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Stannous chloride dehydrate and preparation method thereof

A stannous chloride, dihydrate technology, applied in the directions of stannous chloride, tin halide, etc., can solve the problems of long reaction time, short process route, high reaction temperature, reduce the temperature required for the reaction, shorten the reaction time, The effect of high product purity

Active Publication Date: 2019-12-13
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has a short process route, and the product does not need cumbersome post-treatment steps, but its reaction time is long and the required reaction temperature is high.

Method used

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  • Stannous chloride dehydrate and preparation method thereof
  • Stannous chloride dehydrate and preparation method thereof
  • Stannous chloride dehydrate and preparation method thereof

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preparation example Construction

[0024] The invention provides a kind of preparation method of tin protochloride dihydrate, it comprises the steps:

[0025] (1) melting and quenching a tin ingot with a purity of 3.5N into tin flowers with a size of 1 to 10 mm;

[0026] (2) Add a certain amount of tin flower in the reaction vessel, then add an appropriate amount of hydrochloric acid solution with a mass fraction of 10% to 20% to submerge the tin flower, control the reaction temperature at 40 to 70°C, and then drop in a mass fraction of 10% to 20%. 30% hydrogen peroxide solution, react 3~8h, make tin flower dissolve, obtain the mixed solution that contains tin dichloride and tin tetrachloride; Wherein, the consumption ratio of hydrogen peroxide solution and tin flower is V(H 2 o 2 ): W(Sn)=2:1~4:1(mL / g), the rate of addition of hydrogen peroxide solution is 200~500mL / h;

[0027] (3) Add excessive tin flower in the mixed solution of step (2), react 4~8h, reduce the Sn in the solution 4+ , filter after the rea...

Embodiment 1

[0034] 500g tin flower and 1.5L hydrochloric acid solution (mass fraction 10%) were placed in the reactor, and 1000mL H was added dropwise at a speed of 200mL / h 2 o 2 solution (mass fraction 30%), after reacting at 70° C. for 5 hours, the tin flowers were completely dissolved to obtain a mixed solution containing tin dichloride and tin tetrachloride. Add excess tin flower to the above mixed solution to reduce Sn 4+ , after reacting for 5 hours, filter, adjust the pH of the filtrate to 1.5, and then concentrate under reduced pressure. When the density of the concentrated solution reaches 2.3g / mL (2.0-2.3g / mL is acceptable), the concentration is stopped, the concentrated solution is placed at 0°C (0-5°C is acceptable) for crystallization for 12 hours, and the crystal is placed under nitrogen protection Suction filtration under the atmosphere to remove the liquid in the upper layer of the crystals, and place the separated crystals in a vacuum oven at -0.9 bar (-0.75 to -0.9 bar...

Embodiment 2

[0037] 500g tin flower and 1.5L hydrochloric acid solution (mass fraction 15%) were placed in the reactor, and 1500mL H was added dropwise at a speed of 200mL / h 2 o 2 solution (mass fraction 20%), after reacting at 55° C. for 7.5 hours, the tin flower completely dissolves to obtain a mixed solution containing tin dichloride and tin tetrachloride. Add excess tin flower to the above mixed solution to reduce Sn 4+ , after reacting for 5 hours, filter, adjust the pH of the filtrate to 1.0, and then concentrate under reduced pressure. When the density of the concentrated solution reaches 2.3g / mL (2.0-2.3g / mL is acceptable), the concentration is stopped, the concentrated solution is placed at 0°C (0-5°C is acceptable) for crystallization for 12 hours, and the crystal is placed under nitrogen protection Suction filtration under the atmosphere to remove the liquid in the upper layer of the crystals, and place the separated crystals in a vacuum oven at -0.9 bar (-0.75 to -0.9 bar is ...

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Abstract

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.

Description

technical field [0001] The invention relates to the technical field of inorganic chemical industry, in particular to a stannous chloride dihydrate and a preparation method thereof. Background technique [0002] Tinous chloride dihydrate (SnCl 2 2H 2 O) As an important chemical raw material, it is widely used in industries such as dyes, fragrances, mirrors, and electroplating, and is used as daily necessities such as ultra-high pressure lubricating oil, bleaching agent, reducing agent, mordant, decolorizing agent, analytical reagent, and soap. flavor stabilizers, etc. [0003] At present, the main method of industrially synthesizing tin protochloride dihydrate is to adopt the concentrated hydrochloric acid method. The concentrated hydrochloric acid method is to react concentrated hydrochloric acid directly with metal tin under heating conditions to form a stannous chloride solution, and then prepare stannous chloride dihydrate products through evaporation, crystallization,...

Claims

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Application Information

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IPC IPC(8): C01G19/06
CPCC01G19/06C01P2006/80
Inventor 贾行伟朱刘王权罗洋
Owner 昆明先导新材料科技有限责任公司
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