Preparing process adapted for electronic grade solid aminotrimethylene phosphonic acid

A technology for preparation of aminotrimethylene phosphonic acid, which is applied in the field of preparation technology of electronic-grade solid aminotrimethylene phosphonic acid, can solve the problems of not specifying the purity, meeting certain requirements, not specifying the arsenic content, etc., so as to eliminate Environmental pollution, mild operating conditions, beneficial to the effect of filtration operation

Active Publication Date: 2007-08-15
山东泰和科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In the patent specification, it is not specified that its purity can reach the high purity of the el

Method used

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  • Preparing process adapted for electronic grade solid aminotrimethylene phosphonic acid

Examples

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Example Embodiment

[0048] Example 1:

[0049] Wash the reactor, condenser, pipeline, valve, centrifuge and other related equipment with high-purity water once, add 3 tons of liquid amino trimethylene phosphonic acid with a content of 50% by weight, start stirring, and raise the temperature to 70 ℃ with vacuum Pull negative pressure and vacuum dehydrate 500kg. At this time, the temperature should not be higher than 100℃, and the temperature should be lowered naturally. After 2 hours, the temperature will be slowly lowered. When the temperature drops to 55℃, add seed crystal amino trimethylene phosphonic acid and hydroxy ethylene 150g each of the bisphosphonic acid, slow down the stirring speed to 30rpm, at this time, keep the temperature slowly lowered, and the temperature drop rate per hour is 15°C. When it drops to room temperature, keep it for 12 hours at this temperature. Open the discharge valve at the bottom of the kettle, and put the material liquid into the high-speed centrifuge for centrifug...

Example Embodiment

[0050] Example 2:

[0051] Rinse the reactor, condenser, pipeline, valve, centrifuge and other related equipment with high-purity water once, add 3 tons of liquid amino trimethylene phosphonic acid with a content of 50% by weight, start stirring, and raise the temperature to 60 ℃ with vacuum Pull negative pressure, vacuum dehydration 700kg. At this time, the temperature should not be higher than 110℃, and the temperature should be lowered naturally. After 1 hour, the temperature will be slowly lowered. When the temperature drops to 75℃, add seed crystal sodium acetate and hydroxyethylene diphosphonic acid. 200g, slow down the stirring speed to 50rpm, at this time, keep the temperature slowly lowered, and the temperature drop rate per hour is 25°C. When it drops to room temperature, keep it for 6 hours at this temperature. Open the discharge valve at the bottom of the kettle, and put the material liquid into the high-speed centrifuge for centrifugal dewatering, and the speed of the...

Example Embodiment

[0052] Example 3:

[0053] According to the operating procedure of Example 1, 900kg was vacuum dehydrated. After it is lowered to room temperature, it is kept at this temperature for aging for 10 hours. After testing, the active content of the product based on ATMP is 98%, and the content of arsenic is 3.4ppm.

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Abstract

The invention discloses a making method of electron-grade solid amino trimethylphosphine, which comprises the following steps: (1) cleaning autoclave, condenser and relative equipment clearly; (2) weighing liquid trimethylphosphine into autoclave; stirring; (3) dehydrating in the vacuum under 35-120 deg.c; (4) cooling to 40-90 deg.c naturally; adding seed with quantity at 50-50000ppm; (5) cooling to indoor temperature; stewing; aging 4-20h; (7) centrifuging at high-speed centrifuger to dehydrate with velocity at 500-5000r/min; (8) packing the solid ATMP with activity over 95% and arsenic content less than 7ppm.

Description

technical field [0001] The invention relates to a preparation process of high-purity solid aminotrimethylenephosphonic acid (ATMP), in particular to a kind of solid aminotrimethylenephosphine suitable for electronic grade as cleaning agent and metal surface treatment agent in the electronics industry. Acid (ATMP) preparation process. Background technique [0002] Aminotrimethylenephosphonic acid (hereinafter referred to as ATMP) can be dissociated into 6 positive ions and 6 negatively charged ions in water, and can form polycyclic ring chelates with calcium and magnesium ions in water, and disperse in water in a loose manner. The normal crystallization of calcium and magnesium scale is destroyed. Therefore, ATMP has a good scale inhibition effect on calcium carbonate, magnesium silicate, calcium sulfate, etc. in water. One molecule of ATMP can prevent dozens to hundreds of calcium, magnesium ions, and sulfate ions from producing scale precipitation. This is its unique anti...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 程终发孙宝季刘坤
Owner 山东泰和科技股份有限公司
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