Method and equipment for efficiently synthesizing adipate crystal from ammonium adipate formation waste liquid

A technology of ammonium adipate and adipic acid, which is applied in the field of high-efficiency synthesis of adipic acid crystals, can solve problems such as waste of resources and increased cost of sewage treatment, and achieve energy saving, significant economic and environmental benefits, and balanced growth Effect

Active Publication Date: 2014-02-19
ZHONGKAI UNIV OF AGRI & ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of ammonium adipate is also discharged into the sewage station along with impurities, which not only brings about a substantial increase in sewage treatment costs, but also causes a lot of waste of resources

Method used

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  • Method and equipment for efficiently synthesizing adipate crystal from ammonium adipate formation waste liquid
  • Method and equipment for efficiently synthesizing adipate crystal from ammonium adipate formation waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The pulse microwave assisted reaction crystallizer used in the present invention, its cross-sectional view is as follows figure 1 Shown; the pulse microwave-assisted reaction crystallizer by a cylindrical vessel with a top cover 8, ammonium adipate into a waste liquid feed guide tube 2, adipic acid crystal solid-liquid mixture discharge tube 7, adipic acid The seed crystal introduction port 4, the strong acid introduction port 5, the stirring blade 3 and the pulsed microwave generator 6 are composed; the cylindrical container 8 with a top cover is surrounded by a heat exchange jacket 1; The top cover of the cylindrical container 8 is provided with a feed guide tube 2, adipic acid seed crystal introduction port 4 and a strong acid introduction port 5 for ammonium adipate conversion into waste liquid, all of which extend into the cylindrical container 8 with a top cover Inside; the bottom of the cylindrical container 8 with a top cover is provided with a discharging pipe 7...

Embodiment 2

[0031] Using the pulse microwave-assisted reaction crystallizer described in Example 1 to efficiently synthesize adipic acid crystals from the waste liquid of ammonium adipate:

[0032] (1) Take 800 mL of ammonium adipate with a conductivity of 40ms / cm to convert into waste liquid, filter to remove solid impurities in the waste liquid from ammonium adipate, to obtain an ammonium adipate solution; convert the ammonium adipate solution from adipic acid The ammonium formation waste liquid feed guide tube is introduced into the cylindrical container with a top cover of the pulse microwave assisted reaction crystallizer;

[0033] (2) Cool the ammonium adipate solution to 5°C to obtain a low-temperature ammonium adipate solution;

[0034] (3) Under the condition of stirring at 100rpm, add 95% sulfuric acid to the low-temperature ammonium adipate solution; when the pH value of the ammonium adipate solution drops to about 4.0, the particle size is added 1-10 micron adipic acid seed crystals...

Embodiment 3

[0043] (1) Take 800 mL of ammonium adipate with a conductivity of 40ms / cm to be converted into waste liquid, and filter to remove solid impurities in the waste liquid from the conversion of ammonium adipate to obtain an ammonium adipate solution;

[0044] (2) Cool the ammonium adipate solution to 5°C to obtain a low-temperature ammonium adipate solution;

[0045] (3) Under the condition of stirring at 100 rpm, add dropwise sulfuric acid with a mass concentration of 95% to the low-temperature ammonium adipate solution;

[0046] (4) When the pH value of the solution reaches 0.9, stop adding sulfuric acid with a mass concentration of 95%, the stirring speed is reduced to 20 rpm, and the temperature is kept at 5°C for 2 hours;

[0047] (6) Centrifugal separation of adipic acid crystals, washing with ice water, and vacuum drying at 60°C to obtain adipic acid crystal sample B.

[0048] The particle size, moisture and impurities of the adipic acid crystal sample B were tested, and the results ...

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Abstract

The invention belongs to the field of adipate preparation and discloses a method and equipment for efficiently synthesizing an adipate crystal from ammonium adipate formation waste liquid. The method comprises the steps: filtering to remove solid impurities in the ammonium adipate formation waste liquid; cooling to 0-10 DEG C; dropwise adding strong acid into a low-temperature ammonium adipate solution under stirring; adding an adipate crystal seed with the particle size of 1-10mm when the pH value of the ammonium adipate solution is reduced to 3.0-4.5; starting a pulse microwave generator with the frequency of 30-40MHz and the energy concentration of 0.01-0.1w / cm<2>, and meanwhile, further dropwise adding the strong acid; when the pH value of the solution is up to 0.9-1.2, ending the dropwise adding of the strong acid, reducing the stirring speed, stopping the pulse microwave generator after 15-30min, and preserving the heat for 1-2h; and carrying out suction filtration, washing and drying in vacuum. The method has the advantages of high product yield, relatively uniform crystal shape, size and density, fewer impurities, simple process and relatively remarkable economic and environment-friendly benefits.

Description

Technical field [0001] The invention belongs to the field of preparation of adipic acid, and particularly relates to a method and equipment for efficiently synthesizing adipic acid crystals from ammonium adipic acid into waste liquid. Background technique [0002] Electrolyte must be used in the formation of low-voltage aluminum foil for capacitors, and the main electrolyte component currently used is ammonium adipate. After the formed electrolyte is used for a period of time, due to the inclusion of more aluminum ions, colloids and some metal ion impurities, the electrical performance of the formed foil produced gradually fails to meet the requirements, which requires a new ammonium adipate bath To maintain normal production. However, if used electrolyte waste is discharged randomly into the environment and water bodies, it will cause serious environmental pollution and waste of resources. In addition, ammonium adipate uses adipic acid, an important chemical raw material, as t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/14C07C51/02C07C51/43B01D9/02B01J19/12
CPCB01D9/00B01D2009/0086B01J19/126C07C51/02C07C51/43C07C55/14
Inventor 龚圣谭帼英
Owner ZHONGKAI UNIV OF AGRI & ENG
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