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Low-trimethylene-content amino trimethylene phosphonic acid and preparation method thereof

A technology of trimethylidene amino trimethylene phosphonic acid and amino trimethylene phosphonic acid, applied in the field of chemicals, can solve problems such as turbid precipitation, achieve good compatibility, solve the problem of extra cost and harm to the environment, expand The effect of using the range

Inactive Publication Date: 2013-09-04
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] In order to solve the problem of turbid precipitation in the existing commercially available aminotrimethylene phosphonic acid compounded with zinc corrosion inhibitors, and to give full play to the excellent synergy of its compounded products, the present invention provides a low-trimethylene Amino trimethylene phosphonic acid and its preparation method, the compound product obtained by the preparation method is stable, has good synergistic effect, and meets the needs of a wider range of compound regulation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A specific preparation and implementation process of low trimethylene amino trimethylene phosphonic acid is:

[0030] (1) Add 500kg of ammonium chloride and 480kg of ATMP mother liquor to the reaction kettle, add 500kg of formaldehyde water at the same time, and raise the temperature to 90°C.

[0031] (2) Add 1580kg of phosphorous acid and 1640kg of formaldehyde dropwise at the same time, control the temperature to maintain reflux, and delay the addition of formaldehyde by 15 minutes compared to phosphorous acid.

[0032] (3) After the dropwise addition of formaldehyde, control the temperature at 110±2°C and reflux for 2 hours.

[0033] (4) Detect the content of phosphorous acid, add 100kg of formaldehyde, and continue to keep warm and reflux for 1h.

[0034] (5) Negative pressure steaming to remove ammonium chloride, formaldehyde and hydrochloric acid.

[0035] (6) When it reaches normal temperature, add 3200kg of reverse osmosis water to adjust the content of active...

Embodiment 2

[0037] A specific preparation and implementation process of low trimethylene amino trimethylene phosphonic acid is:

[0038] (1) Add 500kg of ammonium chloride and 450kg of ATMP mother liquor into the reaction kettle, add 700kg of formaldehyde water at the same time, and raise the temperature to 90°C.

[0039] (2) Add 1550kg of phosphorous acid and 1680kg of formaldehyde dropwise at the same time, control the temperature to keep reflux, and delay the addition of formaldehyde to phosphorous acid for 20 minutes.

[0040] (3) After the dropwise addition of formaldehyde, control the temperature at 105±2°C and reflux for 3 hours.

[0041] (4) Detect the content of phosphorous acid, add 75kg of formaldehyde, and continue to keep warm and reflux for 1h.

[0042] (5) Negative pressure steaming to remove ammonium chloride, formaldehyde and hydrochloric acid.

[0043] (6) After reaching normal temperature, add 4000kg of reverse osmosis water to adjust the content of active matter to 5...

Embodiment 3

[0045] A specific preparation and implementation process of low trimethylene amino trimethylene phosphonic acid is:

[0046] (1) Add 550kg of ammonium chloride and 450kg of ATMP mother liquor to the reaction kettle, and at the same time add 700kg of formalin, and raise the temperature to 90°C.

[0047] (2) Add 1550kg of phosphorous acid and 1700kg of formaldehyde dropwise at the same time, control the temperature to keep reflux, and delay the addition of formaldehyde to phosphorous acid for 20 minutes.

[0048] (3) After the dropwise addition of formaldehyde, control the temperature at 105±2°C and reflux for 3 hours.

[0049] (4) Detection of phosphorous acid content.

[0050] (5) Negative pressure steaming to remove ammonium chloride, formaldehyde and hydrochloric acid.

[0051] (6) After reaching normal temperature, add 3850kg of reverse osmosis water to adjust the content of active matter to 50±2%.

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Abstract

The invention relates to a preparation method of low-trimethylene-content amino trimethylene phosphonic acid, which comprises the following specific processing steps: adding ammonium chloride, an amino trimethylene phosphonic acid mother solution and formalin into a reaction kettle, and increasing the temperature to 90 DEG C; dropwisely adding formaldehyde and phosphorous acid, and keeping refluxing while controlling the temperature; after the dropwise addition, performing refluxing reaction while keeping the temperature; detecting the phosphite content, supplementing formaldehyde, and further performing refluxing reaction while keeping the temperature; performing negative pressure outer evaporation to remove the ammonium chloride, the formaldehyde and hydrogen chloride; and cooling, and adding reverse osmosis water to regulate the active matter content. According to the invention, the provided amino trimethylene phosphonic acid has the characteristic of low trimethylene content (the active matter content is 50+ / -2%, and the trimethylene content is 24-26%); and compared with the common commercially available amino trimethylene phosphonic acid, the provided amino trimethylene phosphonic acid has better compatibility with zinc corrosion inhibitor, and can regulate the amount of zinc corrosion inhibitor in a compound product in a wider range. Besides, the invention widens the application range of the amino trimethylene phosphonic acid in different water bodies.

Description

technical field [0001] The invention belongs to the field of chemicals and provides a low-trimethylene amino trimethylene phosphonic acid and a preparation method thereof. Background technique [0002] Organic polyphosphoric acid is a kind of water treatment agent developed in the mid-1960s abroad and confirmed in the 1970s. It has good chemical stability, high temperature resistance, and has the advantages of less dosage, corrosion inhibition and scale inhibition. In addition, organic polyphosphoric acid has excellent chelating ability for many metal ions, so it is widely used in water treatment. The main varieties currently used are amino trimethylene phosphonic acid, hydroxyethylidene diphosphonic acid and ethylenediamine tetramethylene phosphonic acid. Amino trimethylene phosphonic acid is one of the varieties with low cost and easy-to-obtain raw materials. [0003] Amino trimethylene phosphonic acid is a cathodic corrosion inhibitor, which can be dissociated into...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 程终发刘全华万振涛宋盟盟张秀华任泽旭
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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