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Production process of diethylenetriaminepenta(methylene-phosphonic acid)

A technology of diethylenetriamine pentamethylene phosphonic acid and diethylenetriamine, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve unfavorable industrial production of DTPMPA, Increase the content of by-product hydroxymethylphosphonic acid, increase the relative rate of side reactions, etc., to achieve the effects of shortening the total reaction time, inhibiting the production of by-product hydroxymethylphosphonic acid, and improving conversion rate and product yield

Active Publication Date: 2020-02-18
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to completely react diethylenetriamine and phosphorous acid in production, a large amount of excess formaldehyde is usually added, and the recovery and treatment of excess formaldehyde need to consume a lot of resources, and as the concentration of the reaction system decreases, the main reaction rate gradually slows down, and the The relative rate of the reaction increases, which not only increases the content of the by-product hydroxymethylphosphonic acid, but also leads to a long production cycle
Above deficiency is all unfavorable for the industrialized production of DTMPPA

Method used

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  • Production process of diethylenetriaminepenta(methylene-phosphonic acid)

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Experimental program
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Effect test

Embodiment 1

[0024] Add 2813Kg of phosphorous acid aqueous solution with a mass fraction of 71.25% and 2250Kg of hydrochloric acid with a mass fraction of 31.50% into the reactor in sequence, start the stirring and tail gas recovery device, then slowly add 500.0Kg of diethylenetriamine dropwise to the reactor, and the temperature in the reactor is controlled Below 50°C, after the neutralization reaction is completed, heat up to keep the temperature in the reactor at 115±2°C, set and automatically control the formaldehyde drop rate: 250Kg / h for 0.5 hours, 500Kg / h for 0.5 hours , 1000Kg / h was added dropwise to the end of the first stage, and a total of 1573Kg of formaldehyde solution with a mass content of 40.73% was added dropwise. After 1 hour of heat preservation and reaction at 115±2°C, it was evaporated and concentrated to near dryness under normal pressure and then negative pressure conditions; stop negative pressure pressure, and add 225Kg hydrochloric acid to the system, control the s...

Embodiment 2

[0026] Add 2703Kg of phosphorous acid aqueous solution with a mass fraction of 70.69% and 2441Kg of hydrochloric acid with a mass fraction of 32.66% into the reactor in sequence, start the stirring and tail gas recovery device, then slowly add 500.0Kg of diethylenetriamine dropwise to the reactor, and the temperature in the reactor is controlled Below 50°C, after the neutralization reaction is completed, heat up to keep the temperature in the reactor at 115±2°C, set and automatically control the formaldehyde drop rate: 250Kg / h for 0.5 hours, 500Kg / h for 0.5 hours , 1000Kg / h was added dropwise to the end of the first stage, and a total of 1716Kg of formaldehyde solution with a mass content of 40.73% was added dropwise. After 1 hour of heat preservation and reaction at 115±2°C, it was evaporated and concentrated to near dryness under normal pressure and then negative pressure conditions; stop negative pressure Pressure, and add 225Kg hydrochloric acid to the system, control the s...

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Abstract

The invention discloses a production process of diethylenetriaminepenta(methylene-phosphonic acid). The production process comprises the following specific operation steps: (1) adding metered hydrochloric acid, diethylenetriamine and phosphorous acid into a reactor in order, performing continuous stirring in the reactor, and maintaining the temperature at <=50 DEG C; (2) performing heating to a certain temperature, adding a part of a formaldehyde aqueous solution dropwise at different flow rates, after the addition is completed, performing heat preservation, and performing concentration; and (3) adding hydrochloric acid, performing heating to 110-120 DEG C, adding the remaining formaldehyde aqueous solution dropwise, after the addition is completed, performing heat preservation for a reaction, performing evaporation, performing dilution, performing cooling, and adjusting the pH to obtain the qualified finished product. The method accelerates the reaction rate, not only effectively inhibits the production of by-product hydroxymethylphosphonic acid, improves the conversion rate and product yield of the effective active component diethylenetriaminepenta(methylene-phosphonic acid), butalso shortens the total reaction time, and reduces the production costs; and the method is simple, safe, and easy to operate, and is beneficial to industrial production.

Description

technical field [0001] The invention belongs to the technical field of industrial water treatment agent chemical industry, and in particular relates to a production process of diethylenetriaminepentamethylenephosphonic acid. Background technique [0002] Diethylenetriaminepentamethylenephosphonic acid (DTMPPA), also known as diethylenetriaminepentamethylenephosphonic acid, is an organic phosphonic acid scale and corrosion inhibitor. Its molecular structure contains C-P bonds, which are compatible with Compared with the total P-O-P or C-O-P bond of inorganic polymeric phosphate, it has stronger bond energy and stronger bond. Therefore, it has high temperature thermal stability, and its corrosion inhibition performance is 4~7 times stronger than that of inorganic polymeric phosphate. [0003] At the same time, DTPMPA can be dissociated into ten positive ions and ten negatively charged ions in water, and can interact with Ca in water. 2 + , Mg 2+ etc. to form polycyclic ring...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3808
Inventor 程终发林学洲齐晓婧宋盟盟周响刘全华
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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