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Method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthesis liquid

A technology of fluorescent whitening agent and diethyl phosphate, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of large-scale processing and recovery of diethyl phosphate in enterprises Diethyl phosphate sodium salt, restricting the sustainable, healthy and stable development of fluorescent whitening agent enterprises, and the low recovery rate and purity of diethyl phosphate sodium salt, so as to increase the economic benefits of the enterprise, solve the recycling difficulties, and achieve the effect of simple recycling

Pending Publication Date: 2022-03-15
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most domestic enterprises adopt the above-mentioned process, and the process adjustment is basically to replace the solvent and catalyst. However, the recycling of diethyl phosphate sodium salt, a by-product in the CBW production process, has become an important problem for enterprises to manage waste residue and improve economic benefits.
[0003] At present, there are no relevant reports on the treatment and recovery of diethyl phosphate sodium salt in the CBW synthetic liquid
However, the traditional treatment method only adopts distillation method and solid-liquid separation, and there are problems such as high material viscosity, relatively similar physical properties of each component in the system, and low recovery and purity of diethyl phosphate sodium salt, which restricts diethyl phosphate The further development and utilization of sodium salt has affected the large-scale processing and recovery of diethyl phosphate sodium salt in enterprises
[0004] In addition, if the diethyl phosphate sodium salt in the CBW synthetic liquid is not effectively recycled, a large amount of organophosphorus resources will be wasted, and at the same time, it will be discharged into the wastewater, resulting in high COD wastewater, which will increase the difficulty of wastewater treatment. It is conducive to the environmental protection and green production of enterprises, and seriously restricts the sustainable, healthy and stable development of fluorescent whitening agent enterprises

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  • Method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthesis liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthetic liquid, comprising the following steps:

[0036] S1. Add 1000g of fluorescent whitening agent CBW synthetic solution into a 2L three-necked flask, which contains 180g of whitening agent CBW, 112.7g of diethyl phosphate sodium salt, 673g of organic solvents such as methanol, 34.3g of sodium chloride and other substances. Under a vacuum of 0.095MPa, distill under reduced pressure to a residual volume of 347g, and the residual solvent content is <5%.

[0037] S2. Add 680 g of deionized water at about 60°C to 347 g of the concentrate while it is hot, stir to dissolve completely, transfer it to a beaker, cool down, and filter under reduced pressure to obtain 250 g of filter cake and 777 g of filtrate. The filter cake is refined, washed and dried to obtain CBW semi-finished products.

[0038] S3. Distill 777g of the crude filtrate to a residual mass of 260g in the ...

Embodiment 2

[0042] A method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthetic liquid, comprising the following steps:

[0043] S1. Add 1500g of fluorescent whitening agent CBW synthetic solution into a 2L three-necked flask, which contains 270g of whitening agent CBW, 169.05g of diethyl phosphate sodium salt, 1009.5g of organic solvents such as methanol, 51.45g of sodium chloride and other substances. Under a vacuum of 0.096MPa, distill under reduced pressure to a residue of 520.5g, and the residue of solvent is <5%.

[0044] S2. Add 1040 g of deionized water at about 70°C to 520.5 g of the concentrate while it is hot, stir to dissolve completely, transfer it to a beaker, cool down, and filter under reduced pressure to obtain 380 g of filter cake and 1180.5 g of filtrate. The filter cake is refined, washed and dried to obtain CBW semi-finished products.

[0045] S3. Distill 1180.5 g of the crude filtrate to a residual mass of 260 g, and ...

Embodiment 3

[0049] A method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthetic liquid, comprising the following steps:

[0050] S1. Add 1500kg of fluorescent whitening agent CBW synthetic solution to the 3000L reaction kettle, which contains 270kg of whitening agent CBW, 169.05kg of diethyl phosphate sodium salt, 1009.5kg of organic solvents such as methanol, 51.45kg of sodium chloride and other substances. Under a vacuum of 0.096MPa, distill under reduced pressure to a residual mass of 510kg, and the residual solvent content is <5%.

[0051] S2. Add 1000kg of deionized water at about 78°C to the 510kg concentrate while it is hot, stir to dissolve completely, transfer to a cooling kettle, cool down and crystallize, and filter through plate and frame to obtain 350kg of filter cake and 1160kg of filtrate. The filter cake is refined, washed and dried to obtain CBW semi-finished products.

[0052] S3. Distill 1160kg of the crude product fil...

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Abstract

The invention provides a method for separating and recovering diethyl phosphate sodium salt from a fluorescent whitening agent synthetic liquid, which comprises the following steps: S1, distilling the fluorescent whitening agent synthetic liquid, and recovering a solvent to obtain a concentrate A1; s2, adding hot water into the concentrate A1, uniformly dissolving, cooling to room temperature, and filtering to obtain a solid phase B1 and a liquid phase C1; s3, distilling the liquid phase C1 to obtain a concentrate A2, and filtering to obtain a solid phase B2 and a liquid phase C2; s4, continuously distilling the liquid phase C2 to obtain a concentrate A3, adding an alcohol solvent in batches under stirring reflux, uniformly dissolving, cooling to room temperature, and filtering to obtain a solid phase B3 and a liquid phase C3; and S5, distilling the liquid phase C3 to obtain a concentrate A4, cooling, and crushing to obtain the diethyl phosphate sodium salt. The method improves the quality and yield of the diethyl phosphate sodium salt, and solves the problems of difficult recovery, high energy consumption, low yield, poor quality and the like of the diethyl phosphate sodium salt at present.

Description

technical field [0001] The invention relates to the technical field of recovery of by-products of fluorescent whitening agent production, in particular to a method for separating and recovering diethyl phosphate sodium salt from fluorescent whitening agent synthetic liquid. Background technique [0002] Fluorescent whitening agent 4,4′-bis-(2-sulfonate styryl) biphenyl, referred to as CBW, was originally developed by Swiss Ciba-Geigy (now Ciba Fine Chemicals) in the late 1960s Successfully, its process is formed by benzylation of biphenyl, esterification with phosphite, and condensation with sodium o-sulfonate benzaldehyde. For every molecule of CBW produced, two molecules of diethyl phosphate sodium salt are simultaneously produced. At present, most domestic enterprises adopt the above-mentioned process, and the process adjustment is basically to replace the solvent and catalyst. However, the recycling of diethyl phosphate sodium salt, a by-product in the CBW production pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11C07C303/44C07C309/32
CPCC07F9/11C07C303/44C07C309/32
Inventor 郑阿龙沈寒晰成西涛张金峰郭鹏涛南蓉孟璐
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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