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Decolorizing method of iminodiacetonitrile

A technology of iminodiacetonitrile and ceramic membrane, which is applied in the field of decolorization of iminodiacetonitrile, can solve the problems of increasing production process and cost, and achieve the effects of improving competitiveness, stable operation and high recovery rate

Active Publication Date: 2014-05-14
SANDA FILM SCI & TECH XIAMEN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, the subsequent production process and cost are increased

Method used

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  • Decolorizing method of iminodiacetonitrile
  • Decolorizing method of iminodiacetonitrile
  • Decolorizing method of iminodiacetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Experimental feed liquid: use tan iminodiacetonitrile crystals to dissolve, the solution is a tan liquid, the product content is 30%, and contains 10-15% solid suspended matter.

[0037] Experimental membrane core: ceramic membrane Suntar-Y, roll nanofiltration membrane S371, S372, S3B02.

[0038] Cleaning agent: NaOH, NaClO, Suntar-90#.

[0039] After the reaction liquid is pretreated by the ceramic membrane, it enters the roll-type nanofiltration membrane for impurity removal and decolorization. The roll-type nanofiltration membrane dialysate is divided into two parts, and the dialysate before adding water is directly crystallized into the final product; the product after adding water is due to color comparison Deep, in order to ensure the quality of the product, the second nanofiltration treatment is carried out, and the dialysate is directly crystallized. In order to improve the product yield, the concentrated solution is used as water for the ceramic membrane. Thi...

Embodiment 2

[0044] Poor quality iminodiacetonitrile crystals contain about 10-15% solid suspended solids that cannot be dissolved after being dissolved, so that the solution cannot be directly fed into the roll-type membrane core, and pretreatment must be added before entering the roll-type membrane core. To make the feed liquid meet the requirements of roll-in membranes, ceramic membranes are selected for pretreatment. Results Using ceramic membrane + roll nanofiltration process for decolorization can achieve the predetermined decolorization goal. However, the decolorization effect becomes deeper with the increase of the concentration multiple, so the second nanofiltration decolorization of the nanofiltration dialysate after the high concentration multiple is used, the effect is very obvious, see image 3 .

[0045] instruction manual: image 3 , the left is the dialysate after the first nanofiltration concentration, and the right is the second nanofiltration dialysate.

Embodiment 3

[0046] Example 3 Stability

[0047] Stability experiments were carried out according to the process route obtained in the above examples.

[0048] Ceramic membrane pretreatment + nanofiltration membrane experiment

[0049] Dissolve the feed liquid first, pass through the sieve (some of the supernatant is poured directly into the ceramic tank), pass through the ceramic membrane, and the filtrate that comes out passes through the nanofiltration membrane. The operating conditions of the ceramic membrane: inlet pressure 2.0bar, outlet pressure 1.3bar, temperature 59°C, the experimental data obtained are shown in Table 2 and the change of membrane flux is shown in Figure 4 .

[0050] Table 2: Ceramic membrane pretreatment data

[0051]

Concentration factor

Water multiple

Filtrate Appearance

Mean Membrane Flux (LMH)

Yield (%)

Ceramic Membrane 1

No obvious SS

161.56

[0052] Depend on Figure 4 It can be see...

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Abstract

The invention discloses a decolorizing method of iminodiacetonitrile. The decolorizing method comprises the following steps: (1) filtering a reaction liquid through a metal sieve; (2) preprocessing through a ceramic membrane; and (3) transferring the filtrate preprocessed by the ceramic membrane to a coiled nanofiltration membrane to purify and decolorize, dividing the dialyzate of the coiled nanofiltration membrane into two parts, directly crystallizing the dialyzate without water added to obtain the finished product, and processing the water-added product by secondary nanofiltration, and directly crystallizing the dialyzate to obtain the concentrated solution, wherein the concentrated solution is used as the water added to the ceramic membrane in the step (1). According to the decolorizing method of iminodiacetonitrile, the membrane filtration technology is carried out for removing impurities from iminodiacetonitrile solution so as to obtain white or faint yellow crystals, and thus the competitiveness of iminodiacetonitrile is improved; and the decolorizing method has the advantages that the yield is high, the process system runs steadily, and stable membrane flux is remained.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a decolorization method of iminodiacetonitrile. Background technique [0002] Iminodiacetonitrile has a melting point of 75-78°C, is soluble in water (solubility 6-7g, 25°C), and is easily soluble in organic solvents such as acetone. It is mainly used to synthesize the herbicide glyphosate. In addition, as an important fine chemical intermediate, it is widely used in the fields of dyes, electroplating, water treatment, and synthetic resins. The iminodiacetonitrile produced by the traditional process generally contains impurities (about 5% hydroxyacetonitrile). Due to the influence of impurities, these impurities are easy to polymerize under the adjustment of alkaline or weak acidity, forming a brown polymer, which affects the appearance quality of the product. It also affects subsequent use. [0003] The iminodiacetonitrile produced by the traditional method needs to be decolor...

Claims

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Application Information

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IPC IPC(8): C07C255/61C07C253/34
Inventor 王贝辉李硕林林雄水苏义鹏林丽华方富林蓝伟光
Owner SANDA FILM SCI & TECH XIAMEN