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A kind of preparation method and application of styryl phosphonic acid monoester

A technology of styryl phosphonic acid monoester and styrene, which is applied in the field of preparation of styryl phosphonic acid monoester, can solve the problem that the by-product thionyl chloride is difficult to handle, there is no mineral flotation collector, and equipment requirements are relatively low. Advanced problems, to achieve the effects of suppressing side reactions, good foaming performance, and good selectivity

Active Publication Date: 2019-07-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can effectively control the progress of the next step of the substitution reaction by first synthesizing the intermediate styrylphosphonic dichloride, but the synthesis cost of this method is still high, and the distillation of the acid chloride has higher requirements for equipment, and the by-product Disadvantages such as difficulty in handling thionyl chloride
Zheng Longao et al. applied the mixture (B312) of styrene phosphonic acid monoester (B312) to the extraction and separation of copper, cobalt and nickel, and achieved good results ( Zheng Longao, Wang Manzhen, Yu Qinghua, et al. New extractant styrene phosphonic acid monoester I. Extraction and separation of copper, cobalt and nickel with B312 [J]. Mining and Metallurgy Engineering, 1983, 3 (4): 44-48.), but There is no report on its use as a mineral flotation collector

Method used

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  • A kind of preparation method and application of styryl phosphonic acid monoester
  • A kind of preparation method and application of styryl phosphonic acid monoester
  • A kind of preparation method and application of styryl phosphonic acid monoester

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Take 20.8g of phosphorus pentachloride with a purity of 98% and add it to 80ml of chloroform with a purity of 99.8%, stir it in a water bath at 50°C to dissolve it; take 10.4g of styrene with a purity of 99%, dissolve it in 20ml of trichloromethane In methane, add dropwise to the above-mentioned phosphorus pentachloride solution, and fully stir for 4 hours under the condition of 50°C water bath; take 3.84g of methanol with a purity of 99.8% and dropwise into the above-mentioned reaction solution, and fully stir for 1h under the condition of 50°C water bath; 50ml of distilled water was added dropwise to the above reaction solution, and fully stirred for 1 hour under the condition of 50°C water bath. After the reaction is over, separate the liquid in the separatory funnel, remove the upper aqueous phase, add 20ml of NaOH solution with a concentration of 40% to the organic phase, shake fully, leave to stand for stratification, take the upper saponified phase, add 40ml of 5m...

Embodiment 2

[0049] Take 20.8g of phosphorus pentachloride with a purity of 98% and add it to 80ml of chloroform with a purity of 99.8%, stir it in a water bath at 50°C to dissolve it; take 10.4g of styrene with a purity of 99%, dissolve it in 20ml of trichloromethane In methane, add dropwise to the above-mentioned phosphorus pentachloride solution, and fully stir for 4 hours under the condition of 50°C water bath; take 5.52g of ethanol with a purity of 99.8% and dropwise into the above-mentioned reaction solution, and fully stir for 1h under the condition of 50°C water bath; 50ml of distilled water was added dropwise to the above reaction solution, and fully stirred for 1 hour under the condition of 50°C water bath. After the reaction is over, separate the liquid in the separatory funnel, remove the upper aqueous phase, add 20ml of NaOH solution with a concentration of 40% to the organic phase, shake fully, leave to stand for stratification, take the upper saponified phase, add 40ml of 5mo...

Embodiment 3

[0051] Take 20.8g of phosphorus pentachloride with a purity of 98% and add it to 80ml of chloroform with a purity of 99.8%, stir it in a water bath at 50°C to dissolve it; take 10.4g of styrene with a purity of 99%, dissolve it in 20ml of trichloromethane In methane, add dropwise to the above phosphorus pentachloride solution, fully stir for 4h under the condition of 50°C water bath; take 8.88g of n-butanol with a purity of 99.8% and dropwise into the above reaction solution, fully stir for 1h under the condition of 50°C water bath ; Take 50ml of distilled water and add dropwise to the above reaction solution, and fully stir for 1 hour under the condition of 50°C water bath. After the reaction is over, separate the liquid in the separatory funnel, remove the upper aqueous phase, add 20ml of NaOH solution with a concentration of 40% to the organic phase, shake fully, leave to stand for stratification, take the upper saponified phase, add 40ml of 5mol / L was acidified with hydro...

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Abstract

The invention provides a preparation method for styryl phosphonic acid monoester and application. The method is capable of, after adding phosphorus pentachloride to a solvent for dissolving, dropwiseadding styrene and alcohol ROH, stirring, and uniformly mixing to obtain a compound as shown in formula (II), wherein R is selected from an alkyl of C1-C12 or an aralkyl of C6-C12; and dropwise addingdistilled water, post-processing to obtain the styryl phosphonic acid monoester as shown in formula (III). The styryl phosphonic acid monoester is used as a floatation collecting agent which is applied for flotation-selecting oxidized ore, and can be used for effectively realizing the flotation of target minerals. The preparation method is simple, and environmentally friendly, and capable of preventing sulfur dioxide from being used, and avoiding the generation of thionyl chloride. The styryl phosphonic acid monoester is used for the flotation of the oxidized ore, and good in flotation performance.

Description

technical field [0001] The invention relates to the technical field of mineral processing, in particular to a preparation method and application of styryl phosphonic acid monoester. Background technique [0002] Mineral flotation technology is an important separation technology in the field of mining and metallurgy engineering, and flotation collector is one of the key technologies for the separation and extraction of minerals by flotation. Among them, phosphorus-containing compounds are an important class of collectors, which play an important role in improving the comprehensive recovery of metals. [0003] In the field of mineral flotation, phosphorus-containing compounds are mainly used in oxidized ore flotation, mainly including phosphate, phosphite, phosphonic acid, bisphosphonic acid and thiophosphonic acid. Chinese patent CN103923119A discloses a preparation method of alkyl phosphite, which can be used as a collector for flotation of oxide ore. Styrylphosphonic acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40B03D1/014B03D101/02B03D103/04
CPCB03D1/014B03D2201/02B03D2203/04C07F9/4056C07F9/4075
Inventor 钟宏黄凯华王帅
Owner CENT SOUTH UNIV
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