A kind of preparation method of sodium maleate hypophosphite
A technology of acid-based sodium hypophosphite and sodium hypophosphite, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems such as strong acidic environment, large amount of solvents, and complicated process , to avoid environmental pollution, reduce equipment requirements, simple and feasible process
Inactive Publication Date: 2017-03-08
QINGDAO UNIV OF SCI & TECH
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Problems solved by technology
The current method for preparing carboxyl-containing hypophosphite mainly has the following defects: the use of a large amount of solvents, strong acidic environment, high pressure reaction, complex process
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[0030] The present invention will be described in further detail below in conjunction with examples, but the embodiments of the present invention are not limited thereto.
[0031] In some embodiments, the invention provides a kind of preparation method of sodium maleate hypophosphite, comprising the following steps:
[0032] S1. In a reaction kettle with a stirring and reflux device, add sodium hypophosphite and maleic acid in turn at room temperature, raise the temperature to 70-100°C, and keep stirring for 3-5 hours for a reaction time;
[0033] S2. Cool down to 40°C, add 20-40ml of ethanol and water mixture, and stir for 30 minutes;
[0034] S3, cool down to room temperature, then filter and dry to obtain sodium maleate hypophosphite;
[0035] The molar ratio of the sodium hypophosphite to the maleic acid in the step S1 is 1:1-2;
[0036] In the step S2, the volume ratio of the water to the ethanol is 1:4-7.
[0037] In this embodiment, the fusion reaction of maleic acid...
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The invention discloses a maleic acid sodium hypophosphite preparation method, including the following steps: S1, successively adding sodium hypophosphite and maleic acid into a reactor with stirring and refluxing devices at room temperature, heating to 70-100 DEG C, reacting for 3-5 hours, and continuously stirring; S2, cooling to 40 DEG C, adding 20-40ml of an ethanol and water mixture, and stirring for 30 minutes; S3, cooling to room temperature, then filtering, drying to obtain maleic acid sodium hypophosphite. The process of heating melting reaction of sodium phosphate and maleic acid is performed without need of solvent and acidic conditions and addition of an initiator, sodium hypophosphite double bond addition reaction synthesis is greatly simplified, in the treatment process, no complex high pressure equipment is needed, no highly toxic gas is produced, and no complex post treatment process is arranged, so that the production cost is greatly reduced, the pollution to the environment can be avoided, at the same time, the synthesis process is simple and easy to operate.
Description
technical field [0001] The invention belongs to the technical field of preparation of hypophosphite flame-retardant materials, and in particular relates to a preparation method of sodium maleate hypophosphite. Background technique [0002] According to the relationship between the flame retardant and the flame retardant substrate, the flame retardant can be divided into two categories: additive type and reactive type. Additive flame retardant flame retardant high polymer processing technology is simple, and there are many types of flame retardants that can meet the requirements of use, but a series of problems such as dispersion, compatibility, and interface of flame retardants need to be solved; reactive type flame retardants The flame retardancy obtained by the flame retardant is relatively permanent, has low toxicity, and has little influence on the physical properties of the flame retardant polymer. Reactive halogen-free flame retardants are generally organophosphorus m...
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IPC IPC(8): C07F9/30
Inventor 赵文鹏许军武玉民高传慧王传兴王宁宁
Owner QINGDAO UNIV OF SCI & TECH