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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

AI Technical Summary

Problems solved by technology

[0011] In the patent specification, it is not specified that its purity can reach the high purity of the electronic grade, and it is not specified that the arsenic content in its products meets certain requirements.

Method used

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  • Preparing process adapted for electronic grade solid aminotrimethylene phosphonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Rinse the reaction kettle, condenser, pipeline, valve, centrifuge and other related equipment once with high-purity water, add 3 tons of liquid aminotrimethylene phosphonic acid with a weight percentage of 50%, start stirring, and heat up to 70°C with vacuum Pull negative pressure and vacuum dehydrate 500kg. At this time, the temperature should not be higher than 100°C, and the temperature should be lowered naturally. After 2 hours, the temperature should be slowly lowered. When the temperature drops to 55°C, add seed crystals of aminotrimethylene phosphonic acid and hydroxyethylene 150g of diphosphonic acid each, slow down the stirring speed to 30rpm, keep the temperature lowered slowly at a rate of 15°C per hour, and keep aging at this temperature for 12 hours when it drops to room temperature. Open the discharge valve at the bottom of the kettle, put the feed liquid into the high-speed centrifuge for centrifugal dehydration, and the speed of the centrifuge is controll...

Embodiment 2

[0051] Rinse the reaction kettle, condenser, pipeline, valve, centrifuge and other related equipment once with high-purity water, add 3 tons of liquid aminotrimethylene phosphonic acid with a weight percentage of 50%, start stirring, and heat up to 60°C with a vacuum Pull negative pressure and vacuum dehydrate 700kg. At this time, the temperature should not be higher than 110°C. Let the temperature drop naturally, and slowly cool down after 1 hour. When the temperature drops to 75°C, add sodium acetate and hydroxyethylidene diphosphonic acid respectively. 200g, slow down the stirring speed to 50rpm, at this time, keep the temperature slowly lowered, the cooling rate per hour is 25°C, when it drops to room temperature, keep aging at this temperature for 6 hours. Open the discharge valve at the bottom of the kettle, put the feed liquid into the high-speed centrifuge for centrifugal dehydration, and the speed of the centrifuge is controlled at 1000rpm. The solid obtained after ce...

Embodiment 3

[0053] By the operation procedure of embodiment 1, vacuum dehydration 900kg. After being lowered to room temperature, keep aging at this temperature for 10 hours, and the others are the same as in Example 1. After testing, the active content of the product in terms of ATMP is 98%, and the content of arsenic is 3.4ppm.

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PUM

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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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