Continuous synthesis technique of hydroxyethylidenediphosphonic acid

A hydroxyethylene diphosphonic acid, chemical synthesis technology, applied in the field of industrial water treatment, can solve the problems of low yield, high content of phosphorous acid and phosphoric acid, many side reactions, etc., to overcome low yield and reduce labor intensity , The effect of reducing product cost

Active Publication Date: 2015-05-06
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product yield of the continuous production process of hydroxyethylene diphosphonic acid is greater than 95%, and the product quality can reach a phosphorus content of less than 1.0%, and a phosphorus content of less than 0.5%, which overcomes the low yield and many side reactions of other preparation processes. Disadvantages of high content of phosphorous acid and phosphoric acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Pump acetic acid and phosphorus trichloride into the mixing tank, stir evenly, pump the uniformly mixed material into the tubular reactor, the material reaches the gas-liquid separator after passing through the tubular reactor, and is separated by the gas-liquid separator , Acetyl chloride and hydrochloric acid enter the rectification tower, and are collected separately after rectification and separation. Acetate enters the hydrolysis external steamer to continue the hydrolysis reaction to obtain hydroxyethylidene diphosphonic acid and acetic acid. The acetic acid is removed by negative pressure external steaming. Collect and reuse. Specifically, the method of the present invention comprises the following steps:

[0033] (1) Mixing of raw materials: respectively pump phosphorus trichloride and acetic acid stored in the storage tank into the mixing kettle continuously, the pumping speed of phosphorus trichloride is controlled at 100 liters / hour, and the pumping speed of ...

Embodiment 2

[0041] Pump acetic acid and phosphorus trichloride into the mixing tank, stir evenly, pump the uniformly mixed material into the tubular reactor, the material reaches the gas-liquid separator after passing through the tubular reactor, and is separated by the gas-liquid separator , Acetyl chloride and hydrochloric acid enter the rectification tower, and are collected separately after rectification and separation. Acetate enters the hydrolysis external steamer to continue the hydrolysis reaction to obtain hydroxyethylidene diphosphonic acid and acetic acid. The acetic acid is removed by negative pressure external steaming. Collect and reuse. Specifically, the method of the present invention comprises the following steps:

[0042] (1) Mixing of raw materials: respectively pump phosphorus trichloride and acetic acid stored in the storage tank into the mixing kettle continuously, the pumping speed of phosphorus trichloride is controlled at 100 liters / hour, and the pumping speed of ...

Embodiment 3

[0049] Embodiment 3 (best embodiment):

[0050] Pump acetic acid and phosphorus trichloride into the mixing tank, stir evenly, pump the uniformly mixed material into the tubular reactor, the material reaches the gas-liquid separator after passing through the tubular reactor, and is separated by the gas-liquid separator , Acetyl chloride and hydrochloric acid enter the rectification tower, and are collected separately after rectification and separation. Acetate enters the hydrolysis external steamer to continue the hydrolysis reaction to obtain hydroxyethylidene diphosphonic acid and acetic acid. The acetic acid is removed by negative pressure external steaming. Collect and reuse. Specifically, the method of the present invention comprises the following steps:

[0051] (1) Mixing of raw materials: respectively pump phosphorus trichloride and acetic acid stored in the storage tank into the mixing kettle continuously, the pumping speed of phosphorus trichloride is controlled a...

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Abstract

The invention relates to a continuous synthesis technique of hydroxyethylidenediphosphonic acid, which comprises the following steps: 1. mixing raw materials: mixing phosphorus trichloride and acetic acid in a mol ratio of 1:(2.8-3.0) in a mixing kettle; 2. sending the mixture into a tubular reactor: pumping the mixture into the tubular reactor through a diaphragm pump; 3. carrying out esterification reaction while controlling the temperature of the tubular reactor at 70-130 DEG C; 4. separating the reaction mixture in a gas-liquid separator for recycling; 5. carrying out hydrolysis reaction to obtain the hydroxyethylidenediphosphonic acid; and 6. distilling out acetic acid under negative pressure to separate the acetic acid from the product, wherein the acetic acid enters an acetic acid storage tank as a raw material. In the invention, the hydroxyethylidenediphosphonic acid is continuously produced in a semi-closed system, thereby changing the existing intermittent production mode and enhancing the production efficiency; and the invention overcomes the defects of low product yield, too many side reactions and high contents of phosphorous acid and phosphoric acid in other preparation techniques, and implements complete cyclic utilization of acetic acids with different concentrations.

Description

technical field [0001] The invention belongs to the technical field of industrial water treatment, and in particular relates to a production method of an organic phosphine water treatment agent. Background technique [0002] Hydroxyethylene diphosphonic acid (HEDP) is widely used as a water treatment agent (water quality stabilizer) in industrial circulating cooling water systems. It has good scale and corrosion inhibition, and is an anionic corrosion inhibitor. Its oxidation resistance is better than that of aminotrimethylene phosphate (ATMP) and ethylenediaminetetramethylene phosphate (EDTMP), and it decomposes at 250°C. . It has a good effect on inhibiting calcium carbonate, hydrated iron oxide and calcium phosphate, and it has a synergistic effect when used in conjunction with other corrosion and scale inhibitors. At present, the environmental protection department strictly controls the discharge of phosphate, and the industrial circulating water and boiler feed water ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38C07C53/40C07C51/60C01B7/01
Inventor 程终发齐晓婧孙群峰刘全华万振涛
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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