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Preparation method of toothpaste-grade tin chloride

A stannous chloride, toothpaste-grade technology, applied in the field of preparation of toothpaste-grade stannous chloride, can solve the problems of low product purity, long synthesis process time, difficult use, etc., and achieve stable process, low cost, and less three wastes Effect

Active Publication Date: 2015-04-29
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, chlorine gas belongs to Class 2.3 poisonous and dangerous goods, which is difficult to use, and the synthesis process takes a long time. The highly toxic barium chloride is used as the anti-purifying agent for removing heavy metals. kg, cannot be used as a toothpaste additive

Method used

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  • Preparation method of toothpaste-grade tin chloride

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preparation example Construction

[0026] Such as figure 1 Shown, a kind of preparation method of toothpaste grade stannous chloride comprises the following steps:

[0027] (i) Synthesis reaction and primary filtration

[0028] Add deionized water into reaction kettle 1, then add concentrated hydrochloric acid, the amount of concentrated hydrochloric acid added is 3% to 8% of the total aqueous solution mass, then slowly add anhydrous tin tetrachloride dropwise, and finally put in metal tin, react The temperature is 110-120° C., and the reaction time is 1-3 hours. Wherein, the total aqueous solution quality refers to the sum of the aqueous solution contained in deionized water and concentrated hydrochloric acid; the molar ratio of deionized water, anhydrous tin tetrachloride and metallic tin is 4~8:1:1~1.2, the The mass concentration is 38%. The chemical reaction formula is:

[0029] Sn+SnCl 4 +4H 2 O→2SnCl 2 2H 2 o

[0030] The addition of concentrated hydrochloric acid effectively avoids the hyd...

Embodiment 1

[0039] 2.7kg of deionized water, 0.7kg of hydrochloric acid, 10kg of anhydrous tin tetrachloride, and 4.5kg of metal tin are added to the reactor successively, and the reaction temperature is 110°C, and the reaction time is 3h; after the reaction is completed, the metal solid impurities are filtered out; Add 42ml of sulfuric acid (10g / 100ml) to the filtrate, then add 42ml of strontium chloride (saturated solution), filter out solid impurities; take the clear solution and place it in a vacuum distiller for vacuum distillation with a vacuum of 0.01MPa and a temperature of 45 ℃; the distilled solution is introduced into the crystallization tank to stir and crystallize, the temperature is 0 ℃; after the white crystals are precipitated, the entire material system is placed in a centrifuge for solid-liquid separation, and the solid white crystals are put into a vacuum drying oven for drying , the vacuum degree is -0.05MPa, and the finished product is obtained. The weight of the obta...

Embodiment 2

[0041] 4.1kg of deionized water, 0.7kg of hydrochloric acid, 10kg of anhydrous tin tetrachloride, and 5.0kg of metal tin were added to the reactor successively, the reaction temperature was 115°C, and the reaction time was 2h; after the reaction was completed, the metal solid impurities were filtered out; Add 40ml of sulfuric acid (10g / 100ml) to the filtrate, then add 40ml of strontium chloride (saturated solution) to filter out solid impurities; take the clear solution and place it in a vacuum distiller for vacuum distillation with a vacuum of 0.03MPa and a temperature of 70 ℃; the distilled solution is introduced into the crystallization tank to stir and crystallize, the temperature is -5 ℃; after the white crystals are precipitated, the entire material system is placed in a centrifuge for solid-liquid separation, and the solid white crystals are put into a vacuum drying oven Drying, the vacuum degree is -0.08MPa, and the finished product is obtained. The weight of the obtai...

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Abstract

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.

Description

technical field [0001] The invention belongs to a preparation method of a toothpaste additive, in particular to a preparation method of toothpaste grade stannous chloride. Background technique [0002] In the oral care industry, stannous chloride is mostly used in anti-caries and desensitization toothpaste. Its main function is to reduce the solubility of enamel in acid and enhance the remineralization of enamel to prevent dental caries. [0003] The manufacture method of traditional tin protochloride is to directly react with metal tin and hydrochloric acid, evaporate and concentrate then, isolate tin protochloride dihydrate (SnCl 2 2H 2 O) crystallization. The method for preparing tin protochloride in the prior art, such as the Chinese patent "A Preparation Method of Tin Protochloride" (CN85106332) discloses the use of metal tin, chlorine gas and water to generate tin tetrachloride in the presence of hydrochloric acid, and then add metal Tin as a reducing agent method. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/06
Inventor 刘玉静王筠朱昱周红艳郑楠
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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