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Method for preparing phosphate esters light textile adjuvant

A technology of phosphate esters and auxiliaries, which is applied in the field of preparation of phosphate ester textile auxiliaries, can solve the problems of dehydration and carbonization of reaction materials, pollute the environment, and easy agglomeration, and achieve the effect of improving the reaction conversion rate

Inactive Publication Date: 2004-11-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Use P 2 o 5 For phosphorylation, P 2 o 5 The feeding method is still in powder form. Due to its strong moisture absorption and easy agglomeration, it will also dehydrate and carbonize the reaction material, which will affect the progress of the reaction.
Although some people have used organic solvents such as CCl 4 , benzene, etc. will P 2 o 5 Dissolved, but actually not dissolved but added after dispersion, but due to the low boiling point of this type of solvent, it is easy to volatilize during the reaction and pollute the environment, and it must be removed after the reaction, which increases the operating procedures

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] Embodiment 1: first the P of 2 parts by mass parts 2 o 5 Add to 15 parts of C10-25 liquid paraffin, stir evenly and use it as a phosphorylating agent for later use; add 30 parts by mass of castor oil to a three-necked flask equipped with a thermometer, temperature control device and stirrer, and heat up to 60°C Add 10 parts by mass of the dispersed phosphorylating agent, raise the temperature to 95°C and keep it warm for continuous reaction for 2 hours, add 0.3 parts by mass of water, and hydrolyze for 1 hour to prepare acidic phosphoric acid ester; lower the temperature to below 50°C , adding 8 parts of sodium hydroxide with a mass percentage concentration of 40% for neutralization, raising the temperature to 55° C., continuing to stir for 30 minutes, and adding water to control the solid mass percentage to 45%.

Embodiment 2

[0008] Embodiment 2: first the P of 6 parts by mass parts 2 o 5 Add to 10 parts of chlorinated paraffin, stir evenly and use it as a phosphorylating agent for later use; add 100 parts by mass of dehydrated wool with a water content lower than 1% to a three-necked flask equipped with a thermometer, a temperature control device and a stirrer. Grease, heat up to 30°C, add 21 parts by mass of phosphorylating agent that has been dispersed, heat up to 60°C, keep warm for 4 hours, add 1.0 parts by mass of water, hydrolyze for 3 hours, and prepare acidic phosphoric acid ester Cool down to below 50°C, add 2 parts of sodium hydroxide with a mass percentage concentration of 10% for neutralization, heat up to 70°C, continue stirring for 120 minutes, add water to control the mass percentage of solids to 85%.

Embodiment 3

[0009] Embodiment 3: first the P of 4 parts by mass parts 2 o 5 Add it to 8 parts of alkylsulfonyl chloride, stir well and use it as a phosphorylating agent for later use; add 60 parts by mass of castor oil to a three-necked flask equipped with a thermometer, a temperature control device, and a stirrer, and heat up to 54°C to add mass 15 parts of the dispersed phosphorylating agent are heated up to 75°C and kept for continuous reaction for 3 hours, then 1.2 parts by mass of water is added and hydrolyzed for 2 hours to obtain an acidic phosphoric acid ester; the temperature is lowered to below 50°C and added Neutralize with 5 parts of sodium hydroxide with a concentration of 20% by mass, raise the temperature to 60° C., continue stirring for 100 minutes, and add water to control the mass percentage of solids to 60%.

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PUM

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Abstract

The invention is a manufacturing method for phosphate textile assistants. At first, the P2O5 is added into high molecular aliphatic hydrocarbon and its derivant solvent of mineral oil long carbon chains or plant oil dispersing solvent, they are blended evenly to be used as phosphorylation agent; castor oil or dewatered wool grease are heated to 30-60 degrees and adds in phosphorylation agent, adds in water to hydrolyze them after the heating reaction to produce acid phosphate ester; decreases the temperature to below 50 degrees, then adds in natrium oxyhydrogen to neutralize, heats up and stirs, adds in water to control the solid content between 45%-85%.

Description

technical field [0001] The invention relates to a preparation method of a light spinning auxiliary agent, in particular to a preparation method of a phosphate ester light spinning auxiliary agent. Background technique [0002] There is little research on the synthesis and research of phosphoric esters, especially the selection of phosphorylation reagents in the synthesis of phosphoric acid esters and the greening of phosphorylation methods. Commonly used phosphorylating agents are pyrophosphate, P 2 o 5 , POCl 3 , PCl 3 etc., due to POCl 3 , PCl 3 HCl is produced in the reaction, polluting the environment, and the phosphorylation of pyrophosphoric acid should be carried out under xylene azeotropic dehydration. Widely used in industry P 2 o 5 Phosphorylation is carried out. Use P 2 o 5 For phosphorylation, P 2 o 5 The feeding method is still in powder form. Due to its strong moisture absorption and easy agglomeration, it will also dehydrate and carbonize the reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/282
Inventor 王学川冯见艳孙明
Owner SHAANXI UNIV OF SCI & TECH
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