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Preparation process for a solid aminotrimethylenephosphonic acid (ATMP) or 1-hydoxy ethyidene-1.1-diphosphonic acid

A technology of aminotrimethylene phosphonic acid and hydroxyethylene diphosphonic acid, which is applied in the fields of compounds, chemical instruments and methods, and organic chemistry of elements of Group 5/15 of the periodic table to achieve the effect of reducing packaging costs

Inactive Publication Date: 2009-12-09
CHANGZHOU YAOS TONGDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the above-mentioned defects, the technical problem to be solved in the present invention is to provide a solid aminotrimethylene phosphonic acid or hydroxyethylene diphosphine for the problem of introducing impurity crystal nuclei in the solid preparation process. The preparation technology of phosphonic acid or hydroxyethylene diphosphonic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 600kgCH to a 1000L glass-lined kettle with stirring and reflux condensation device 3 COOH, water 200 ~ 150kg, under the premise that the cooling water of the condenser is opened at a high level and the reflux of the cooling water is smooth and the absorption of hydrogen chloride is smooth, add 500kg of phosphorus trichloride dropwise at a temperature below 45°C, and the time is not less than 5 hours. State The main kettle is heated to 50-60°C and the temperature is controlled to 50-60°C. Add 500kg of phosphorus trichloride dropwise for no less than 5 hours. After the second drop of phosphorus trichloride, start to slowly heat to 105°C-140°C for 3 hours. . At the end of the heat preservation, control the temperature at 90-120°C and add 200kg of water dropwise. After the water drips, keep the flow state for 1-3 hours, and then pass steam from the bottom to purge the material directly with steam for 4-5 hours (or the distillate has no CH 3 COOH odor) to recover the hy...

Embodiment 2

[0024] The aminotrimethylene phosphonic acid liquid that can be purchased on the market is used as a refined raw material. The content of aminotrimethylene phosphonic acid in the aminotrimethylene phosphonic acid liquid that can be purchased on the market is 50-60%, which cannot reach According to the requirements of this refining process, the aminotrimethylene phosphonic acid needs to be concentrated and dehydrated before use, so that the aminotrimethylene phosphonic acid content in the aminotrimethylene phosphonic acid liquid is 68-85%, and then it is produced and solidified.

[0025] a. Crystallization: Control the temperature of the aminotrimethylene phosphonic acid liquid with an active substance content of 68-85% at 45° C., add ice crystal particles to the aminotrimethylene phosphonic acid liquid to precipitate crystals;

[0026] b. Solid-liquid separation: after the crystal precipitation stops, the material is subjected to centrifugal dehydration, and the solid is aminot...

Embodiment 3

[0029] Add 120kgNH to a 1000L glass-lined kettle with stirring and reflux condensing device, hydrogen chloride absorption device, dripping device 4 Cl, 500-1000kg of water, under the premise that the cooling water of the condenser is turned on and the absorption of hydrogen chloride is smooth, add 900kg of phosphorus trichloride dropwise at a temperature below 45°C, and the time is not less than 5 hours. After the phosphorus is dripped, start to slowly heat to 95°C-105°C and drop 750kg of formaldehyde solution at 95°C-105°C under reflux control for 1-5 hours. The temperature of the reactor is controlled by the speed of dropping formaldehyde. After dropping the formaldehyde, keep the flow state for 1-3 hours and then pass steam from the bottom to purge the material directly with steam for 4-5 hours (or the distillate has no formaldehyde smell).

[0030] B[amino trimethylene phosphonic acid (ATMP)]} solid preparation: the above-mentioned [amino trimethylene phosphonic acid (ATMP...

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Abstract

The invention relates to a preparation process for a solid aminotrimethylenephosphonic acid (ATMP) or 1-hydoxy ethyidene-1.1-diphosphonic acid, in particular to a high purity preparation process for the solid aminotrimethylenephosphonic acid (ATMP) or the 1-hydoxy ethyidene-1.1-diphosphonic acid, comprising the following steps: a, crystallization: controlling the temperature of the aminotrimethylenephosphonic acid (ATMP) or 1-hydoxy ethyidene-1.1-diphosphonic acid with 68-85% of the content of effective substance at 30-90 DEG C, adding ice crystal particles, and then precipitating the crystal; b, solid-liquid separation: carrying out centrifugal dewatering on the materials after crystal precipitation, and obtaining the sold aminotrimethylenephosphonic acid (ATMP) or the 1-hydoxy ethyidene-1.1-diphosphonic acid; c, product post-treatment: drying the solid aminotrimethylenephosphonic acid (ATMP) or the 1-hydoxy ethyidene-1.1-diphosphonic acid, removing crystal water under the temperature of 60-120 DEG C, then solid packing. The preparation process in the invention solves the problem of introducing impurity crystal nucleus in the solid preparation process of the aminotrimethylenephosphonic acid (ATMP) or the 1-hydoxy ethyidene-1.1-diphosphonic acid.

Description

technical field [0001] The invention relates to a preparation process of solid aminotrimethylene phosphonic acid or hydroxyethylene diphosphonic acid, in particular to a preparation process of high-purity solid aminotrimethylene phosphonic acid or hydroxyethylene diphosphonic acid. Background technique [0002] Aminotrimethylenephosphonic acid (hereinafter referred to as ATMP) and hydroxyethylenediphosphonic acid (abbreviated as HEDP) are commonly used water treatment reagents. Aminotrimethylenephosphonic acid ATMP can dissociate into 6 positive ions and 6 positive ions in water. A negatively charged ion can form a polycyclic ring chelate with calcium and magnesium ions in water, disperse in water in a loose manner, and destroy the normal crystallization of calcium and magnesium scales. Magnesium, calcium sulfate, etc. have good scale inhibition effect, and one molecule of ATMP can prevent dozens to hundreds of calcium, magnesium ions and sulfate ions from producing scale pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 顾青军姚斌
Owner CHANGZHOU YAOS TONGDE CHEM
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