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Preparation method of low iron and low chloride hydroxyethylidene-1,1-diphosphonic acid (HEDP)

A technology of low-chlorine hydroxyethylene diphosphonic acid and hydroxyethylene diphosphonic acid, which is applied in the field of chemical products to achieve the effect of expanding the application field

Inactive Publication Date: 2013-12-11
SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to meet the special requirements of the market, solve the problem of excessive iron ions and chloride ions in hydroxyethylene diphosphonic acid, and expand the application field of hydroxyethylene diphosphonic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 (best embodiment)

[0023] A preparation method of low-iron, low-chlorine hydroxyethylene diphosphonic acid is implemented through the following specific processes:

[0024] (1) Clean the equipment with high-purity water.

[0025] (2) Add 44% hydroxyethylidene diphosphonic acid solution into the reaction kettle, and steam at 100±5°C and pressure -0.085MPa.

[0026] (3) When the concentration is 78~80%, stop external steaming, and put the material into the crystallization kettle.

[0027] (4) Slowly stir at 50r / min, slowly cool down at 2~4°C / h, when the temperature is ≤60°C, add seed crystal hydroxyethylene diphosphonic acid.

[0028] (5) Cool down naturally to 30-50°C, and dehydrate by centrifugation.

[0029] (6) Add solid hydroxyethylene diphosphonic acid to the reaction kettle, add high-purity water, and repeat steps (2)~(5) 3 times.

[0030] (7) Detect the content of each element Nickel: not detected; iron: 0.0222ppm; copper: not detected; lead: not...

Embodiment 2

[0032] A preparation method of low-iron, low-chlorine hydroxyethylene diphosphonic acid is implemented through the following specific processes:

[0033] (1) Clean the equipment with high-purity water.

[0034] (2) Add 50% hydroxyethylidene diphosphonic acid solution into the reaction kettle, steam at 90±5°C and pressure -0.09MPa.

[0035] (3) When the concentration is 78~80%, stop external steaming, and put the material into the crystallization kettle.

[0036] (4) Slowly stir at 50r / min, slowly cool down at 2~4°C / h, when the temperature is ≤60°C, add seed crystal hydroxyethylene diphosphonic acid.

[0037] (5) Cool down naturally to 30-50°C, and dehydrate by centrifugation.

[0038] (6) Add solid hydroxyethylene diphosphonic acid to the reaction kettle, add high-purity water, and repeat steps (2)~(5) 3 times.

[0039] (7) Detection of the content of each element Nickel: not detected; iron: 0.0175ppm; copper: 0.0104ppm; lead: not detected; arsenic: 0.0572ppm;

Embodiment 3

[0041] A preparation method of low-iron, low-chlorine hydroxyethylene diphosphonic acid is implemented through the following specific processes:

[0042] (1) Clean the equipment with high-purity water.

[0043] (2) Add 60% hydroxyethylidene diphosphonic acid solution into the reaction kettle, steam at 110±5°C and pressure -0.07MPa.

[0044] (3) When the concentration is 78~80%, stop external steaming, and put the material into the crystallization kettle.

[0045] (4) Stir slowly at 60r / min, and slowly lower the temperature at 3~5°C / h. When the temperature is ≤60°C, add seed crystal hydroxyethylene diphosphonic acid.

[0046] (5) Cool down naturally to 30-50°C, and dehydrate by centrifugation.

[0047] (6) Add solid hydroxyethylene diphosphonic acid to the reaction kettle, add high-purity water, and repeat steps (2)~(5) 4 times.

[0048] (7) Detect the content of each element: nickel: 0.0084ppm; iron: 0.0264ppm; copper: not detected; lead: not detected; arsenic: 0.0335ppm;

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PUM

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Abstract

The invention provides a preparation method of low iron and low chloride hydroxyethylidene-1,1-diphosphonic acid (HEDP) to meet the requirements of the special industries such as electronics and the like on iron ions, chloride ions and the like in HEDP products. The preparation method is specially characterized by recrystallizing common HEDP solution to obtain the special low iron and low chloride HEDP product. The preparation method has the prominent benefits that by repeatedly recrystallizing common HEDP to remove the iron and chloride ions, the special requirements of the industries such as electronics and the like are met and the application field of HEDP is expanded.

Description

technical field [0001] The invention belongs to the field of chemical products and provides a method for preparing low-iron and low-chlorine hydroxyethylene diphosphonic acid. Background technique [0002] Hydroxyethylene diphosphonic acid is a commonly used chemical in the water treatment industry, and its consumption accounts for 20% of the total water treatment chemicals. Accounting for about 4 billion US dollars, it accounts for about 5% of the high-end water treatment agent market. At present, in the domestic market, there is only about 1.4 billion yuan in water treatment. In addition, hydroxyethylene diphosphonic acid is used in petroleum, paper, It is widely used in printing and dyeing, medicine, electronics industry cleaning, civil washing, agriculture and so on. Adding 0.01~5% of hydroxyethylene diphosphonic acid or its salt to soap can increase the stability of soap; adding it to toothpaste can effectively prevent the formation of dental calculus; in medicine,...

Claims

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Application Information

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IPC IPC(8): C07F9/38
Inventor 王燕平程终发齐晓婧万振涛刘全华张秀华
Owner SHANDONG TAIHE WATER TREATMENT TECH CO LTD
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