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A kind of preparation method of high-purity sodium sulfide crystal

A technology of sodium sulfide and crystals, which is applied in the field of preparation of high-purity sodium sulfide crystals, can solve the problems that the purity cannot meet the requirements of sodium sulfide purity, waste of resources, increase the cost of sodium sulfide crystal preparation, etc., to meet the concept of green chemical industry and realize Recycling, better economic value

Active Publication Date: 2021-02-23
GUIZHOU REDSTAR DEVING
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  • Claims
  • Application Information

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Problems solved by technology

But because the raw material that it adopts is refined sodium sulfide, therefore, undoubtedly increased the preparation cost of sodium sulfide crystal, also caused the waste of resources
For example, in the preparation method of the disclosed anhydrous sodium sulfide crystal of CN1308013A, the content of the sodium sulfide crystal obtained is more than or equal to 94%, and the appearance is light yellow, and its purity cannot meet the requirements of sodium sulfide in industries such as pharmaceutical intermediates, electrolysis, and the synthesis of sulfur-containing polymers. Purity requirements

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  • A kind of preparation method of high-purity sodium sulfide crystal
  • A kind of preparation method of high-purity sodium sulfide crystal
  • A kind of preparation method of high-purity sodium sulfide crystal

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preparation example Construction

[0027] Concrete, the invention provides a kind of preparation method of high-purity sodium sulfide crystal, comprises the following steps:

[0028] (1) Evaporate and concentrate the by-product sodium sulfide solution produced by the Glauber's salt method to obtain the sodium sulfide concentrate.

[0029] Wherein, the reaction equation of Glauber's salt method to produce barium sulfate is:

[0030] Na 2 SO 4 + BaS = BaSO 4 ↓+Na 2 S

[0031] In the process of producing barium sulfate by Glauber's salt method, in order to make barium sulfide react completely, the input amount of reducing production cost sodium sulfate is excessive. Therefore, in addition to Na in the by-product sodium sulfide solution 2 There is also sodium sulfate in addition to S. In addition, since Na 2 S and BaS are strong alkali and weak acid salts, which can be hydrolyzed in water to generate sodium hydrosulfide, sodium hydroxide, barium hydrosulfide, and barium hydroxide. Therefore, sodium sulfide...

Embodiment 1

[0050] The concentration of sodium sulfide in the sodium sulfide solution of the by-product sodium sulfide solution produced by Glauber's salt method is 5%, and the 80m 3 The by-product sodium sulfide solution is evaporated and concentrated to 35% by 2205 material evaporator. Then, take 6m 3 Put 35% sodium sulfide solution in a refining kettle, add 7kg of sodium hydroxide, stir at 120°C for 30min, solids precipitate out of the solution. Then, it is filtered by a filter press, and the filter cake is sent to the barium sulfate production system, and the filtrate is naturally cooled and crystallized to 70°C under stirring. After the crystallization is completed, dehydrate with a centrifuge, and the mother liquor is input into the evaporator, and the solid is cooled and sieved to obtain 2 tons of high-purity sodium sulfide crystals.

Embodiment 2

[0052] The concentration of sodium sulfide in the sodium sulfide solution of the by-product sodium sulfide solution produced by Glauber's salt method is 5%, and the 80m 3 The by-product sodium sulfide solution is evaporated and concentrated to 36% by 2205 material evaporator. Then, take 6m 3 Put 36% sodium sulfide solution in a refining kettle, add 8kg of sodium hydroxide, stir at 122°C for 35min, solids precipitate out of the solution. Then, it is filtered by a filter press, and the filter cake is sent to the barium sulfate production system, and the filtrate is naturally cooled and crystallized to 72°C under stirring. After the crystallization is completed, the centrifuge is used for dehydration, the mother liquor is input into the evaporator, and the solid is cooled and sieved to obtain 2.1 tons of high-purity sodium sulfide crystals.

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Abstract

The invention belongs to the field of inorganic fine chemicals, and relates to a method for preparing high-purity sodium sulfide crystals, comprising the following steps: (1) evaporating and concentrating the sodium sulfide solution, a by-product of barium sulfate produced by the mirabilite method, to obtain a sodium sulfide concentrate; (2) ) adding sodium hydroxide to the sodium sulfide concentrate, and stirring at 115-125°C to precipitate solids; (3) filtering, naturally cooling the filtrate to 70-75°C, and crystals are precipitated; (4) centrifugal dehydration , cooling and sieving the crystals to obtain high-purity sodium sulfide crystals. The preparation method of the high-purity sodium sulfide crystal of the present invention uses the by-product sodium sulfide solution produced by the Glauber's salt method as a raw material, and obtains the high-purity sodium sulfide crystal after simple treatment, which not only overcomes the preparation of high-purity sodium sulfide in the prior art Crystals have high requirements for raw materials, but also realize the effective recycling of by-products, meet the concept of green chemical industry, and are suitable for industrial promotion and application.

Description

technical field [0001] The invention belongs to the field of inorganic fine chemicals and relates to a preparation method of high-purity sodium sulfide crystals. Background technique [0002] Industrial sodium sulfide is widely used in papermaking, dyestuff, ore dressing and other industries, but in industries with higher quality requirements such as pharmaceutical intermediates, electrolysis, and synthesis of sulfur-containing polymers, industrial sodium sulfide is restricted due to its high impurity content. [0003] At present, the purity or cost of high-purity sodium sulfide cannot meet normal requirements due to various defects in existing methods for producing high-purity sodium sulfide. For example, the production method of CN1944241A high-purity crystalline sodium sulfide adopts acidolysis of barium sulfide solution to produce hydrogen sulfide, then absorbs and produces sodium sulfide solution with ionic membrane caustic soda, and makes through evaporation, crystalli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/36
CPCC01B17/36C01P2006/80
Inventor 郭汉光杨德林陈兴军曾开文张松
Owner GUIZHOU REDSTAR DEVING