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Process method for preparing zinc borate

A process method, the technology of zinc borate, applied in the directions of borates, chemical instruments and methods, boron compounds, etc., can solve the problems of difficult processing, poor thermal stability, irregular morphology, etc., to solve unstable quality, improve Excellent product quality and thermal stability

Inactive Publication Date: 2018-10-26
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, the following problems currently exist in the preparation process of domestic zinc borate products: (1) the process is backward, the reaction conditions are unreasonable, the product quality is low, especially the thermal stability is poor; (2) the size distribution of the product is not uniform , the shape is irregular, the follow-up processing is difficult, and the performance is lower than that of imported products

Method used

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  • Process method for preparing zinc borate
  • Process method for preparing zinc borate
  • Process method for preparing zinc borate

Examples

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Embodiment 1

[0031] Add 45g of zinc sulfate and 83.5g of water to prepare a solution with a content of 35% by mass, adjust the pH of the solution to 3, add it to the reactor, add 67g of borax (borax pentahydrate), 0.3g of zinc oxide , 0.03g 1-5μm zinc borate seed crystals are added to the reactor, according to the ratio of the solid reactant and water added above, add 2.9g of water to make the solid-liquid ratio of the system 1.3:1, and start the reaction at 97°C. After the reaction is kept for 5 hours, 112.33g of water is added to the reaction kettle, the temperature is naturally cooled to 50°C, and the reaction is finished after 3 hours of keeping for crystallization. The reaction liquid is suction filtered, washed, and dried at 80°C for 2 hours to obtain the product of the present invention.

Embodiment 2

[0033] Add 40g of zinc sulfate and 74.3g of water to prepare a solution with a content of 35%, adjust the pH of the solution to 2, add it to the reactor, add 70g of borax, 0.5g of zinc oxide, and 0.02g of 6-10μm Zinc borate seed crystals are added to the reaction kettle. According to the ratio of the solid reactants and water added above, 34.72g of water is added to make the solid-liquid ratio of the system 1.5:1. The temperature is raised to 95°C for the reaction, and the reaction is kept warm for 6 hours. 110.52g of water was added to the kettle, the temperature was naturally lowered to 50°C, and the reaction was completed after 2 hours of holding and crystallization. The reaction liquid is suction filtered, washed, and dried at 80°C for 2 hours to obtain the product of the present invention.

Embodiment 3

[0035] Add 50g of zinc sulfate and 93g of water to prepare a 35% solution, adjust the pH of the solution to 4, add it to the reactor, add 60g of borax, 0.1g of zinc oxide, and 0.05g of zinc borate seed crystals Add to the reactor, add 17.05g of water to make the solid-liquid ratio of the system 1:1 according to the ratio of the solid reactant and water added above, start the reaction at 102°C, keep the reaction for 4 hours, add 110.15g to the reactor The water is naturally cooled to 50°C, and the reaction is completed after 4 hours of holding and crystallization. The reaction liquid is suction filtered, washed, and dried at 80°C for 2 hours to obtain the product of the present invention.

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Abstract

The invention discloses a process method for preparing zinc borate. The method comprises the following steps: adding water into solid zinc sulfate to prepare a zinc sulfate solution, and regulating the pH value of the zinc sulfate solution to be 2-4; adding borax, zinc oxide, zinc borate crystal seed and water to enable the solid-liquid mass ratio to be (1-1.5):1, heating and reacting; and addingwater having the same mass to the solid, cooling, maintaining the temperature, crystallizing, and performing after-treatment, thereby obtaining the product. According to the process method disclosed by the invention, zinc borate is prepared by taking borax, zinc sulfate solution and zinc oxide as main raw materials, the product quality is greatly improved by methods for regulating the pH value ofthe reaction, controlling the solid-liquid ratio of the reaction and the like, and the product of uniform size is prepared by adding the screened crystal seed of a special particle size range to guidethe zinc borate crystal growth process. The zinc borate prepared by the method disclosed by the invention has excellent thermal stability, and 1% of dehydration temperature reaches 345 DEG C.

Description

Technical field [0001] The invention relates to a process method for preparing zinc borate. It belongs to the field of chemical synthesis technology. Background technique [0002] Zinc borate is one of the earliest inorganic flame retardants. It is a multifunctional additive with multiple functions such as flame retardant, char formation, smoke suppression, smoldering suppression and droplet prevention. It has low toxicity, low cost, High transparency and not easy to precipitate. Because zinc borate 2ZnO 3B 2 O 3 ·3.5H 2 O has a higher dehydration temperature and still retains crystal water above 250°C, so it has a higher commercial value. However, the current traditional industrial preparation process of zinc borate has a large number of defects, which limits the application and promotion of its products. For example, in the boric acid-zinc hydroxide method, the required zinc hydroxide needs to be prepared on site, and the process is complicated and inevitably produces a larg...

Claims

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Application Information

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IPC IPC(8): C01B35/12
CPCC01B35/127C01P2002/88C01P2004/03
Inventor 岳涛邢文国冯维春高维丹翟云鸽王瑞菲
Owner QINGDAO UNIV OF SCI & TECH
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