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Preparation method of hydroxyethylidene diphosphonic acid

A technology of hydroxyethylene diphosphonic acid and glacial acetic acid, applied in the field of industrial water treatment, can solve the problems of many side reactions, high production cost per ton of product, long reaction period, etc., so as to reduce the occurrence of side reactions and shorten the reaction period , the effect of improving the efficiency of esterification

Inactive Publication Date: 2019-07-02
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN106588979A discloses a multi-stage non-powered bubbling method for synthesizing hydroxyethylene diphosphonic acid. Therefore, although this process has the advantages of low equipment investment and easy operation, it mostly adopts single or multi-pot intermittent production method, the product yield is low, the production cost per ton of product is high, and due to the long reaction cycle and complicated route, there are many side reactions, which easily lead to high phosphorus content in the product, which affects product quality and performance, and also greatly limits industrial production capacity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) At room temperature, mix 550g of phosphorus trichloride and 1100g of glacial acetic acid (m (三氯化磷) :m （冰醋酸） =1:2.0) mix well;

[0036] (2) Pump the homogeneously mixed materials in step (1) into the disc-type PTFE reaction tube, and then inject HCl gas to ensure that the reaction tube is HCl atmosphere, and then the inlet and outlet of the reaction tube are fixed with wires. Tie up the seal and immerse in an oil bath at 170±2°C, heat and react under 0.318MPa pressure for 45min;

[0037] (3) After the reaction is over, take out the esterification product while it is hot and put it into the kettle, add 350g of water and 13.80g of catalyst (hydroxyethylene diphosphonic acid with an active content of 60%), fully stir and hydrolyze at 125~130°C for 1.5 hours , decolorized by activated carbon to obtain 664.20 g of a colorless and transparent liquid hydroxyethylene diphosphonic acid product, the activity (calculated by HEDP) was 60.41%, and the yield (calculated by the i...

Embodiment 2

[0041] (1) At room temperature, mix 550g of phosphorus trichloride and 1485g of glacial acetic acid (m (三氯化磷) :m （冰醋酸） =1:2.7) mixed with 1% concentrated hydrochloric acid;

[0042] (2) Pump the homogeneously mixed materials in step (1) into the disc-type PTFE reaction tube, and then inject HCl gas to ensure that the reaction tube is HCl atmosphere, and then the inlet and outlet of the reaction tube are fixed with wires. Tie up the seal and immerse in an oil bath at 165±2°C, heat and react for 50min under a pressure of 0.403MPa;

[0043] (3) After the reaction is over, take out the esterification product and put it into the kettle, add 350g of water and 12.36g of catalyst (60% hydroxyethylene diphosphonic acid), stir and hydrolyze it for 2 hours at 125~130°C, pass through activated carbon After decolorization, 669.35 g of hydroxyethylene diphosphonic acid product was obtained as a colorless transparent liquid, the activity (calculated as HEDP) was 60.34%, and the yield (calc...

Embodiment 3

[0047] (1) At room temperature, mix 550g of phosphorus trichloride and 990g of glacial acetic acid (m (三氯化磷) :m （冰醋酸） =1:1.8) mix well;

[0048] (2) Pump the homogeneously mixed material in step (1) into the disc-type PTFE reaction tube, and then inject HCl gas to ensure the HCl atmosphere in the reaction tube. The inlet and outlet of the reaction tube are tied with fixed wires. Well-sealed and immersed in an oil bath at 155±2°C, heated and reacted for 25 minutes under a pressure of 0.381MPa;

[0049] (3) After the reaction is over, take out the esterification product and put it into the kettle, add 350g of water and 13.80g of catalyst (60% hydroxyethylene diphosphonic acid), stir and hydrolyze it for 1 hour at 125~130°C, pass through activated carbon After decolorization, 662.66 g of hydroxyethylene diphosphonic acid product was obtained as a colorless transparent liquid, the activity (calculated as HEDP) was 60.47%, and the yield (calculated as phosphorus trichloride input...

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Abstract

The invention discloses a preparation method of hydroxyethylidene diphosphonic acid. The method specifically comprises the following steps: (1) uniformly mixing phosphorus trichloride and glacial acetic acid in a mass ratio of 1:(1.3-3.0); (2) feeding the uniformly mixed materials in the step (1) into a reaction tube, closing the reaction tube, immersing the reaction tube into an oil bath at 130-240 DEG C, and carrying out heating reaction for 15-100 minutes under the pressure of 0.3-0.5 MPa; and (3) after the reaction is finished, moving out an esterification product while hot, feeding the esterification product into a reaction kettle, adding water and a catalyst, and fully stirring and hydrolyzing the esterification product at 125-130 DEG C for 1-2 hours. Under the conditions of increasing reaction pressure and at high temperature, phosphorus trichloride and glacial acetic acid are used as raw materials to complete rapid esterification in a sealed reaction tube in an anhydrous environment; and then carrying out catalytic hydrolysis, rectification purification separation and other treatments to synthesize the hydroxyethylidene diphosphonic acid. According to the method, the esterification reaction time is effectively shortened, side reactions are reduced, and the product yield is increased.

Description

technical field [0001] The invention belongs to the technical field of industrial water treatment, and in particular relates to a preparation method of a water treatment agent hydroxyethylene diphosphonic acid. Background technique [0002] Hydroxyethylenediphosphonic acid is an anionic corrosion inhibitor. Compared with other similar products such as aminotrimethylenephosphonic acid, ethylenediaminetetramethylenephosphonic acid and its salts, it has higher oxidation resistance and thermal stability. sex. At the same time, it has a good inhibitory effect on carbonate scale, iron scale and phosphate scale, and shows a good synergistic effect when compatible with other chemicals. Therefore, hydroxyethylene diphosphonic acid has been used as the main component of low-phosphorus formulations, and is widely used in the treatment of circulating cooling water in petrochemical, electric power, chemical fertilizer and other industrial production equipment. [0003] The preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3808
Inventor 程终发齐晓婧王燕平王东海刘全华
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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