pass yield of the product is 92%, and the total amount of metal impurities is smaller than or equal to 5 ppb.

The invention relates to the field of chemical synthesis, in particular to a production process of allyl diethylene glycol dicarbonate, which comprises the following steps: by taking allyl alcohol and dimethyl carbonate as raw materials, carrying out transesterification under the action of a core-shell catalyst to generate dipropylene carbonate; carrying out solid-liquid separation, carrying out reduced pressure distillation to recover methanol and dimethyl carbonate, and then carrying out second-step ester exchange reaction with diethylene glycol under the action of the same catalyst to generate allyl diethylene glycol dicarbonate; and finally, performing multi-stage reduced pressure distillation purification to obtain a high-purity product. According to the core-shell type catalyst, an MCM-41 molecular sieve is used as a carrier, an inner core is formed after amino modification and zirconium ion coordination, then an interface layer and a phenyl modified silicon dioxide shell are used for packaging, and the core-shell type catalyst has high activity, high selectivity and excellent structural stability. The method has the advantages of mild process conditions, recyclable catalyst, high product yield and excellent purity, and is suitable for industrial production.

The invention provides a method for preparing polyarylester by interfacial polycondensation, which comprises the following steps: dissolving a diphenol monomer in an alkali solution to prepare a bisphenol salt solution, and dissolving an interfacial catalyst in a bisphenol salt water phase to obtain a water phase; dissolving aromatic dicarboxylic acid acyl chloride in a halogenated hydrocarbon solvent to obtain an organic phase; s2, slowly adding the organic phase obtained in the step S1 into the water phase in a stirring state within 10-60 minutes, and continuously reacting for 10-120 minutes in the stirring state; the product is separated out in the form of precipitate, the precipitated precipitate absorbs the halogenated hydrocarbon solvent, so that a liquid phase main body is water, a solid phase is a muddy product containing the halogenated hydrocarbon solvent, and the obtained muddy product is filtered, washed and dried to obtain a powdery product. According to the method disclosed by the invention, the polymer is directly precipitated by controlling the solute concentration and the mixing ratio, so that the efficient in-situ removal of the solvent is realized, the solvent is directly separated from water through simple filtration, and'zero separation, zero crushing and zero distillation 'is realized.

The invention provides an efficient technological method and system for preparing aromatic hydrocarbon through CO2 hydrogenation. The process method comprises the following steps: 1) mixing feed gas containing CO2 and H2 with recycle gas to obtain a mixture flow, and carrying out first-stage reaction on the mixture flow after heat exchange heating to obtain a first-stage reaction product; 2) performing heat exchange and separation on the primary reaction product to obtain a water phase, a gas phase and an oil phase, discharging the water phase out of the system, compressing most of the gas phase to obtain continuous circulating gas, and circulating the circulating gas back to the step 1) to continue the reaction; a small part of gas phase is discharged as purge gas; 3) distilling out light hydrocarbon from the top of the tower by rectifying the oil phase to obtain aromatic hydrocarbon-rich oil from a tower kettle; 4) heating the light hydrocarbon and then carrying out secondary reaction to obtain a secondary reaction product; and 5) carrying out heat exchange and separation on the secondary reaction product to obtain a gas-phase product and a liquid-phase product, discharging the gas-phase product as purge gas, and circulating the liquid-phase product back to the light component removal tower for rectification and separation to obtain aromatic hydrocarbon-rich oil. The first-stage reaction realizes high per-pass conversion of CO2, and the two-stage reaction is coupled to realize high selectivity of aromatic hydrocarbon.

The invention relates to the technical field of metallurgy, and provides a method and system for preparing a spongy TC4 alloy raw material, and the method comprises the following steps: heating and mechanically stirring titanium tetrachloride, aluminum trichloride and vanadium tetrachloride according to a component proportion required for preparing a TC4 alloy to form a uniform chloride mixture; the chloride mixture is subjected to a reduction distillation reaction in the presence of magnesium, and inert gas is continuously introduced in the reaction process for stirring; and after the reaction is completed, separating the byproduct magnesium chloride to obtain the spongy TC4 alloy raw material. According to the scheme, use of high-cost metal raw materials is avoided from the source, meanwhile, the complex steps of electrode preparation and repeated smelting are omitted through the one-step reduction distillation reaction, and energy consumption and time cost are greatly reduced.

The utility model relates to a negative-pressure crude benzene distillation system adopting a tubular furnace for heating. The negative-pressure crude benzene distillation system comprises a debenzolization tower, the tubular furnace and a crude benzene condensing, cooling and separating integrated device, the debenzolization tower is sequentially provided with a rectifying section, a stripping section, a storage tank section and a regeneration section from top to bottom; the crude benzene condensing, cooling and separating integrated device comprises a heat exchange tower and a separating tank; a low-temperature water heat exchanger is arranged at the lower part of the heat exchange tower; a crude benzene collecting section, an oil-gas-water separating section and a water collecting section are arranged in the separating tank; a first heating section and a second heating section are arranged in the tubular furnace. Compared with an existing negative-pressure crude benzene distillation process system, the negative-pressure crude benzene distillation process system has the remarkable advantages that the tail gas output is low, the tail gas is not discharged, the tube furnace operation temperature is low, the washing oil consumption is small, no additional separated water is generated, the one-time investment is low, and the like.

The utility model relates to the technical field of chemical engineering, in particular to a pH value system of a lean solvent / stripping water heat exchanger, which comprises a lean solvent / stripping water heat exchanger, a reflux pipeline, a heat exchanger inlet line, a heat exchanger outlet line, a lean solvent / feeding heater, an extraction distillation tower, a first outlet line and a second outlet line, one end of the reflux pipeline is connected to an outlet I of the lean solvent / stripping water heat exchanger, and the other end is connected to an inlet I of the lean solvent / stripping water heat exchanger; a shell pass outlet valve, a solvent regeneration tower, a solvent recovery tower, a recovery tower top air cooler, a recovery tower top water cooler, a reflux tank, a steam stripping water pump, a stripping water flow meter, a front valve, a stripping water regulating valve, a rear valve and a shell pass inlet valve are sequentially arranged on the reflux pipeline. The stable pH value in the system is ensured when the lean solvent / stripping water heat exchanger is overhauled, so that water circulates in the system, and the economic loss caused by continuous injection of monoethanolamine into the system is reduced.

The present invention belongs to the technical field of petrochemical catalysis, and relates to a preparation method for improving the stability of a Cu-Beta zeolite catalyst for preparing caprolactam from caprolactone, and the use thereof. In the present invention, a cavity-modified dealuminated Beta zeolite is used as a carrier, and copper is loaded in pore channels of the zeolite carrier by means of an improved ammonia distillation method. The cavity modification refers to subjecting the dealuminated Beta zeolite carrier to a desiliconization technique controlled by the use of a weak organic base so as to enlarge silanol nests generated by dealumination of the dealuminated Beta zeolite carrier, thereby better accommodating and stabilizing the nano and sub-nano copper particles. The core of the improved ammonia distillation method involves impregnating a zeolite carrier with an equal volume of a copper-ammonia complex solution, such that the copper-ammonia complex mainly undergoes, during ammonia distillation, a reaction of depositing copper hydroxide in zeolite pore channels, thereby improving the sintering resistance. The Cu-Beta catalyst prepared using the method provided by the present invention exhibits high activity, selectivity and stability when applied to the reaction of caprolactam prepared from caprolactone via gas-solid phase hydroamination.

The invention provides a preparation method of dicapryl carbonate, belongs to the field of preparation of dicapryl carbonate, and can solve the problems of unstable reaction system, low raw material conversion rate, low catalyst efficiency, poor phase contact effect, many side reactions, low product purity and poor quality in the existing preparation method of dicapryl carbonate. The preparation method of dicapryl carbonate comprises the following steps: fully mixing n-caprylic alcohol, a basic catalyst and a cosolvent, continuously dropwise adding low-grade dialkyl carbonate into the mixed solution for 5-10 hours through a liquid material distributor, carrying out ester exchange reaction, continuously extracting low-boiling-point substances, controlling the reflux quantity, and carrying out reduced pressure distillation to obtain the dicapryl carbonate. The method comprises the following steps: adding a cosolvent into a reaction solution, enabling the cosolvent with an initial addition amount to always exist in the reaction solution, after the reaction is finished, dealcoholizing by reduced pressure distillation, and removing impurities by washing to obtain a crude product of dioctyl carbonate, and rectifying to obtain a dioctyl carbonate product. The preparation method is high in raw material conversion rate and high in product yield, and the purity of the obtained product is gt; the content of impurities is low, and the method can be applied to preparation of cosmetics.

The invention discloses cyclodextrin alkyl ether sulfonic acid as well as a preparation method and application thereof, and relates to the technical field of oil and gas field auxiliaries. The preparation method of the cyclodextrin alkyl ether sulfonic acid comprises the following steps: adding hydroxyl alkyl sulfonic acid into dichloromethane, adding alkali and a sulfonyl chloride reagent, and reacting for 3-5 hours to obtain sulfonate; the preparation method comprises the following steps: adding sulfonate into iodide, adding acetone, reacting for 5-8 hours, and removing excessive iodide after the reaction is finished, so as to obtain iodo-hydrocarbyl sulfonic acid; the preparation method comprises the following steps: dissolving cyclodextrin in tetrahydrofuran, cooling to 0 DEG C, adding alkali under the protection of nitrogen, reacting for 0.5-2 hours, then adding iodo-alkyl sulfonic acid, reacting for 30-60 hours at room temperature, cooling to 0 DEG C, and carrying out reduced pressure distillation to obtain cyclodextrin alkyl ether sulfonic acid; the cyclodextrin alkyl ether sulfonic acid prepared by the invention is used as a cosolvent of the powder resistance-reducing agent, can effectively prevent aggregation among molecules of the powder resistance-reducing agent, improves the dispersity, reduces agglomeration and precipitation phenomena, and meanwhile, can avoid pipeline blockage in a conveying process.

The application discloses a double-hearth two-stage heating vacuum distillation furnace, which comprises an evaporation furnace and a condensation furnace which are communicated through a gas passage, wherein the evaporation furnace comprises an evaporation furnace body and at least one top heating mechanism which is detachably arranged on the top of the evaporation furnace body; and the condensation furnace comprises a condensation furnace body, a side heating structure and a furnace cover, wherein the condensation furnace body is divided into a temperature control condensation chamber and a plurality of layers of multistage condensation chambers, and the gas passage can be combined or replaced according to the required reaction conditions of different materials. The vacuum distillation furnace can collect different metals through the gradient change of the temperature of the two hearths, reduces the process of secondary distillation of volatile matters after the furnace is stopped, can complete the processing of diversified raw materials, improves the work efficiency and reduces the processing cost; the modular top heating mode directly radiates heat to the materials, improves the heat utilization rate, can realize the working mode of stopping the furnace without stopping the work, helps to improve the work efficiency, and is convenient for completing the furnace cleaning, maintenance and solid material taking and placing.

The invention relates to a method for preparing a gasoline component and an aviation fuel component through ethylene oligomerization, which comprises the following steps: contacting an ethylene-containing raw material with a first catalyst to carry out a first oligomerization reaction to obtain a first oligomerization product; the first catalyst comprises an FER structure molecular sieve; contacting the first oligomerization product with a second catalyst filled in the fixed bed reactor to carry out a second oligomerization reaction so as to obtain a second oligomerization product; the second catalyst is a molecular sieve catalyst and / or an amorphous silica-alumina catalyst; carrying out gas-liquid separation on the second oligomerization product to obtain a gas product and a liquid product, and carrying out distillation separation on the liquid product to obtain a C5-C9 fraction and a C9 + fraction; according to the method provided by the invention, the ethylene conversion rate is high, and the yield of C9 < + > fraction in the liquid product can be obviously improved.

The utility model discloses a device for continuously producing polyether. The device comprises a mixing kettle, a mixing kettle discharging pump, a receiving tank A, a receiving tank discharging pump A, a PO feeding pump, a static mixer, a pipeline reactor, a reactor discharging pump, an adsorption tower, an adsorption tower discharging pump, a receiving tank B, a receiving tank discharging pump B and a distillation tower, the method comprises the following steps: mixing an alcohol raw material and a catalyst in a mixing kettle, pumping into a receiving tank A for temporary storage, pumping the mixed material in the receiving tank A into a static mixer, mixing with epoxypropane, feeding into a pipeline reactor for reaction, pumping the reaction product in the pipeline reactor into an adsorption tower to remove metal elements introduced by the catalyst, a reaction product in the adsorption tower is pumped into a receiving tank B for temporary storage through an adsorption tower discharging pump, a reaction product in the receiving tank B is pumped into a distillation tower for distillation and purification, and purified polyether is obtained. By adopting the continuous production device, the energy consumption can be reduced, the generation of waste gas, waste residues and waste water is reduced, and the production cost is further reduced.

The invention discloses a method for improving molecular weight uniformity of polycarbosilane, and relates to the field of materials and chemical engineering. A packed distillation tower is additionally arranged in a polycarbosilane (PCS) reaction kettle, low-boiling-point small molecules in the reaction kettle in the synthesis process are distilled and separated out through the packed distillation tower, precise separation of the small molecules is achieved in combination with three-stage heating and a corresponding distillation mode, and the low-medium-boiling-point small molecules are removed in real time through rectification separation. The content of low-boiling-point components easily causing molecular weight fluctuation in the PCS is reduced, the randomness of the softening point of the PCS product is remarkably reduced, and the quality stability of the PCS is improved. And the temperature uniformity is improved, a reaction kettle with a larger volume is adapted, the problems of random molecular weight distribution, unstable softening point and the like of the existing PCS are effectively solved, and a reliable process is provided for preparing the high-quality PCS.

A hydrocarbon cleaning agent recovery and industrial wastewater reduction device belongs to the technical field of evaporation and concentration and comprises a distillation kettle, an evaporator, a first partition plate heat exchanger, a second partition plate heat exchanger, a cleaning agent liquid storage tank and a distilled water liquid storage tank. The distillation still is connected with the first partition plate heat exchanger and the second partition plate heat exchanger through the evaporator, the first partition plate heat exchanger is connected with the cleaning agent storage tank, the second partition plate heat exchanger is connected with the distilled water storage tank, the first partition plate heat exchanger is connected with the distillation still, and the second partition plate heat exchanger is connected with the evaporator. The equipment can simultaneously treat waste cleaning agents and waste water, does not need a cooling-water machine of traditional recovery equipment and a core component compressor of an evaporator, greatly saves equipment cost, and greatly reduces waste liquid treatment cost.

A process for the synthesis of methanol (MeOH) comprising the following steps: (a) passing a water-containing stream (3) through an electrolysis unit (4) to produce a cathode-side stream (5) comprising hydrogen (H2) and an anode-side stream (6) comprising oxygen (O2); (b) heat-exchanging said cathode-side stream (5) and optionally said anode-side stream (6) in one or more indirect heat exchanger(s) (7, 8, 32, 33) to obtain a cathode-side heat-exchanged stream (9) and optionally an anode-side heat-exchanged stream (10); (c) condensing said cathode-side heat-exchanged stream (9) to separate a liquid condensate product (11) and a syngas (12); said cathode-side stream (5) and / or said syngas (12) comprise carbon dioxide and optional carbon monoxide added through a separate stream (2); (d) compressing said syngas (12) in a compressor (27, 28) and then feeding compressed syngas (13) to a MeOH synthesis loop (14) wherein catalytic conversion of said compressed syngas (13) into MeOH is carried out under methanol synthesis conditions, thus obtaining a crude methanol stream (15); (e) distilling said crude methanol stream (15) in one or more distillation column(s) (16, 17) to give a refined MeOH product (19, 22); (i) recycling as feed to the electrolysis unit (4) at least a portion of at least one of: (A) a portion (31) of said compressed syngas (13); and / or (B) a bottom water stream (20) of a distillation column (16, 17).

The invention belongs to the technical field of brominated flame retardant synthesis, and particularly provides a decabromodiphenyl ethane bromine distillation process chlorination bromine removal process, which comprises the following steps: S1, adding bromine into a reaction kettle, adding a catalyst, and mixing; cooling and dropwise adding molten diphenylethane; then heating, carrying out a heat preservation reaction, and cooling to obtain a brominated crude product; s2, S201, adding the brominated crude product obtained in S1 into a bromine steaming kettle, and heating; s202, chlorine is introduced, and the total amount of bromine and chlorine is detected; carrying out segmented control on the introduced chlorine according to the total amount of bromine and chlorine; s203, when the total amount of bromine and chlorine is reduced to a threshold value, stopping introducing chlorine, standing, cooling, and introducing nitrogen; s3, filtering the feed liquid in the bromine steaming kettle, washing and purifying for three times, and finally, centrifugally dewatering to obtain a faint yellow solid; and S4, adding the faint yellow solid into a high-temperature jet mill, performing high-temperature aging to obtain white powder, and then performing jet milling on the white powder to obtain a finished product. Physical distillation is replaced by chemical replacement, so that bromine is highly separated.

The invention relates to a method for preparing norambrox ether from sclareolide. The method comprises the following steps: 1) preparing a red aluminum toluene solution; 2) dissolving sclareolide with toluene to obtain a sclareolide toluene solution, adding the sclareolide toluene solution into the red aluminum toluene solution for complete reaction, and quenching with a NaCl solution to obtain a reactant containing sclarediol; 3) carrying out oil-water separation on the reactant to obtain a primary organic phase and a water phase, so as to obtain an organic phase containing sclarediol; 4) carrying out a dehydration reaction on the organic phase containing sclarediol by using a molecular sieve, and after the reaction is completed, separating out an organic phase containing norambrox ether; 5, the organic phase containing the norambergyl ether is subjected to distillation concentration and crystallization separation, and a norambergyl ether product is obtained.According to the method, sclareolide is reduced through the red aluminum, and compared with lithium aluminum hydride, hydroboron and red aluminum, the red aluminum has the advantages of being good in stability, beneficial to industrialization, low in reaction temperature and safe.

The utility model relates to the technical field of waste liquid distillation, in particular to a waste liquid distillation retort which comprises a water container part and an auxiliary evaporation retort part, the water container part comprises a water container barrel and a water container lower sealing head, the water container lower sealing head is welded and fixed at the lower end of the water container barrel, and a transition conical barrel is welded and fixed at the upper end of the water container barrel. Water container supporting legs are fixedly arranged at the lower end of the outer wall of the water container barrel, the auxiliary evaporation tank part comprises an auxiliary evaporation tank barrel, an auxiliary evaporation tank upper sealing head and a steam pipe, a heating device is fixedly arranged on the outer wall of the water container barrel, the heating device comprises a heating pipe, a connecting flange and a heating connecting pipe, and a jacket treatment device is fixedly welded to one side of the water container barrel. The jacket treatment device comprises an integrated connecting pipe, a jacket liquid adding pipe, a pressure detection pipe, a jacket exhaust pipe and a safety valve connecting pipe, the integrated connecting pipe is welded and fixed to the outer wall of the water container barrel and communicated with the interior of the water container barrel, and the jacket liquid adding pipe, the pressure detection pipe, the jacket exhaust pipe and the safety valve connecting pipe are communicated to the upper end of the integrated connecting pipe.

The disclosure relates to a purification system and a purification bag (6) for use therein, configured for (solar) heat-driven water purification of contaminated water. The purification bag (6) comprises a distillation assembly (601,..60n), comprising: - a contaminated water chamber (30) for collecting contaminated water, the contaminated water chamber (30) comprising a top sheet configured for absorbing heat; - a purified water chamber (50) for collecting purified water, the purified water chamber (50) comprising a condensation sheet configured for collecting condensed purified water; - a membrane (40) arranged between the top sheet and condensation sheet, the membrane dividing the distillation assembly into the contaminated water chamber (30) and the purified water chamber (50), wherein the membrane (40) comprises a membrane sheet configured for separation of the associate part of the contaminated water portion received by the distillation assembly into the purified water portion and a residual water portion comprising water and contaminants remaining in the contaminated water chamber by at least one of membrane distillation and pervaporation through the membrane sheet; wherein the top sheet and the membrane sheet are polymeric sheets that are bonded to each other by welding according to a welding pattern.

The invention provides a method for analyzing the oxygen stable isotope ratio of water in a highly alcoholic beverage, and relates to the technical field of oxygen isotope analysis. The analysis method comprises the following steps: selecting at least two water samples with known oxygen isotope ratios and different values as additive water; diluting the same high-alcohol beverage to be detected by adding water to obtain a diluted sample; measuring an oxygen isotope ratio; and according to the oxygen isotope ratio of the added water and the oxygen isotope ratio of the diluted sample, calculating the oxygen isotope ratio of the water in the highly alcoholic beverage to be measured. According to the analysis method, the concentration of ethanol is reduced through dilution, so that interference of isobaric elements is avoided; and physical separation is replaced by mass conservation equation calculation, and a complex distillation device is not needed. According to the method, pretreatment is remarkably simplified, cost and errors are reduced, and rapid and accurate analysis of the water oxygen isotope in the highly alcoholic beverage is achieved.

The invention belongs to the technical field of comprehensive utilization of seawater resources, and particularly relates to a green circulation method and system integrating seawater desalination and high-efficiency bromine extraction of concentrated seawater, and the system comprises a seawater desalination unit, a pretreatment unit, an oxidation replacement unit, a bromine elementary substance blowing-out unit, a bromine elementary substance absorption and enrichment unit and a bromine rectification and purification unit which are sequentially connected in series, the pipelines of the units are communicated to form a continuous material channel; the seawater desalination unit is used for producing fresh water and enriching concentrated seawater; the pretreatment unit removes impurities through a security filter and adjusts pH through an acidification pool; the oxidation replacement unit mixes chlorine and concentrated seawater through a gas-liquid mixer, and a bromine solution is generated in a reaction tank; the stripping tower realizes bromine gas stripping through atomization spraying, a filler area and a gas distributor; the absorption tower enriches bromine into hydrobromic acid by using a sulfur dioxide aqueous solution; the rectification unit is oxidized by a distillation tower, condensed and separated to obtain liquid bromine. The method realizes synchronous recovery of fresh water and bromine resources, conforms to a green circulation concept, and has remarkable economic and ecological benefits.

A hydrometallurgical process for recovering a plurality of metals from a complex rare and precious material, comprising the following steps: step 1: adding a complex rare and precious material to a hydrochloric acid solution, adding an oxidant for reaction, and then performing filtration to obtain a chlorination liquid and a chlorination residue; step 2: using two-stage counter-current gold loading to obtain a gold-loaded liquid and a post-loading liquid, reducing the gold-loaded liquid, performing clarification to obtain an organic phase, and filtering a precipitate to separate a post-reduction liquid and sponge gold; performing evaporation and concentration on the post-reduction liquid to produce a concentrate 1 and a condensate; and cooling and crystallizing the concentrate, performing filtration to obtain residual oxalic acid, and returning the residual oxalic acid to the reduction process and a post-crystallization liquid to gold loading; step 3: performing low-temperature distillation on the post-loading liquid to obtain a concentrate 2; step 4: performing high-temperature distillation on the concentrate 2 to obtain a concentrate 3; step 5: performing directional crystallization and centrifugal filtration on the concentrate 3 to obtain a crystallization residue and selenous acid; and step 6: washing the crystallization residue by using cold water or a low-acid-level condensate produced in step 3, and performing filtration to obtain a tellurium residue and a palladium-platinum-rhodium-rich liquid.

The invention relates to the technical field of chemical equipment, and discloses a sodium carbonate production system adopting an ammonia-soda process. The system for producing sodium carbonate by the ammonia-soda process comprises a thin liquid distillation tower and a flash evaporation module. The thin liquid distillation tower is used for discharging waste thin liquid; the flash evaporation module comprises a second flash evaporation device and a water injection assembly; a steam outlet of the second flash tank is communicated with a steam inlet of the thin liquid distillation tower; the water inlet end of the water injection assembly is communicated with the thin liquid distillation tower, and the water outlet end of the water injection assembly is located in the second flash tank and used for discharging waste thin liquid to flush flash steam in the second flash tank. According to the invention, by arranging the water injection assembly, the waste thin liquid discharged from the thin liquid distillation tower is introduced into the second flash tank for flushing flash steam in the second flash tank so as to flush away droplets in the flash steam, and the content of calcium ions introduced into the thin liquid distillation tower can be reduced, so that the calcium ions in the waste thin liquid are reduced and even eliminated; and the waste thin liquid discharged from the thin liquid distillation tower can be used as filtering washing water.

The invention relates to the field of agilawood essence extraction, in particular to an agilawood essence substance extraction method which comprises the steps of raw material pretreatment, subcritical fluid extraction, molecular distillation purification, alcohol extraction and concentration and macroporous adsorption resin purification. According to the method, subcritical low-temperature extraction and molecular distillation technologies are combined, efficient, high-purity and sectional extraction of volatile essential oil and non-volatile essence substances in agilawood under the low-temperature condition is achieved, damage to thermosensitive components is effectively avoided, and no organic solvent is left.

The invention relates to the field of silane coupling agents, and discloses a preparation method of a sulfur-containing silane coupling agent, which comprises the following steps: step 1, mixing alkali metal sulfide with sulfur, stirring, and reacting to obtain a sodium polysulfide solution; step 2, adding a pH regulator, a hydrolysis inhibitor and a phase transfer catalyst into the sodium polysulfide solution, dropwise adding 3-halogen propyl trialkoxysilane, and stirring for condensation reaction to obtain a crude product reaction solution; 3, the crude product reaction liquid is sequentially subjected to distillation, decolorization with a decolorizing agent and filtration, and the sulfur-containing silane coupling agent is prepared after the steps are completed. The crystal water contained in the raw materials is used as a reaction medium, so that additional addition of an organic solvent and pre-drying and dehydration treatment are not needed, the spontaneous combustion risk of sodium sulfide is avoided, raw material pretreatment and solvent recovery procedures are omitted, and the whole technological process is simplified, so that the operation is simple and convenient, and the cost is low. The method is suitable for large-scale industrial production.

The application provides a synthesis method of p-benzoquinone dioxime. The synthesis method comprises the following steps: (1) adding solid acid into an ethanol solution of phenol to obtain a mixed solution A, then vacuumizing and filling with inert gas; dissolving nitrite into ethanol, uniformly mixing to obtain an ethanol solution of nitrite, then vacuumizing and filling with inert gas; in an inert gas atmosphere, adding the ethanol solution of nitrite into the mixed solution A dropwise to perform nitrosation reaction, to obtain a reaction liquid B; in the inert gas atmosphere, adding an ethanol solution of hydroxylamine into the obtained reaction liquid B to perform oximation reaction; after the reaction is completed, filtering the obtained reaction liquid C, performing reduced pressure distillation on the obtained filtrate, and performing washing, filtering and drying on the obtained residual liquid of the reduced pressure distillation, to obtain p-benzoquinone dioxime. The method provided by the application reduces the occurrence of side reactions, improves the conversion rate of the reaction, and improves the yield and purity of p-benzoquinone dioxime.

The invention relates to the field of comprehensive utilization of biomass energy, and particularly discloses a process for preparing biological coal based on atmospheric distillation of biochar and biological oil, which comprises the following steps: performing atmospheric distillation on unpickled biochar or pickled biochar and biological oil to finally obtain light fraction and biological coal; biochar which is not subjected to acid pickling or biochar subjected to acid pickling serves as an in-situ catalyst, rich pores and oxygen-containing functional groups of the biochar can synergistically catalyze bio-oil to be subjected to condensation polymerization such as esterification and etherification, and finally the prepared bio-coal is good in combustion performance and high in productivity; the process is simple and controllable, and large-scale industrial production is expected to be carried out.

The application discloses a continuous synthesis method of an amicarbazone intermediate 5-isopropyl-1,3,4-oxadiazole-2(3H)-ketone. The method comprises two continuous processes of hydrazinolysis and phosgenation: continuously feeding a mixture of isobutyric acid and a solvent, a mixture of hydrazine hydrate and a catalyst into a hydrazinolysis continuous reactor respectively, carrying out a warming reflux dehydration reaction, and obtaining an isobutyryl hydrazine solution shown in formula I; continuously feeding the isobutyryl hydrazine solution and phosgene into a phosgenation continuous reactor, carrying out a phosgenation reaction, and after distillation and desolventizing treatment of a reaction solution, obtaining 5-isopropyl-1,3,4-oxadiazole-2(3H)-ketone shown in formula II. The application has the advantages of simple reaction flow, high product yield, and significant production efficiency improvement, and is suitable for industrial large-scale production.

The invention discloses a production method of high-grade flavoring liquor of Luzhou-flavor liquor, and relates to the field of liquor brewing. Aiming at the problems of insufficient substrate conversion, easy unbalance of flavor and easy rancidification of fermentation in the traditional double-round fermentation process, the technical scheme of combining double-round fermentation of 15-20% of fermented grains at the bottom of a cellar, mother grain acidity / starch double-index screening, precise regulation and control of sterile air in three-round fermentation / feeding before entering the cellar, and segmented distillation and graded storage is adopted. The process can improve the fermented grain conversion efficiency and stabilize the acidity of a fermentation system; the content of characteristic flavor substances such as ethyl hexanoate is greatly increased, and the flavor ratio is balanced; the sensory quality of raw wine is improved, and the cellar aroma and the ester aroma are stronger. The technological parameter range is feasible through experimental verification, the technical effect is obviously superior to that of a traditional technology, and the method is suitable for producing high-quality Luzhou-flavor liquor.