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A cationic curing agent and production process technology, applied in the direction of inorganic chemistry, antimony compounds, chemical instruments and methods, etc., can solve the problems of complex impurity removal process, high cost of raw materials, low purity, etc.
Inactive Publication Date: 2021-07-06
NANTONG SYNASIA NEW MATERIAL CO LTD
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Problems solved by technology
[0007] The technical problem to be solved by the present invention is to provide a cationic curing agent production process, which can solve the problems of high raw material cost, complicated impurity removal process in the early stage, many recrystallization times and low purity of general cationic curing agent
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Embodiment 1
[0028] Such as figure 1 Shown a kind of cationic curing agent production process, concrete production process is as follows:
[0029] S1: Preparation of sodium pyroantimonate: Add sodium hydroxide and water to the reaction kettle, then add antimony trioxide, and react at a constant temperature of 80-120°C for 2 hours; cool down to 30-50°C, and inject ozone while stirring to carry out Oxidation reaction for 5 hours; then heat up to 100°C, stand for crystallization, centrifuge, and dry to obtain sodium pyroantimonate;
[0030] S2: Preparation of hexafluoroantimonic acid: at 60-120°C, mix antimony trioxide with acetic acid solution containing hydrogen fluoride, then add hydrogen peroxide dropwise at a rate of 5mL / min while stirring, and obtain hexafluoroantimony after the reaction is complete acid solution;
[0031] S3: Preparation of silver hexafluoroantimonate mother liquor: under the condition of 60-120°C, equimolar amounts of sodium pyroantimonate solid and silver carbonate...
Embodiment 2
[0038] Such as figure 1 Shown a kind of cationic curing agent production process, concrete production process is as follows:
[0039] S1: Preparation of sodium pyroantimonate: Add sodium hydroxide and water to the reaction kettle, then add antimony trioxide, and react at a constant temperature of 80-120°C for 3 hours; cool down to 50°C, and introduce ozone while stirring to carry out oxidation reaction 6 hours; then heat up to 100°C, stand for crystallization, centrifuge, and dry to obtain sodium pyroantimonate;
[0040] S2: Preparation of hexafluoroantimonic acid: at 60-120°C, mix antimony trioxide with acetic acid solution containing hydrogen fluoride, then add hydrogen peroxide dropwise at a rate of 15mL / min while stirring, and obtain hexafluoroantimony after the reaction is complete acid solution;
[0041] S3: Preparation of silver hexafluoroantimonate mother liquor: under the condition of 60-120°C, equimolar amounts of sodium pyroantimonate solid and silver carbonate so...
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Abstract
The invention relates to a production process of a cationic curing agent. The production process is characterized by specifically comprising the following steps: S1, preparing sodium pyroantimonate; S2, preparing hexafluoroantimonic acid; S3, preparing a silver hexafluoroantimonate mother solution; S4, concentrating, cooling and crystallizing the silver hexafluoroantimonate mother solution; and S5, recrystallizing and purifying coarse silver hexafluoroantimonate crystals. According to the present invention, the mixing of the antimony trioxide and a hydrogen fluoride-containing acetic acid solution has advantages of mild reaction condition, simple and easily available raw materials, low equipment requirement, high generation rate of hexafluoroantimonic acid, less impurity content, and high yield of the silver hexafluoroantimonate product compared with the mixing of antimony trioxide and a hydrofluoric acid aqueous solution or anhydrous hydrofluoric acid. Hexafluoroantimonic acid reacts with silver carbonate to generate a silver hexafluoroantimonate mother solution; and then silver hexafluoroantimonate is prepared from sodium pyroantimonate and silver carbonate in a hydrogen fluoride aqueous solution in one step. The method is mild in reaction condition, low in raw material price, small in environmental pollution and high in impurity removal rate, and the purity of the finally obtained product is high and reaches 99% or above.
Description
technical field [0001] The invention relates to the technical field of epoxy resin reaction catalysts, in particular to a production process of a cationic curing agent. Background technique [0002] Epoxy resin is a kind of thermosetting polymer material with good adhesion, electrical insulation and chemical stability. It is widely used in construction, machinery, electronics, aerospace, etc. and other fields. When epoxy resin is used, curing agent must be added, and the curing reaction is carried out under certain conditions to form a three-dimensional network structure product, which will show various excellent properties and become an epoxy material with real use value. Therefore, the curing agent is indispensable in the application of epoxy resin, and even plays a decisive role to some extent; the common cationic photoinitiator is UV6992 (diphenyl-(4-phenylsulfur) phenylsulfonium Hexafluorophosphate), UV6976 (diphenyl-(4-phenylthio)phenylsulfonium hexafluoroantimonate)...
Claims
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