31 results about "Anthraquinone process" patented technology

The invention relates to the technical field of hydrogen peroxide preparation through an anthraquinone method, in particular to a working solution regeneration treatment method and device in the process of hydrogen peroxide preparation through the anthraquinone method, and the method comprises the following steps: step 1, adsorbing and removing moisture in a working solution by adopting a solid alkaline material; step 2, applying an electric field to the working solution, so that water drops mixed in the working solution are charged; step 3, enabling the working solution to flow along a surface with sieve pores, applying another electric field on the surface, enabling the electrified water drops to move towards the surface under the action of the electric field, enabling the water drops to be polarized and subjected to electrostatic induction by the electric field, enabling two ends of the water drops to be charged with opposite charges to form induced dipoles, enabling positive and negative dipoles of adjacent water drops to attract each other, colliding with each other, and coalescing into large water drops, large water drops are discharged along the surface with the sieve holes; 4, the working solution is transferred to a carclazyte bed, a degradation product is reduced into anthraquinone, and then the working solution repeatedly enters a hydrogenation workshop section. The method has the following beneficial effects that the regeneration effect is good, the cost is low, and the service life of aluminum oxide is prolonged.

The application provides an extraction device and process for producing hydrogen peroxide by an anthraquinone method. The device comprises an extraction tower, a high-concentration hydrogen peroxide discharge port arranged at the bottom of the extraction tower, a feed inlet arranged at the lower part of the extraction tower, and a water inlet arranged at the upper part of the extraction tower. A raffinate phase discharge port is arranged at the top of the extraction tower and is connected to a raffinate separator through a pipeline. A light phase outlet is arranged at the upper part of the raffinate separator, and a heavy phase outlet is arranged at the lower part of the raffinate separator. The heavy phase outlet is connected to multiple outlet pipelines according to different hydrogen peroxide concentrations after passing through a hydrogen peroxide concentration controller. The outlet pipeline with low hydrogen peroxide concentration is connected to a back feeding port of the extraction tower. The device and process can realize high extraction concentration, high extraction efficiency, controllable product concentration, and the like. Meanwhile, the device is provided with a safety interlocking system, which can effectively reduce the risk of over-temperature and over-pressure accidents.

Described is a catalyst obtained by supporting magnesium and cerium on activated alumina, firing same to immobilize the metals, and then impregnating same with palladium and performing reduction thereon, and is applied, when hydrogen peroxide is prepared by means of an anthraquinone process, to operation solution regeneration or hydrogenation, and thus an efficient regeneration conversion rate or synthesis yield is achieved.

The invention belongs to the technical field of catalyst preparation and application, and particularly relates to a method for large-scale preparation of a supported palladium monatomic catalyst and application of the catalyst in production of hydrogen peroxide by an anthraquinone method. The preparation method comprises the following steps: dissolving palladium chloride and an aryl complex or a palladium amine complex in a mixed organic solvent; then dipping with a gamma-Al2O3 microsphere carrier with a specific crystal phase according to a certain mass ratio; then reducing a palladium monatomic precursor in situ through an ultraviolet irradiation method; and carrying out medium-low temperature hydrogenation to obtain the supported palladium monatomic catalyst. The large-steric-hindrance monatomic dispersion technology and in-situ carrier regulation and control are combined, large-scale production of the catalyst is achieved, and the obtained catalyst has high activity, high dispersity and excellent mechanical property and stability, is suitable for hydrogenation reaction in anthraquinone process hydrogen peroxide production, and has wide application prospects. The equivalent hydrogenation efficiency can be improved, and the production cost of the catalyst can be reduced.

The utility model discloses an anthraquinone process hydrogen peroxide palladium catalyst in-situ regeneration device, and belongs to the field of catalyst regeneration. The regeneration device comprises an in-situ regeneration hydrogenation tower, a purging unit is arranged in the in-situ regeneration hydrogenation tower, a gas inlet of the purging unit is connected with a steam pipeline and a nitrogen pipeline outside the tower, the in-situ regeneration hydrogenation tower is provided with a soak solution inlet and a waste liquid outlet, and the soak solution inlet is connected with an ethanol tank, an acetic acid tank, a thermionic water tank and a soft water tank. The in-situ regeneration hydrogenation tower is provided with a vacuumizing pipe orifice; and the vacuumizing pipe orifice is connected with a vacuumizing system. Compared with the prior art, the regeneration device disclosed by the utility model can thoroughly remove all inorganic and organic impurities on the palladium catalyst, is high in regeneration efficiency and low in cost, and has good popularization and application values.

The utility model discloses an anthraquinone recovery device which comprises a heavy aromatics soaking pool, a heavy aromatics anthraquinone recovery pipe and a heating device, and by utilizing the characteristic that the solubility of anthraquinone in heavy aromatics is large, in the process of producing hydrogen peroxide by an anthraquinone method, a replaced waste filter element containing a large amount of anthraquinone is put into the heavy aromatics soaking pool, and the heavy aromatics anthraquinone recovery pipe is used for recovering the heavy aromatics. The heavy aromatics soaking pool is heated through the heating device, residual anthraquinone on the filter element is fully dissolved in the heavy aromatics soaking pool, a heavy aromatics solution containing anthraquinone enters the anthraquinone recovery system through the heavy aromatics anthraquinone recovery pipe, anthraquinone is fully recycled, waste of anthraquinone is avoided, and meanwhile, the utilization rate of the heavy aromatics is improved. The harm of wastes to the environment is greatly reduced.

The application discloses a process method for conversion of working liquid solvent in hydrogen peroxide production and belongs to the technical field of hydrogen peroxide production. The process method realizes conversion between acetic ester system and tetrabutylammonium system of working liquid solvent by improving process parameters of hydrogenation, extraction and white clay bed regeneration among anthraquinone method hydrogen peroxide solvents. The application can be used by mutual conversion according to market raw material price change, maximally reduces raw material cost, meets diversified chemical production, meanwhile, the process method can reduce system acidity, reduce hydrogenation side reaction, reduce alumina consumption and reduce energy consumption in the running process.

This invention discloses a one-step method for synthesizing metal-organic framework materials encapsulating high atomic number oxides and its application in the green catalytic synthesis of hydrogen peroxide using high-energy radiation. This invention utilizes high atomic number-doped metal-organic framework materials as catalysts, dispersing them in water while maintaining an oxygen atmosphere. Hydrogen peroxide is then obtained using high-energy radiation such as X-rays, gamma rays, alpha rays, and electron accelerators. This method is simple; compared to the industrial anthraquinone method, it does not require large-scale equipment and is pollution-free; compared to electrocatalysis, it does not require the addition of electrolytes; compared to direct hydrogen-oxygen synthesis, it does not require mixing hydrogen and oxygen, eliminating the risk of explosion; and compared to photocatalysts, it does not require additional sacrificial agents. Hydrogen peroxide can be synthesized in pure water, which facilitates subsequent separation and collection. This invention enables the synthesis of H2O2 in pure water, possessing significant economic value and broad application potential.

The application discloses a method for preparing hydrogen peroxide by photocatalysis without a sacrifice agent based on naphthalene imide / perylene imide polymer. The naphthalene imide / perylene imide polymer photocatalyst is synthesized by a hydrothermal method, and the catalyst can catalyze the reaction of oxygen and water to prepare hydrogen peroxide by photocatalysis without adding a sacrifice agent. The naphthalene imide / perylene imide polymer synthesized by the application is a photocatalyst with a donor / acceptor electron transport interface, and the structure greatly improves the electron-hole transport rate, thereby promoting the generation of hydrogen peroxide and inhibiting the decomposition of hydrogen peroxide. The application first applies the naphthalene imide / perylene imide polymer catalyst to the field of photocatalytic preparation of hydrogen peroxide. Compared with the industrial anthraquinone method and the method for preparing hydrogen peroxide by electric and thermal catalysis, the application is safe and environmentally friendly, simple to operate and low in cost.

The invention discloses a concentration process for hydrogen peroxide production extraction reaction, and belongs to the technical field of hydrogen peroxide production. The technical problem to be solved is that in an existing extraction process for producing hydrogen peroxide through an anthraquinone method, the concentration of hydrogen peroxide obtained through extraction is low, and the requirement of the market for high-concentration hydrogen peroxide is difficult to meet. According to the technical scheme, the concentration process of the extraction section in hydrogen peroxide production is characterized by comprising the following steps: pumping an acidic pure water extraction agent and a working solution into an extraction tower according to a flow rate ratio of 1: (53-60), carrying out reverse mass transfer extraction separation, and enriching acidic components to obtain hydrogen peroxide; the acidity of the acidic pure water extraction agent is 0.25-0.35 g / L, and the temperature is 50-55 DEG C; the working solution is a mixture of anthraquinone, heavy aromatics and a polar solvent.

The utility model discloses a working solution reaction device for anthraquinone process hydrogen peroxide. The working solution reaction device comprises a vertically arranged reaction outer cylinder, each partition plate comprises two grating plates which are oppositely arranged up and down, the outer edges of the grating plates are connected to the inner wall of the reaction outer cylinder, a containing bin is formed between the two grating plates, and the four partition plates are arranged at intervals in the axial direction of the reaction outer cylinder; each flow guide cylinder is provided with two closed ends and is provided with a plurality of liquid penetrating holes, the hole diameter of each liquid penetrating hole is smaller than the particle size of a palladium catalyst, a plurality of flow guide cylinders are installed in the containing bins except the containing bin on the top layer, the flow guide cylinders are arranged in the axial direction of the reaction outer cylinder, and the diameters of the flow guide cylinders are gradually increased downwards layer by layer; and the number of the guide cylinders arranged in each layer of accommodating bin is the same. The utility model solves the problems that the resistance of a bed layer is increased and a catalyst is easy to block after a fixed bed in a working solution hydrogenation stage in the production process of hydrogen peroxide by an anthraquinone process is used for a period of time.

The application discloses a kind of high-efficiency condensing separation equipment for anthraquinone hydrogen peroxide production, anthraquinone hydrogen peroxide technical field, including: pipe box section and separation section, pipe box section is equipped with symmetrically arranged upper tube sheet and lower tube sheet, baffles are arranged staggeredly between upper tube sheet and lower tube sheet, a plurality of vertically arranged heat transfer tube bundles are inserted between baffle, heat transfer tube bundle is located in the separation section and is sleeved with back cooling section, both sides of back cooling section are respectively communicated with pipe box section, one side of pipe box section is equipped with cold flow inlet, and the other side of pipe box section is equipped with cold flow outlet, cooling medium flows into pipe box section through cold flow inlet, one way along baffle and passes through cold flow outlet, another way along back cooling section recondenses heat transfer tube bundle and converges with one way along baffle and passes through cold flow outlet.This application has high condensing efficiency and good condensing effect, improves the use efficiency of equipment and increases the operating efficiency of heat exchange, improves the reliability of equipment, and increases the production performance.

This invention discloses a working solution for synthesizing hydrogen peroxide via the anthraquinone method, comprising a solvent and a working carrier. The solvent comprises aromatic hydrocarbons, diisobutylmethanol, and terephthalamide derivative A. Terephthalamide derivative A, by volume, has C9~C64... 10 The aromatic hydrocarbon comprises 30-95 parts, preferably 60-80 parts; the diisobutylmethanol comprises 2-20 parts, preferably 5-15 parts; and the terephthalamide derivative A comprises 5-30 parts, preferably 5-15 parts; the aromatic hydrocarbon is generally C9-C6. 10 Aromatic hydrocarbons; the working carrier is one or more of anthraquinone and its derivatives. This working solution exhibits excellent solubility and mass transfer capabilities for hydrogen, anthraquinone, and hydroanthraquinone, with a hydrogenation efficiency exceeding 13 g / L. It has low miscibility with water, good extraction and separation effects, and stable physicochemical properties. It can improve the production efficiency of the anthraquinone process for producing hydrogen peroxide and has promising prospects for industrial application.

The present invention relates to a process for the purification of an aqueous effluent (A) generated in the manufacture of hydrogen peroxide by the anthraquinone method, comprising the steps of a) adding to the aqueous effluent (A) an acid (C) and an organic solvent (B) to obtain a mixed medium (D); b) decanting the mixed medium (D) obtained in step a) to obtain 2 phases (E, F), wherein the aqueous phase (E) has a TOC content lower than the aqueous effluent (A) and the liquid organic phase (F) has a TOC content higher than the aqueous effluent (A); and c) entering the aqueous phase (E) obtained in step b) into a coalescer (4) to separate the aqueous phase (E) in 2 new phases, a first fluid (G) with a TOC content lower than the aqueous phase, and a second fluid (H) with a TOC content higher than the aqueous phase. Further, the present invention relates to an apparatus for the purification of an aqueous effluent generated in the manufacture of hydrogen peroxide by the anthraquinone method. Further, the present invention relates to the use of the inventive process in the manufacture of hydrogen peroxide by the anthraquinone method; and to a process for the manufacture of hydrogen peroxide and for the purification of an aqueous effluent (A) generated in said manufacture of hydrogen peroxide.

The invention relates to an anthraquinone process (AO) for producing hydrogen peroxide, in which the hydrogenation step is carried out by means of a catalyst which contains, in addition to palladium (Pd), at least one other metal and an amorphous catalyst support.

The application discloses an ionic COF catalyst, a preparation method thereof and application of the catalyst in photocatalytic production of hydrogen peroxide. The catalyst is prepared from 2,4,6-triformylphloroglucinol and a phenanthridine monomer containing a double amino group through Schiff base condensation reaction under catalysis of acetic acid in a mixed solvent, and has an ionic covalent organic framework structure connected with beta-ketoenamine. The catalyst prepared by the application has irregular sheet-like agglomeration, a layered porous structure, a high specific surface area and a controllable ionic microenvironment, and can simultaneously strengthen oxygen adsorption activation and photogenerated carrier separation efficiency. When the catalyst is applied to photocatalytic production of hydrogen peroxide, efficient production of hydrogen peroxide can be realized under the conditions of pure water, visible light and no sacrificial agent, and the yield can reach 457 μM h ‑1 The application provides a green, mild and sustainable new solution to solve the problems of high energy consumption and high pollution of the traditional anthraquinone method and the bottleneck problem of the existing COF photocatalytic performance.

The application discloses a ballast water sterilization reactor based on photocatalytic production of hydrogen peroxide and a use method thereof. Hydrogen peroxide water solution is obtained through a hydrogen peroxide production module and is transmitted to a mixing module to be mixed with untreated ballast water to obtain a mixed solution. Ocean microorganisms in the mixed solution are killed through a sterilization module to realize treatment of the ballast water. The ballast water sterilization reactor has simple structure and convenient operation. Only light source, water and oxygen are needed to safely and greenly produce hydrogen peroxide and apply the hydrogen peroxide to ship ballast water sterilization. The ballast water sterilization reactor solves the defects of high energy consumption, high transportation cost and unsuitability for use on ships of the traditional anthraquinone method.

The invention relates to the technical field of anthraquinone process hydrogen peroxide production, and discloses a method for reducing the total carbon content in an anthraquinone process hydrogen peroxide product, and the method comprises the following steps: in an oxidation system, introducing initial oxidation tail gas discharged by an oxidation tower into a separation unit, and carrying out cooling and separation treatment to obtain first aromatic hydrocarbon, second aromatic hydrocarbon and third aromatic hydrocarbon; circulating the first aromatic hydrocarbon back to the hydrogenation system and / or the oxidation system to be reused as a circulating working solution; and circulating the second aromatic hydrocarbon and / or the third aromatic hydrocarbon back to the hydrogen peroxide purification system to be reused as the extraction agent. The hydrogen peroxide production method provided by the invention is high in purification efficiency and low in cost, can maintain stable aromatic hydrocarbon mass fraction of a working solution system, and can further reduce the total carbon content of hydrogen peroxide.

The invention discloses an eggshell type catalyst for producing hydrogen peroxide through anthraquinone hydrogenation and a preparation method of the eggshell type catalyst, and belongs to the technical field of catalysts. Compared with the traditional uniform palladium catalyst, the active center of the eggshell-type palladium catalyst is intensively dispersed on the surface of the catalyst, so that the internal diffusion limitation is fundamentally overcome, and the utilization rate and the reaction selectivity of the noble metal are remarkably improved. The particle size equivalent diameter of the catalyst prepared by the method is 2mm, the specific surface area of the catalyst is 200m < 2 > / g, the pore volume is 0.3-0.9 cm < 3 > / g, the dispersion degree of palladium is 56%, and the strength of the catalyst is 80N / mm. The preparation method of the eggshell type catalyst for producing hydrogen peroxide through anthraquinone hydrogenation is simple and easy to operate, low in energy consumption and convenient for large-scale production and use, and has the advantage of promoting the progress of an anthraquinone process hydrogen peroxide production technology.

The application discloses a solvent system for working solution of hydrogen peroxide produced by an anthraquinone method, which comprises the following components: an imide derivative A and an aromatic hydrocarbon, wherein the imide derivative A is 5-60 parts, preferably 10-50 parts, and more preferably 15-35 parts, and the aromatic hydrocarbon is 30-95 parts, preferably 60-80 parts, in volume fraction. The solvent system for working solution of hydrogen peroxide produced by the anthraquinone method has good solubility to anthraquinone and hydrogen anthraquinone, low mutual solubility with water, stable physical and chemical properties, meets the use requirements of the anthraquinone method, can significantly improve the production efficiency of the anthraquinone method for producing hydrogen peroxide, and has a good industrial application prospect.

The invention discloses a D-pi-A type polymer based on a bisindeno-anthrazoline compound, a preparation method of the D-pi-A type polymer, and hydrogen peroxide produced by photocatalysis of the D-pi-A type polymer. The polymer is prepared through Suzuki coupling by taking a halogenated bisindeno-anthrazoline compound, 1, 4-phenylenediboronic acid and a halogenated donor molecule as monomers, the preparation method is simple, and the polymer has good absorption in a visible light range, has a short-range ordered structure and is beneficial to carrier separation and transmission. The D-pi-A type polymer based on the bisindeno-anthrazoline compound can catalytically synthesize hydrogen peroxide without a sacrificial agent under visible light irradiation and in an air atmosphere, and is excellent in performance. Compared with high energy consumption and multiple pollution defects of a traditional anthraquinone method and dependence on complex equipment of an electro-catalysis method, green synthesis of hydrogen peroxide is achieved only through water, air and light energy, the method has the comprehensive advantages of being high in activity, low in cost and environmentally friendly, and a new scheme is provided for the fields of clean energy and green chemical industry.

The invention discloses an electrochemical preparation method of hydrogen peroxide, and relates to the technical field of electrochemistry, the electrochemical preparation method of hydrogen peroxide comprises the following steps: S1, mixing an anthraquinone compound, an electrolyte and an organic solvent to obtain a catholyte; s2, the cathode electrolyte is subjected to an electrochemical hydrogenation reaction, and a hydrogenated solution is obtained; and S3, carrying out oxidation treatment on the hydrogenated liquid to obtain a hydrogen peroxide solution. Compared with a traditional anthraquinone method, the method disclosed by the invention is beneficial to improving the production efficiency and selectivity of hydrogen peroxide, synthesis can be realized at normal temperature and normal pressure, and the problems of high energy consumption and high production cost caused by high temperature and high pressure are avoided.

The application discloses a solvent system of working solution for hydrogen peroxide production by an anthraquinone method, which comprises the following components: aromatic hydrocarbon, imide derivative A and tri-octyl phosphate (TOP); the aromatic hydrocarbon is 30-95 parts, preferably 60-80 parts, the tri-octyl phosphate is 2-30 parts, and the imide derivative A is 2-30 parts in volume fraction. The working solution solvent system has good dissolving and mass transfer capacity for hydrogen, anthraquinone and hydrogen anthraquinone, the hydrogenation efficiency can reach more than 13 g / L, the mutual solubility of the working solution and water is low, the physical and chemical properties are stable, the working solution meets the use requirements of the anthraquinone method hydrogen peroxide production process, the production efficiency of the anthraquinone method hydrogen peroxide production process can be obviously improved, and the working solution has a good industrial application prospect.

The invention relates to the technical field of catalysts, in particular to a monatomic catalyst, a preparation method of the monatomic catalyst and application of the monatomic catalyst as a catalyst to production of hydrogen peroxide by an anthraquinone method. The preparation method comprises the following steps: dipping a carrier in a first metal precursor solution with a relatively high concentration, taking out, filtering, freeze-drying, and calcining in a mixed atmosphere of nitrogen and hydrogen to obtain a first metal-loaded carrier; and under a nitrogen atmosphere, dipping the carrier loaded with the first metal in a second metal precursor solution with a relatively low concentration, taking out, filtering, washing, and carrying out vacuum drying at room temperature to obtain the monatomic catalyst taking the second metal as an active component, the activity of the first metal is greater than that of the second metal. By controlling the preparation steps and the precursor concentration, the second metal which is low in density, dispersed in a monatomic mode and completely exposed is obtained on the carrier, and the loading capacity of the second metal is greatly reduced on the premise that high catalytic activity and stability are guaranteed.

The invention relates to the technical field of production regulation and control, and particularly discloses a green and efficient anthraquinone process fluidized bed hydrogen peroxide production system, which comprises an acquisition module for acquiring a scene set, a plurality of application demand data, production formula data and a plurality of historical production data; the first analysis module is used for determining a plurality of demand parameter sets and demand range sets; the second analysis module is used for determining a plurality of production parameter sets and a production range set of each formula environment equipment set; the determining module is used for determining candidate formula data of each application scene; the calculation module is used for acquiring real-time production data and calculating real-time formula data and a real-time environment equipment set; and the production module is used for determining an optimized operation value of each operation parameter, producing hydrogen peroxide in real time and realizing real-time regulation and control of the operation parameters. Precise linkage of scene requirements and production formulas can be achieved, the method adapts to multi-scene requirement differences, operation parameters are guaranteed to be optimal, resource waste and substandard products are reduced, and high efficiency and greenness of production are both considered.

The application discloses a working solution for producing hydrogen peroxide by an anthraquinone method, which comprises a solvent and a working carrier, wherein the solvent comprises p-phenylenediacetamide derivative A and heavy aromatic hydrocarbon, the heavy aromatic hydrocarbon is generally C7-C 10 The solvent comprises 5-50 parts of p-phenylenediacetamide derivative A and 30-95 parts of heavy aromatic hydrocarbon, preferably 10-30 parts and 60-80 parts respectively; and the working carrier is one or more of anthraquinone and its derivatives, preferably 2-alkyl anthraquinone, and further preferably 2-ethyl anthraquinone, 2-butyl anthraquinone or 2-pentyl anthraquinone. The working solution has good solubility for anthraquinone and hydrogen anthraquinone, low mutual solubility with water, stable physical and chemical properties, and can meet the use requirements of the anthraquinone method process, improve the production efficiency of the anthraquinone method process for producing hydrogen peroxide, and has a good industrial application prospect.

This application relates to an effective device for protecting the catalyst and a purification method based on the device, relating to the technical field of anthraquinone process for hydrogen peroxide production. The device includes a primary unit and a secondary unit. The primary unit includes a primary shell and a primary filter element. The filter element has an inner layer and an outer layer; the inner layer is a composite layer composed of one or two of polyester and glass fiber layers, and the outer layer is a cation exchange resin layer. The secondary unit includes a secondary shell and a secondary filter element; the filter element has a fluorine-containing material layer. The primary and secondary units, connected in series, purify the regenerated liquid, removing dust particles and metal ions through a systematic purification method. This mitigates the impact of dust particles and metal ions introduced into the regenerated liquid by the clay bed on the catalyst and the finished product, and addresses a series of problems during hydrogen peroxide production, such as high pressure drop in the hydrogenation tower bed, rapid activity decline, increased side reactions, and unstable hydrogen peroxide production.

The invention relates to the technical field of chemical production, in particular to a treatment method and a treatment system of a working solution in anthraquinone process hydrogen peroxide production. The treatment method comprises the following steps: introducing a working solution into an efficient pretreater, and sequentially carrying out membrane filtration and oxidation treatment; introducing the treated working solution into a multifunctional composite membrane purifier, and sequentially carrying out membrane filtration and alumina bed adsorption; and the treated working solution is introduced into an intelligent configuration repairing device, the pH value is adjusted to 7-8 through alkali washing, and treatment is completed. According to the treatment method, on the premise of safety and reliability, the purification and recovery efficiency and recovery quality of the hydrogen peroxide, the solvent and the working solution are effectively improved through multi-stage separation purification / repair of the working solution, and the treatment method has wide applicability and good application effect in anthraquinone process hydrogen peroxide production and has remarkable economic benefits, environmental benefits and social benefits.

The invention discloses a modification method and application of a titanium silicalite molecular sieve TS-1, and the modification method comprises the following steps: (1) mixing oxidation raffinate generated by an anthraquinone process hydrogen peroxide production device with water to prepare a modified mother solution; (2) mixing the modified mother liquor prepared in the step (1) with titanium silicalite molecular sieve TS-1 raw powder, and heating; and (3) cooling the solid-liquid mixture obtained in the step (2), filtering, washing, drying and roasting to obtain the modified titanium silicalite molecular sieve TS-1. According to the method, the oxidation residual liquid of the anthraquinone process hydrogen peroxide production device is used for a post-treatment procedure for preparing the titanium silicalite molecular sieve TS-1 catalyst, so that high-added-value reutilization of the hydrogen peroxide production industrial wastewater is realized, and the wastewater treatment cost is reduced. According to the present invention, the non-skeleton amorphous titanium species in the titanium silicalite molecular sieve TS-1 raw powder can be effectively removed, the operation method is simple and convenient, the cost is low, and the prepared titanium silicalite molecular sieve TS-1 has excellent performance in the cyclohexanone ammoximation process.

According to the technical scheme, the novel hydrogenation system comprises a working solution inlet pipe and a hydrogen inlet pipe, the working solution inlet pipe and the hydrogen inlet pipe are connected to the top of a gas-liquid mixer, and a bottom outlet of the gas-liquid mixer is connected with a bottom inlet of a hydrogenation tower; a top outlet of the hydrogenation tower is connected with a side inlet of the gas-liquid separator, a bottom outlet of the gas-liquid separator is connected to a next working section, and an emptying pipeline is arranged at the top of the gas-liquid separator. The hydrogenation tower has the beneficial effects that the feeding and discharging modes of the hydrogenation tower are changed, the phenomenon of bias flow of a working solution in the hydrogenation tower is reduced, a catalyst is fully soaked in the working solution, the utilization rate of the catalyst is improved, the hydrogen efficiency of the hydrogenation solution is improved by 5-15%, and the yield of hydrogen peroxide is improved.