Preparation technology suitable for electronic grade solid ethylenediamine tetramethylene phosphonic acid

A technology of ethylenediaminetetramethylenephosphonic acid and preparation process, which is applied in the field of preparation technology of electronic grade solid ethylenediaminetetramethylenephosphonic acid, can solve the problem of not specifying the arsenic content, not specifying the purity, and reaching a certain level. requirements and other issues, to achieve the effect of being conducive to filtration operation, eliminating environmental pollution and mild operating conditions

Active Publication Date: 2009-03-11
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the patent specification, it is not specified that its purity can reach the high purity of electronic grade, especially it does not specify that the arsenic content in its products meets certain requirements

Method used

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  • Preparation technology suitable for electronic grade solid ethylenediamine tetramethylene phosphonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Rinse the reactor, condenser, pipeline, valve, metering tank, centrifuge and other equipment once with high-purity water. Put 2000kg of high-purity phosphorous acid and 2000kg of 30% hydrochloric acid into the reactor, start stirring slowly at a stirring rate of 60rpm, add 500kg of ethylenediamine dropwise at 50°C for 4 hours; 1800kg of formaldehyde, adding time of 2 hours, formaldehyde is kept at 75°C for 1 hour after dropping; after the temperature drops to 65°C, add 1200g of crystal nucleating agent ethylenediamine tetramethylene phosphonic acid solid, at this time, crystals are precipitated; After the temperature was raised to 85°C, 1100kg of formaldehyde was added dropwise for 1 hour. After the dropwise addition was completed, the temperature was kept for 2 hours; the temperature was gradually lowered to 15°C, and the gradient cooling rate was controlled at 25°C per hour. At this time, a large number of crystals were precipitated. Centrifuge with a centrifuge at a ...

Embodiment 2

[0046] Rinse the reaction kettle, condenser, pipeline, valve, metering tank, centrifuge and other equipment twice with high-purity water. Put 1200kg of high-purity phosphorous acid and 800kg of 30% hydrochloric acid into the reaction kettle, start stirring slowly at a stirring rate of 60rpm, add 320kg of ethylenediamine dropwise at 50°C for 2 hours; 800kg of formaldehyde, adding time of 2 hours, after dropping the formaldehyde, keep it at 75°C for 1 hour; after the temperature drops to 65°C, add 800g of crystal nucleating agent ethylenediamine tetramethylene phosphonic acid solid, at this time, crystals are precipitated; After the temperature was raised to 85°C, 800kg of formaldehyde was added dropwise for 1 hour. After the dropwise addition was completed, the temperature was kept for 2 hours; the temperature was gradually lowered to 35°C, and the gradient cooling rate was controlled at 15°C per hour. At this time, a large number of crystals were precipitated. Centrifuge with ...

Embodiment 3

[0048] According to the operating procedure of Example 1, 1000 g of crystal nucleating agent hydroxyethylene diphosphoric acid was added, and the others were the same as in Example 1. After testing, the active content of the product in terms of EDTMPA is 98%, and the content of arsenic is 0.2mg / L.

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Abstract

The invention discloses a production process of high-purity solid ethylene diamine tetra (methylene phosphonic acid). The production process comprises the following steps: (1) first-phrase preparation which is to clean related equipment; (2) dissolving orthophosphorous acid crystals in high-purity water for recrystallization, and obtaining high purity orthophosphorous acid for later use; (3) placing the high-purity orthophosphorous acid and hydrochloric acid into a reaction kettle with stirring and temperate raising, and dripping ethylene diamine into the reaction kettle; (4) dripping methyl alcohol and keeping temperature; (5) dripping crystal nucleating agent till crystals are precipitated; (6) raising temperature and continuing to dripping methyl alcohol; (7) decreasing temperature step by step; (8) centrifugation, drying, screening and packaging. The white solid particles of EDTMPA has a content of active EDTMPA of more than 95 percent, a content of arsenic less than 0.5 mg/L. The high-purity solid ethylene diamine tetra (methylene phosphonic acid) can be used as metal-chelator for textile dyeing industry, a washing agent for electronic industry, a metal conditioner, etc., and has the advantages of simple package, convenient storage and transportation.

Description

technical field [0001] The invention relates to a high-purity solid ethylenediamine tetramethylene phosphonic acid (EDTMPA), in particular to a high-purity solid ethylenediamine suitable for use as a cleaning agent and a metal surface treatment agent in the electronics industry. Preparation process of tetramethylene phosphonic acid (EDTMPA). Background technique [0002] EDTMPA has a strong ability to chelate metal ions, and its complexation constant with copper ions is the largest among all chelating agents including EDTA. EDTMPA is a high-purity reagent and non-toxic. It can be used as a cleaning agent for semiconductor chips in the electronics industry to manufacture integrated circuits; it can be used as a carrier of radioactive elements in the pharmaceutical industry for inspection and treatment of diseases; the chelating ability of EDTMPA far exceeds that of EDTA And DTPA, EDTMPA can be used in almost all places where EDTA is used as a chelating agent. [0003] Howev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 程终发孙宝季
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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