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Method for joint production of hypophosphite of calcium, magnesium and aluminum

A joint production and hypophosphite technology, which is applied in the direction of hypophosphorous acid and phosphorus oxyacid, can solve the problems of human environment and water pollution, low utilization rate of raw materials, low comprehensive yield, etc., and achieve low cost and large scale The effect of high production and overall yield

Inactive Publication Date: 2016-10-12
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, calcium, magnesium, and aluminum hypophosphites are all prepared separately at present, and there is no report that adopts the joint production method to prepare
Separate preparation has the disadvantages of low yield and low utilization rate of raw materials
[0005] Shortcomings of the prior art: the preparation of the hypophosphite of calcium and magnesium mostly adopts the oxide or hydroxide of calcium and magnesium and hypophosphorous acid through acid-base neutralization Reaction preparation
This method uses hypophosphorous acid as a reactant, and there are disadvantages that inhaling hypophosphorous acid vapor or mist will cause greater harm to the human body and greater pollution to the environment and water bodies.
At present, calcium, magnesium, and aluminum hypophosphites are prepared separately, which has the disadvantages of low utilization rate of raw materials and low comprehensive yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 2000mL water and 1100g calcium chloride hexahydrate into the there-necked flask, stir and dissolve; weigh 1060g sodium hypophosphite monohydrate, dissolve it in 800mL water, add the sodium hypophosphite solution to the calcium chloride solution for 25 o After stirring and reacting at C for 2 hours, a white precipitate was obtained, and sodium chloride was dissolved at 20-30 o The solubility at C is 35.9-36.1g / 100g water, and the total amount of solvent water can fully dissolve the generated sodium chloride, so the white precipitate obtained is calcium hypophosphite. Filter, wash with cold water, sieve, and dry to obtain 679g of white powder calcium hypophosphite product, with a yield of 79.9%, a purity of 98.4%, and an average particle size (d 50 ) 14.58 μm. About 20% of the hypophosphite ions remain unreacted in the filtrate, which is collected as a reactant for the preparation of aluminum hypophosphite. Add 3000g sodium hypophosphite monohydrate to the filtrate ...

Embodiment 2

[0035] Add 1500mL water and 1800g calcium nitrate tetrahydrate into the there-necked bottle, stir and dissolve; weigh 1500g sodium hypophosphite monohydrate, dissolve it in 1200mL water, add the sodium hypophosphite solution to the calcium nitrate solution for 30 o After stirring and reacting for 2 hours at C, a white precipitate was obtained, and sodium nitrate was dissolved at 30 o The solubility under C is 91.2g / 100g water, and the total amount of solvent water can fully dissolve the generated sodium nitrate, so the white precipitate obtained is calcium hypophosphite. Filter, wash with cold water, sieve, and dry to obtain 956 g of white powder calcium hypophosphite product, with a yield of 79.5%, a purity of 98.2%, and an average particle size (d 50 ) 15.02 μm. Also remaining about 20% of the hypophosphite ion does not react in the filtrate, which is collected as a reactant for the preparation of aluminum hypophosphite. Add 3000 g sodium hypophosphite monohydrate to the f...

Embodiment 3

[0037] Add 2000mL of water and 500g of anhydrous magnesium sulfate into the there-necked flask, stir and dissolve; weigh 800g of sodium hypophosphite monohydrate, dissolve it in 800mL of water, add the sodium hypophosphite solution into the magnesium sulfate solution for 27 o After stirring and reacting for 2 hours at C, a white precipitate was obtained, and sodium sulfate was oThe solubility under C) is 19.5-40.8 g / 100g water, and the total amount of solvent water can fully dissolve the generated sodium sulfate, so the white precipitate obtained is magnesium hypophosphite hexahydrate. Filter, wash with cold water, sieve, and dry to obtain 794g of a white powder magnesium hypophosphite hexahydrate product, with a yield of 80.3%, a purity of 98.3%, and an average particle size (d 50 ) 19.07 μm. About 20% of the hypophosphite ions remain unreacted in the filtrate, which is collected as a reactant for the preparation of aluminum hypophosphite. Add 3000g sodium hypophosphite mon...

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Abstract

The invention relates to a method for joint production of hypophosphite of calcium, magnesium and aluminum. The method provided by the invention employs sodium hypophosphite, a calcium salt, and a magnesium salt to carry out double decomposition reaction to prepare calcium hypophosphite and magnesium hypophosphite, and avoids the harm of using hypophosphorous acid as the reactant, also gives consideration to the technological shortcoming that after preparation of calcium hypophosphite and magnesium hypophosphite, a lot of hypophosphite still exists in waste liquid and cannot be completely extracted, after preparation of calcium hypophosphite and magnesium hypophosphite, a joint production technique is employed for the first time to prepare hypophosphite of aluminum. The preparation method has the advantages of mild reaction conditions, little pollution, pure product, high utilization rate of hypophosphite ions, high comprehensive yield, greatly reduced cost, and simple and practicable process route, and is convenient for mass production.

Description

technical field [0001] The invention relates to a method for joint production and preparation of calcium, magnesium and aluminum hypophosphite, which belongs to the field of manufacturing and processing polymer material flame retardants. Background technique [0002] Phosphorus-containing flame retardant is a kind of flame retardant with high flame retardant efficiency. Compared with halogen-based flame retardants, phosphorus-based flame retardants have lower smoke generation, toxicity and corrosion. Phosphorous flame retardants can be used alone or in combination with other types of flame retardants. In general, the higher the phosphorus content, the better the flame retardant effect. Regarding the synthesis of calcium hypophosphite and magnesium hypophosphite, the oxides or hydroxides of calcium and magnesium and hypophosphorous acid are prepared by acid-base neutralization reaction. With hypophosphorous acid as the reactant, inhalation of hypophosphorous acid vapor or ...

Claims

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Application Information

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IPC IPC(8): C01B25/165
Inventor 任晓婷何金选叶丹阳
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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