31results about "Stannous chloride" patented technology

The invention relates to an ordered ball type big mesoporous Alpha-Fe2O3 material, belonging to the technical filed of material preparation. The ball type big mesoporous Alpha-Fe2O3 material with an aperture diameter of 37 plus or minus 3nm and an aperture wall of 12 plus or minus 2nm, which orderly extends along the three-dimensional direction, is obtained by taking the polymethacrylic methyl rosmarinate milk-globule the ball diameter of which is 71 plus or minus 5nm and the colloidal crystals which are closely accumulated and distributed along the three-dimensional direction as templates, and through dipping the templates by the ethanol-water mixture of FeC2O4.2H2O, and then removing the PMMA templates through heating, solidifying and roasting. The structure and the magnetic performance of the big mesoporous are determined into a novel ordered ball type big mesoporous Alpha-Fe2O3 material through SEM, TEM, XRD and N2 adsorption test and squid. The material of the invention has the advantages of crystal aperture wall, particular ball type big mesoporous and weak ferromagnetism. The material can be used for preparing for catalyst and sensor.

The invention relates to a preparation method of stannous chloride, and belongs to the technical field of inorganic stannum preparation. The method comprises the following steps: carrying out one-step synthesis of a stannous chloride solution through applying supersonic waves having frequencies of 20-30kHZ to raw materials comprising metallic stannum flowers and hydrochloric acid having a concentration of 25-34wt%, and concentrating and crystallizing to obtain colorless and transparent stannous chloride crystals. The method provided by the invention, which introduces the supersonic waves to the reaction process, overcomes disadvantages of high reaction temperature, large hydrochloric acid volatilization amount and long reaction time of present stannous chloride preparation technologies, has the advantages of low cost, low acid consumption, fast reaction rate, less hydrochloric acid volatilization and easy industrialization, and has a bright application prospect.

The invention provides a method for preparing reagent-grade stannous chloride dehydrate crystals from industrial-grade raw materials. The method comprises the following steps: melting industrial tin ingots and quenching the molten industrial tin ingots into tin flower; then enabling reaction between filtered industrial hydrochloric acid and tin hydroxide to produce stannic chloride pentahydrate; adding the tin flower into the stannic chloride pentahydrate solution; enabling heat-insulating reaction for 12-18 h at 100-105 DEG C; when the mass concentration of quadrivalent tin in the solution is detected to be less than 0.01%, concentrating under reduced pressure till the specific weight of the solution is 2.0-2.4; filtering the solution into a cooling device to be cooled for 12-20 h at 0-10 DEG C; then discharging; carrying out vacuum suction filtration and centrifugal separation to obtain the required reagent-grade stannous chloride dehydrate crystals. The preparation method is short in process route, simple to operate, easy for processing parameter control and relatively high in production efficiency; the obtained product can meet the standards of the reagent-grade (high-purity) stannous chloride dehydrate crystals without crushing or screening, and can satisfy the requirements of industries (such as chemical analysis, catalytic synthesis and PCB colloid-Pd sensitization) which demand much on the quality of stannous chloride.

The invention discloses a preparation method of premium-grade stannous chloride from low-tin waste residues. The invention comprises the following steps: preparing a reaction solution, introducing chlorine, settling, settling for a second time, filtrating, concentrating, freeze crystallization and solid-liquid separation, wherein the obtained solid is the premium-grade stannous chloride. According to the invention, low-tin waste residues produced in tin manufacturing process are used as raw materials, various indexes of the stannous chloride product are controlled through acidity, concentration and time, and multiple setting, filtering and concentrating are performed to remove impurities, so as to obtain premium-grade stannous chloride products. The preparation method disclosed by the invention is simple in process, low in cost and environmentally friendly, provides a new way for recycling of low-tin waste residues produced in a tin manufacturing process and satisfies requirements of circular economy.

The invention discloses a preparation method of a toothpaste-grade tin chloride. The preparation method comprises the following steps: (i) synthetic reaction and primary filtration: adding deionized water, anhydrous tin tetrachloride and metallic tin into a reaction kettle according to a molar ratio of (4-8): 1: (1-1.2), and then adding concentrated hydrochloric acid to carry out synthetic reaction and primary filtration; (ii) purification and secondary filtration: adding excessive sulfuric acid into a purifying kettle, and then adding an appropriate amount of toothpaste-grade strontium chloride to carry out purification and secondary filtration; (iii) carrying out distillation and crystallization; (iv) carrying out vacuum drying, thus obtaining a finished product of dry white crystal toothpaste-grade tin chloride. The preparation method disclosed by the invention is stable in process, easy to control, low in cost and little in three wastes; the synthesized toothpaste-grade tin chloride is stable in quality and accords with addition standards of toothpaste.

The invention relates to a chlorine introducing method and a chlorine introducing device, in particular to a chlorine introducing method and a chlorine introducing device for producing stannous chloride by liquid chlorine. The method comprises the following steps of: introducing liquid chlorine into a coiled tube to be heated and gasified, introducing chlorine to a chlorine introducing tank for use, and heating the coiled tube by external hot water at the temperature of between 40 and 60 DEG C. The device comprises a liquid chlorine cylinder, the toiled tube, a heating water tank and a chlorine buffer tank, wherein the coiled tube is arranged in the heating water tank; an inlet of the coiled tube is communicated with the liquid chlorine cylinder, and an outlet of the coiled tube is communicated with the chlorine buffer tank; and the chlorine buffer tank is communicated to the chlorine introducing tank. In the method and the device, an operating mode of the natural gasification of the liquid chlorine is changed, and the liquid chlorine is introduced into the coiled tube in liquid mode and is heated by utilizing the coiled tube to accelerate the gasification speed of the liquid chlorine and improve the efficiency of a chlorination reaction in stannous chloride production; and the requirement of the production on the speed of a chlorine introducing reaction can be met only by opening one cylinder of liquid chlorine (one ton/cylinder), and the reliability of safety performance of the liquid chlorine during use is enhanced.

The invention discloses a synthetic method of stannous chloride. The method comprises the following steps: by using anhydrous stannic tetrachloride and hydrochloric acid with concentration of 20 wt% as raw materials, adding a precious metal catalyst, heating to 110 to 140 DEG C, introducing hydrogen with the pressure intensity of 1.5 to 3MPa, performing heat insulation reaction for 2 to 6 hours at125 to 135 DEG C, and performing press filtration to obtain a stannous chloride solution and a dilute hydrochloric acid solution with required concentrations; then performing concentration and crystallization to obtain a stannous chloride crystal. According to the synthetic method of stannous chloride disclosed by the invention, by using hydrogen as a reducing agent, a catalyst can be reacted andrecycled for being reused, and the phenomenon that tin is used as the reducing agent in a conventional process is avoided, so that the interference of impurity elements carried by metal tin on the quality of a product is effectively eliminated. The method disclosed by the invention has the advantages of stable process, strong operability, low cost, environment-friendly property, high security andthe like, and can be applied to industrial popularization.

The invention relates to a dynamic crystallization technological method and device for a stannous chloride solution. The technological method comprises the following steps of: A, adding a stannous chloride concentrated solution into rotation equipment with a clamping sleeve; B, introducing a coolant into the clamping sleeve of the rotation equipment; C, starting the rotation equipment, controlling the rotation speed of the rotation equipment to be 2-5r/min, and controlling the temperature difference between the stannous chloride concentrated solution and the coolant in the whole crystallizing process to be 5-10 DEG C, and D, ending crystallization when the concentration temperature T of stannous chloride is not more than 10 DEG C, stopping introduction of the coolant and the rotation equipment, spinning to dry slurry crystal in the rotation equipment in a centrifuger, and packaging to obtain a product of the stannous chloride. In the invention, the traditional static crystallization mode of the stannous chloride solution is changed into a dynamic crystallization mode, and the advantages of improved production efficiency, high crystallization rate, uniform particle sizes of stannous chloride crystals and simplified crystallization production process are achieved.

The invention discloses a preparation method of stannous chloride dehydrate. The method comprises the following steps: 1, adding a hydrochloric acid solution and metallic tin into a reactor; controlling the reaction temperature to be 40-70 DEG C; dropwise adding a hydrogen peroxide solution to dissolve metallic tin, adding metallic tin, reducing Sn<4+>, filtering, adjusting the pH value of an obtained filtrate to 0.5-1.5, concentrating the filtrate, adding metallic tin into the filtrate at the same time, inhibiting Sn<2+> oxidation, and stopping concentration when the density of the filtrate reaches 2.0-2.3 g/mL so as to obtain a concentrated solution; and crystallizing the concentrated solution at 0-5 DEG C, separating out precipitated stannous chloride crystals, and drying to obtain stannous chloride dehydrate. The preparation method disclosed by the invention is simple in process route, can remarkably improve the reaction rate, shorten the reaction time, and effectively reduce the temperature required by the reaction; concentrated hydrochloric acid and chlorine are not needed in the reaction process; the preparation method is environment-friendly, high in process safety and highin product purity.

The invention discloses a method for reducing stannic chloride. Aluminum particles are taken as a reducing agent in the method. The method comprises the following specific steps: adding diluted hydrochloric acid solution of stannic chloride generated by reducing diazonium salt with stannous chloride into a corrosion-resistant device provided with a tail gas air induction emptying system and a stirrer; starting stirring; slowly heating up and slowly adding the aluminum particles at the temperature of 20-55 DEG C for reaction; centrifugally drying after no divalent stannum is detected in the solution; and obtaining simple substance stannum after the reaction is finished. According to the method, the disadvantages in the prior art are overcome, and the method is simpler, convenient and environment-friendly, low in cost and high in yield and is more beneficial to reducing stannic chloride in industrial production.

The invention discloses a method for reducing lead content in stannous chloride. The method comprises the following steps of (1) dissolution: dissolving stannous chloride in water and preparing into a stannous chloride solution; (2) adjustment of a pH value: adjusting a pH value of the stannous chloride solution to 8-9 with an alkaline solution and heating to a temperature of 60-80 DEG C with stirring; (3) lead removal: dropwise adding a certain amount of a barium chloride-sodium carbonate solution into the stannous chloride solution with the pH value adjusted, controlling a reaction end point to a natural pH value, wherein a ratio of the amount of barium chloride to that of lead ions in stannous chloride is 20-60:1; and a ratio of the amount of substance of sodium carbonate to that of barium and lead ions is 13:12; and (4) solid-liquid separation: separating the stannous chloride solution with the lead removed by centrifugation and removing the precipitate. Lead content of high lead stannous chloride is reduced to below 0.005% through a barium carbonate co-precipitation method, thereby producing low lead stannous pyrophosphate. The lead content of the product can reach an industrial standard.

The invention relates to the technical field of preparation methods of stannous chloride crystals, and provides a method for preparing stannous chloride crystals by utilizing PCB tin stripping waste liquid, which comprises the following steps: washing tin hydroxide solids recovered from the PCB tin stripping waste liquid, dissolving tin hydroxide into a tin tetrachloride solution by using hydrochloric acid, reducing the stannous chloride solution the stannous chloride solution through a diaphragm electrolysis method, further purifying and concentrating the stannous chloride solution under reduced pressure, performing cooling to obtain clean and white stannous chloride crystals, and stannous chloride prepared through the method is free of caking, good in liquidity and free of crushing and screening. According to the method, the stannic chloride solution is reduced into the stannous chloride solution through diaphragm electrolysis, a traditional process for reducing the stannous chloridesolution mainly through a metallic tin ingot is replaced, expensive metallic tin is saved, and the production efficiency is greatly improved.

The invention discloses a hydrothermal synthesis method of stannous oxide nanosheet. 0.677-1 g of stannous chloride and 0.24-0.5 g of sodium hydroxide are respectively dispersed in mixed solutions ofethanol and deionized water to obtain a solution A and a solution B, mixing and stirring the solution A and the solution B for 2.5 h to obtain a milky yellowish colloidal product; and the obtained milky yellowish colloidal product is placed in a reactor for reaction at 120 DEG C for 8 h, pumping filtration is carried out, the product is alternately washed with deionized water and ethanol for threetimes, a small part of a sample at an upper layer is white, most of the sample at a lower layer is black, and the black sample at the lower layer is placed into a baking box for drying to obtain nano-flake stannous oxide. The hydrothermal synthesis method of the stannous oxide nanosheet of the invention is high in efficiency, low in cost, environmentally friendly and easy in storage.

The application of tin hemispheres in the preparation of tin chemical products is to make tin ingots into hemispherical tin raw materials for the synthesis of tin-containing chemical products. The invention can reduce friction and corrosion of equipment, reduce equipment investment, reduce labor intensity of workers, reduce energy consumption, improve production efficiency and product quality stability.

The invention discloses a method for preparing stannous chloride by recycling diluted hydrochloric acid tail gas, which comprises the steps of adding hydrochloric acid and tin into a concentrated hydrochloric acid reactor, heating, reacting to form stannous chloride liquid, and gradually concentrating; generating dilute hydrochloric acid tail gas mixed by HCl steam and water vapor through reaction, entering a heat exchanger, feeding cold dilute acid salt in a cold dilute hydrochloric acid storage tank into the heat exchanger at the same time so as to obtain hot dilute hydrochloric acid by heating cold dilute hydrochloric acid through the hot dilute hydrochloric acid tail gas, feeding into a hot dilute hydrochloric acid heat preservation storage tank to be stored for standby application, and condensing the diluted hydrochloric acid tail gas and returning to a cold diluted hydrochloric acid storage tank for later use; and pumping the hot diluted hydrochloric acid in the hot diluted hydrochloric acid heat preservation storage tank into a diluted hydrochloric acid reactor, adding tin into the diluted hydrochloric acid reactor for reaction to prepare a stannous chloride solution, pumping the stannous chloride solution into a concentrated hydrochloric acid reactor for concentration after the reaction is completed, and then discharging, cooling and crystallizing to obtain stannous chloride crystals. The method can directly recycle dilute hydrochloric acid tail gas to prepare stannous chloride, and is energy-saving, environment-friendly and efficient.