Preparing process adapted for electronic grade solid hydroxyethylidene diphosphonic acid

A hydroxyethylene diphosphonic acid and a preparation technology, which is applied in the field of preparation of high-purity solid hydroxyethylene diphosphonic acid, can solve the problems of not specifying the arsenic content, not specifying the purity, meeting certain requirements, etc., reaching It is beneficial to filter operation, prevent environmental pollution, and have mild operating conditions.

Active Publication Date: 2007-08-15
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

[0010] 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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  • Preparing process adapted for electronic grade solid hydroxyethylidene diphosphonic acid

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preparation example Construction

[0044] The preparation technique of the present invention has very significant advantages: (1) the active content of the solid hydroxyethylene diphosphonic acid product produced by the present invention is more than 95% in terms of HEDP, and the content of arsenic is reduced from 70ppm in the previous liquid product Below 7ppm in the solid product, the content of impurities is greatly reduced, which can meet the quality requirements of the electronic industry for high-purity hydroxyethylidene diphosphonic acid; (2) the operating conditions of the present invention are mild, and the production process has no corrosion and no waste discharge , is a green production process; (3) the present invention does not need to add organic solvents, thereby eliminating the pollution to the environment caused by VOC emissions; (4) the present invention has a large crystal size, which is conducive to filtering operations and high product yield; (5) The solid hydroxyethylidene diphosphonic acid...

Embodiment 1

[0047] Rinse the reaction kettle, condenser, pipeline, valve, centrifuge and other related equipment once with high-purity water, add 3 tons of liquid hydroxyethylidene diphosphonic acid with a weight percentage of 50%, start stirring, and heat up to 70°C for use Vacuum negative pressure, vacuum dehydration 500kg, at this time the temperature should not be higher than 100 ℃, natural cooling, slow cooling after 2 hours, when the temperature drops to 55 ℃, add seed crystal amino trimethylene phosphonic acid and hydroxyethylene 150g each of diphosphonic acids, slow down the stirring speed to 30rpm, keep the temperature down 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 controlled at 2000rpm. The solid obtained after centrifugation is high-puri...

Embodiment 2

[0049] Rinse the reaction kettle, condenser, pipeline, valve, centrifuge and other related equipment once with high-purity water, add 3 tons of liquid hydroxyethylidene diphosphonic acid with a weight percentage of 50%, start stirring, and heat up to 60°C Use vacuum to pull negative pressure and vacuum dehydrate 700kg. At this time, the temperature should not be higher than 110°C, and the temperature should be lowered naturally. After 1 hour, the temperature should be slowly lowered. When the temperature drops to 75°C, add seed crystal sodium acetate and aminotrimethylenephosphonic acid 200g each, 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 ...

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Abstract

The invention discloses a making method of electron-grade solid hydroxy trimethylphosphine, which comprises the following steps: (1) cleaning autoclave, condenser and relative equipment clearly; (2) weighing liquid hydroxy 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 HEDP 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 hydroxyethylene diphosphonic acid (HEDP), in particular to a kind of electronic-grade solid hydroxyethylene diphosphonic acid (HEDP) which can be used as a cleaning agent and a metal surface treatment agent in the electronics industry. Preparation process of diphosphonic acid. Background technique [0002] Hydroxyethylidene diphosphonic acid (hereinafter referred to as HEDP) is an organic phosphonic acid scale and corrosion inhibitor, which can form stable complexes with various metal ions such as iron, copper, zinc, etc., and can dissolve oxidation on the metal surface. things. HEDP is generally used as an anti-scaling agent for circulating cooling water, oil field water injection and printing and dyeing water. Its acid and alkali resistance and chlorine oxidation resistance are better than other organic phosphonic acids (salts). It can form six-ring chelates with metal ions in wate...

Claims

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Application Information

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