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Preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid

A technology of aminotrimethylene phosphonic acid and phosphorous acid, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as strong ammonia smell and side effects of environmental protection , to achieve the effect of expanding the application field

Inactive Publication Date: 2014-04-02
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the aminotrimethylene phosphonic acid liquid products on the market have high chloride ion content, and the smell of ammonia is very strong during alkali adjustment, which brings great harm to high-end water treatment such as seawater desalination, membrane treatment and environmental protection. had a big side effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of low chlorine and low ammonia amino trimethylene phosphonic acid is specifically realized through the following steps:

[0024] (1) Add phosphorous acid and ammonium chloride to the reaction kettle, heat to 70±5°C, add 45% formaldehyde solution dropwise, and keep reflux;

[0025] (2) After the dropwise addition is completed, keep the reaction at 105±5°C for 2 hours;

[0026] (3) Steam at 100°C under a negative pressure of -0.075MPa to a solid content of 80%;

[0027] (4) Add reverse osmosis water to a solid content of 40%, increase the temperature to 100°C, negative pressure -0.075MPa, and steam to a solid content of 80%;

[0028] (5) Repeat step (4) 3 times, if the test is qualified, add reverse osmosis water to dilute.

Embodiment 2

[0030] A preparation method of low chlorine and low ammonia amino trimethylene phosphonic acid is specifically realized through the following steps:

[0031] (1) Add phosphorous acid and ammonium chloride to the reaction kettle, heat to 70±5°C, add 40% formaldehyde solution dropwise, and keep reflux;

[0032] (2) After the dropwise addition is completed, keep the reaction at 100±5°C for 3 hours;

[0033] (3) Steam at 80°C under a negative pressure of -0.08MPa to a solid content of 80%;

[0034] (4) Add reverse osmosis water to a solid content of 40%, increase the temperature to 80°C, negative pressure -0.08MPa, and steam to a solid content of 80%;

[0035] (5) Repeat step (4) 4 times, if the test is qualified, add reverse osmosis water to dilute.

Embodiment 3

[0037] A preparation method of low chlorine and low ammonia amino trimethylene phosphonic acid is specifically realized through the following steps:

[0038] (1) Add phosphorous acid and ammonium chloride to the reaction kettle, heat to 70±5°C, add 55% formaldehyde solution dropwise, and keep reflux;

[0039] (2) After the dropwise addition, keep the reaction at 95±5°C for 3 hours;

[0040] (3) Steam at 80°C under negative pressure -0.075MPa until the solid content is 80%;

[0041] (4) Add reverse osmosis water to a solid content of 40%, increase the temperature to 80°C, negative pressure -0.075MPa, and steam to a solid content of 80%;

[0042] (5) Repeat step (4) 3 times, if the test is qualified, add reverse osmosis water to dilute.

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PUM

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Abstract

The invention provides a preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid. A synthesis method comprises the steps of adding phosphorous acid and ammonium chloride into a reaction kettle, increasing the temperature, dropwise adding formaldehyde and maintaining backflow; after dropwise adding, preserving heat in a backflow state; after the heat preservation, performing negative-pressure external steaming until the solid content is over 80%; adding reverse osmosis water, increasing the temperature and performing negative-pressure external steaming until the solid content is over 80%; repeating the steps; after the product is qualified by detection, adding water for dilution until the solid content meets the requirement. The amino trimethylene phosphonic acid prepared by the method provided by the invention has the characteristics of low chloride content and low ammonia content (the content of chlorides based on Cl<-1> is less than or equal to 0.5%, and the ammonia content is less than or equal to 100mg / L), and can be applied to a strong-base environment; with low chlorine ion content, the amino trimethylene phosphonic acid can meet some requirements for high-end water treatment application.

Description

technical field [0001] The invention belongs to the field of synthesis of water treatment chemicals and provides a method for preparing low-chlorine and low-ammonia amino trimethylene phosphonic acid. Background technique [0002] Aminotrimethylenephosphonic acid (aminotrimethylenephosphonic acid) is an organic phosphonic acid scale and corrosion inhibitor, which can form stable complexes with iron, copper, zinc and other metal ions, and can dissolve the metal surface of oxides. Amino trimethylene phosphonic acid is generally used as an anti-scaling agent for circulating cooling water, oil field water injection and printing and dyeing water, as well as a corrosion inhibitor and anti-scaling agent in boiler water equipment. In addition, it can be used in conjunction with various buffers and scale inhibitors. It has a synergistic effect with polycarboxylate, etc., which can increase the effect of corrosion and scale inhibition, and can also be used as a cleaning agen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 刘全华程终发万振涛宋盟盟齐晓婧李鹏飞张秀华
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD