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Method of using glufocinate byproduct waste residue to prepare aluminum hypophosphite

A technology of aluminum hypophosphite and glufosinate-ammonium, which is applied in the direction of hypophosphorous acid and phosphorus oxyacids, can solve the problems of deterioration of material mechanical properties, affecting the particle size of aluminum hypophosphite, affecting the purity of products, etc., and achieves good reaction and good affinity. The effect of oil performance and fast reaction rate

Inactive Publication Date: 2017-07-28
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the process of preparing aluminum hypophosphite, if the control of process parameters is not rigorous enough, side reactions will easily occur, affecting the purity of the product and producing the highly toxic substance hypophosphite
[0005] In addition, in the process of preparing aluminum hypophosphite, the dispersion form and dropping speed of aluminum chloride will also greatly affect the particle size of aluminum hypophosphite; Poor performance, when used in rubber and plastic flame retardant, aluminum hypophosphite needs to be crushed into ultra-fine powder by mechanical crushing, and dust is easy to be generated in the process, which poses a threat to safe production
On the other hand, aluminum hypophosphite is an inorganic salt with a charge on the surface, hydrophilic and oleophobic, and it is difficult to disperse evenly in the material when blended with polymer materials, resulting in rapid deterioration of the mechanical properties of the material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Slowly add 7g of industrial by-products (including 4.6g of aluminum chloride) into 100ml of water, stir for 30min, and filter; remove the filter residue, and use the filtrate for later use.

[0021] Add 7.7 g of sodium hypophosphite and 110 mL of water into a 500 mL four-neck flask equipped with a serpentine reflux condenser, an electric stirrer and a thermometer, stir to dissolve, and add hydrochloric acid dropwise to adjust the pH to 3.

[0022] Heat the sodium hypophosphite solution to 50°C, add 50 mL of filtrate containing 2.3 g of aluminum chloride dropwise under high-speed stirring at 2000 r / min, and react under low-speed stirring at 50 r / min for 2 h to obtain a white precipitate. The time of dropping of whole filtrate is controlled in 10 minutes and finishes, and the rate of addition of first 5 minutes is 8ml / minute, and the rate of addition of last 5 minutes is 2ml / minute.

[0023] After the white precipitate is filtered, washed and dried in sequence, a powdery ...

Embodiment 2

[0025] The only difference between this example and Example 1 is that after slowly adding 7g of industrial by-products (containing 4.6g of aluminum chloride) into 100ml of water, 0.14g of dispersant microcrystalline cellulose powder needs to be added. As a result, the subsequent process is slightly different, and the product performance has also been improved, as follows:

[0026] Slowly add 7g of industrial by-products (including 4.6g of aluminum chloride) into 100ml of water, then add 0.14g of microcrystalline cellulose powder as a dispersant, stir for 30 minutes, and filter; remove the filter residue, and use the filtrate for later use.

[0027] Add 7.7 g of sodium hypophosphite and 110 mL of water into a 500 mL four-neck flask equipped with a serpentine reflux condenser, an electric stirrer and a thermometer, stir to dissolve, and add hydrochloric acid dropwise to adjust the pH to 3.

[0028] Heat the sodium hypophosphite solution to 50°C, add dropwise 50 mL of filtrate co...

Embodiment 3

[0031] Slowly add 10g of industrial by-products (including 6.5g of aluminum chloride) into 100ml of water, stir for 30min, then filter; remove the filter residue, and use the filtrate for later use.

[0032] Add 12 g of sodium hypophosphite and 110 mL of water into a 500 mL four-necked flask equipped with a serpentine reflux condenser, an electric stirrer and a thermometer, stir to dissolve, and add hydrochloric acid dropwise to adjust the pH to 4.5.

[0033] Heat the sodium hypophosphite solution to 40°C, add dropwise 50 mL of filtrate containing 3.25 g of aluminum chloride under high-speed stirring at 1600 r / min, and react under low-speed stirring at 75 r / min for 1 h to obtain a white precipitate. The dropping time of the whole filtrate was controlled to be completed in 12 minutes, and the rate of addition in the first 6 minutes was 6.8ml / min, and the rate of addition in the latter 6 minutes was 1.5ml / min.

[0034] After the white precipitate is filtered, washed and dried in...

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Abstract

The invention discloses a method of using glufocinate byproduct waste residue to prepare aluminum hypophosphite. The method includes following steps: (1), slowly adding a glufocinate industrial byproduct into water, sufficiently stirring, filtering to remove filter residue, and taking filtrate for standby use; dissolving sodium hypophosphite in water to prepare a sodium hypophosphite solution, and adding hydrochloric acid to adjust pH value of the sodium hypophosphite solution to 3-6; (2), taking the filtrate and the sodium hypophosphite solution according to a reactant molar feeding ratio of sodium hypophosphite to aluminum chloride being (4-5):1; (3), putting the sodium hypophosphite solution in a container provided with a snake-shaped condensing pipe, heating to 30-50 DEG C, and dropwise adding the filtrate while stirring at a high speed; after dripping of the filtrate is finished, finishing reaction while slowly stirring; (4), subjecting a reaction product obtained in the step (3) sequentially to separating, washing and drying to obtain powdery white solid which is a product containing aluminum hypophosphite. Therefore, by optimizing the process of using the glufocinate byproduct waste residue to prepare aluminum hypophosphite, a reaction system has the advantages of mild reaction and high reaction rate.

Description

technical field [0001] The invention relates to a method for preparing aluminum hypophosphite, in particular to a method for preparing aluminum hypophosphite from glufosinate-ammonium by-product waste residue. Background technique [0002] Glufosinate-ammonium is a non-selective, non-residue herbicide that kills perennial root weeds and is widely used in rubber, mulberry, tea, orchards and sugarcane fields. In the production process of glufosinate-ammonium, the industrial by-products (mainly composed of aluminum trichloride and sodium chloride) are characterized by large amount (about 10,000 tons per year), strong corrosion and difficult to landfill. Therefore, How to utilize this industrial by-product and achieve the treatment of the three wastes up to the standard is a problem urgently faced by glufosinate-ammonium manufacturers. [0003] At present, some glufosinate-ammonium production enterprises, by analyzing the composition of the industrial by-products of glufosinate...

Claims

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Application Information

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IPC IPC(8): C01B25/165C08K3/32
CPCC01B25/165C01P2004/61C01P2006/80C08K3/32C08K2201/003
Inventor 李舟何路涛
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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