Preparation technology suitable for electronic grade solid hexamethylenediamine tetramethylene phosphonic acid

A technology for the preparation of hexamethylene diamine tetramethylene phosphonic acid, which is applied in the field of preparation of high-purity solid hexamethylene diamine tetramethylene phosphonic acid. and other issues, to achieve the effect of eliminating environmental pollution, mild operating conditions, and conducive to filtering operations

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 electro

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0043] Example 1:

[0044] Use high-purity water to flush the reactor, condenser, pipeline, valve, centrifuge and other related equipment once. Put 2000kg of high-purity phosphorous acid and 2000kg of 30% hydrochloric acid into the reactor, stir slowly, stir at 60rpm, and add 500kg of hexamethylenediamine dropwise at 50℃ for 4 hours; after dripping, heat to 60℃ and add dropwise 1800kg of formaldehyde, 2 hours of dropping time, after dropping formaldehyde, keeping it at 75°C for 1 hour; after the temperature drops to 65°C, add crystal nucleating agent 1200g of diaminetetramethylenephosphonic acid solid, at this time crystals are precipitated; After the temperature was raised to 85°C, 1100kg of formaldehyde was added dropwise. The dropping time was 1 hour. After the dropping, 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 amount of crystals were precipitated. Ce...

Example Embodiment

[0045] Example 2:

[0046] Use high-purity water to flush the reactor, condenser, pipeline, valve, centrifuge and other related equipment once. Put 1200kg of high-purity phosphorous acid and 800kg of 30% hydrochloric acid into the reactor, stir slowly, stir at 60rpm, add 320kg of hexamethylenediamine dropwise at 50℃ for 2 hours; after dripping, heat up to 60℃ and add dropwise 800kg of formaldehyde, dripping time for 2 hours, after dripping formaldehyde, keep it at 75°C for 1 hour; after the temperature drops to 65°C, add 800g of crystal nucleating agent diamine tetramethylene phosphonic acid solid, at this time crystals precipitate; After the temperature was raised to 85°C, 800kg of formaldehyde was added dropwise. The dropping time was 1 hour. After the dropping was completed, the temperature was kept for 2 hours; the temperature was gradually reduced to 35°C, and the gradient cooling rate was controlled at 15°C per hour. At this time, a large amount of crystals were precipitated...

Example Embodiment

[0047] Example 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 based on HDTMPA is 98%, and the content of arsenic is 0.3mg / L.

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Abstract

The invention relates to a process for preparing electronic grade hexamethylenediaminetetra (methylenephosphonic acid) solid. The 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 30 percent hydrochloric acid into a reaction kettle with stirring and temperate raising, and dripping ethylene diamine into the reaction kettle; (4) raising temperature, dripping methyl alcohol and then keeping temperature; (5) after slight temperature drop, 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 as a solid.

Description

technical field [0001] The invention relates to a preparation process of high-purity solid hexamethylenediaminetetramethylenephosphonic acid (HDTMPA), in particular to a high-purity solid suitable for electronic grades that can be used as a cleaning agent and a metal surface treatment agent in the electronics industry. The preparation process of hexamethylene diamine tetramethylene phosphonic acid (HDTMPA). Background technique [0002] HDTMPA has a strong ability to chelate metal ions, and its complexation constant with copper ions is the largest among all chelating agents including EDTA. HDTMPA 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; HDTMPA's chelation ability far exceeds EDTA And DTPA, almost all places where EDTA is used as a ...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 程终发孙宝季魏学清
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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