Preparation method of preferential water permeable membrane and morpholine wastewater treatment and morpholine substance recovery method

A technology that prioritizes water permeation and morpholine, and is used in infiltration/dialysis water/sewage treatment, water/sewage treatment, extraction water/sewage treatment, etc. large problems, to achieve the effects of high comprehensive economic benefits, high energy integration, and small footprint

Active Publication Date: 2021-03-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] patent CN101516830A discloses a method for continuous rectification separation of morpholine, monoaminodiglycol, ammonia and water mixture, the method uses six rectification towers Continuous separation, the disadvantage of this method is that the process is complicated and the energy consumption of separation is high.
[0005] Patent US2776972 discloses a method of reclaiming morpholine from aqueous solution, the method uses the aqueous solution of concentrated alkali metal hydroxide to extract morpholine, the deficiency of this method The disadvantage is that the use of concentrated alkali is large, the regeneration of alkali solution is difficult, and the alkali causes serious corrosion to the equipment, etc.
The disadvantage of the method involved is that the amount of extractant is large and the energy consumption in the separation process is high
[0007] Patent CN102674621 discloses a biological method for treating high-concentration morpholine wastewater, which uses microorganisms to sequentially pass through processes such as anaerobic, nitrification, aerobic and chemical oxidation , to decompose morpholine in wastewater. The disadvantage of this method is that microorganisms have strict requirements on wastewater components, and it is not easy to integrate with existing processes, etc.
[0009]1. The use of multi-tower continuous distillation to treat morpholine wastewater has problems such as complicated process and high energy consumption for separation
[0010]2. In the process of using extractive distillation to treat a large amount of morpholine-containing wastewater, there are problems such as large amount of extractant, high separation cost, poor environmental friendliness, and large footprint
[0011]3. The comprehensive economic benefit is not high when the existing technology is dealing with a large amount of morpholine-containing wastewater

Method used

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  • Preparation method of preferential water permeable membrane and morpholine wastewater treatment and morpholine substance recovery method

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Experimental program
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Effect test

Embodiment 1

[0043] The preparation method of the preferential water-permeable membrane is as follows:

[0044] Preparation of polymer coating solution: where N,N-dimethylformamide is used as a solvent. Mix 8% methyl methacrylate, 3% sodium diamino-p-benzenesulfonate, 2% hydroxylated graphene oxide and N,N-dimethylformamide, which account for the total amount of the polymer coating solution, and use The mechanical stirring was carried out at 70° C. to disperse evenly, the stirring speed was 2000 r / min, and the stirring time was 18 hours to obtain a polymer coating liquid. The polymer coating liquid was coated on the polysulfone membrane twice by spraying, and the coating thickness was 3 μm. Place the coated film in a constant-temperature vacuum oven and dry it at 80°C for 48 hours to obtain a preferentially water-permeable film.

[0045] The content of morpholines in the process wastewater is 15wt%, and the COD is 300000mg / L, which is recovered by the following process, such as figure 1...

Embodiment 2

[0050] The preparation method of the preferential water-permeable membrane is as follows:

[0051] Mix 6% of methyl acrylate, 2% of sodium p-aminobenzenesulfonate, 2% of hydroxylated graphene oxide, and solvent acetone in the total amount of the polymer coating solution, and disperse evenly at 60°C using mechanical stirring. The rotational speed was 1000 r / min, and the stirring time was 24 hours to obtain a polymer coating liquid. The polymer coating liquid was coated on the polyacrylonitrile film four times by scraping, and the coating thickness was 8 μm. Place the coated film in a constant-temperature vacuum oven and dry it at 80°C for 48 hours to obtain a preferentially water-permeable film.

[0052] The content of morpholines in the process wastewater is 25wt%, and the COD is 500000mg / L. The morpholines are reclaimed by the following process, as figure 1 Shown:

[0053] (1) The morpholine wastewater is subjected to atmospheric distillation to remove light components, th...

Embodiment 3

[0057] The preparation method of the preferential water-permeable membrane is as follows: the total amount of polymer coating liquid 8% ethyl methacrylate, 4% sodium lignosulfonate sodium sulfonate, 3% hydroxylated graphene oxide and ethanol are mixed, use Ultrasound was dispersed evenly at 80°C to obtain a polymer coating solution, which was sprayed onto the polyacrylonitrile film three times with a coating thickness of 5 μm, and the coated film Place it in a constant-temperature vacuum oven, keep the temperature at 100°C and dry for 72 hours to obtain a preferential water-permeable membrane.

[0058] The content of morpholines in the process wastewater is 5wt%, and the COD is 50000mg / L. The morpholines are reclaimed by the following process, as figure 1 Shown:

[0059] (1) The morpholine wastewater is subjected to atmospheric distillation to remove light components, the operating pressure is atmospheric pressure, the temperature at the bottom of the tower is 115°C, the temp...

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Abstract

The invention provides a morpholine wastewater treatment and morpholine substance recovery method. The wastewater can come from a morpholine production process or a morpholine byproduct process. The method mainly comprises the steps of (1) rectifying morpholine wastewater under normal pressure to remove light components, cooling a heavy component I at the bottom of a tower, feeding the cooled heavy component I into a reduced pressure rectifying tower for rectification, extracting wastewater with extremely low COD content from the top of the tower, and extracting a heavy component II rich in morpholine substances from the bottom of the tower; (2) feeding the heavy component II into a membrane assembly provided with a preferential water permeable membrane for separation, and obtaining a morpholine substance-containing heavy component III of which the water content is lower than 0.5% on the interception side; (3) feeding the heavy component III into a morpholine refining tower for rectification, and extracting high-purity and low-chroma morpholine substances from the top of the tower. The method provided by the invention is simple in process flow, does not involve common solvents required by extraction or azeotropic distillation, and is low in energy consumption and environment-friendly, and morpholine obtained by separation is high in purity and low in chromaticity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry separation, and in particular relates to a method for treating morpholine wastewater and recovering morpholine substances. Background technique [0002] With the rapid development of my country's fine chemical industry, morpholine, as an important intermediate in fine chemical industry, is widely used in rubber additives, medicine, pesticides, coatings, anti-corrosion and other fields. At present, there are many morpholine production processes and morpholine by-product processes. The characteristics of this process are that it will produce a large amount of waste water with high COD, high ammonia nitrogen and rich morpholine. The morpholine substances in the waste water are miscible with water and can form Homogeneous azeotrope, resulting in wastewater can not be directly distilled to separate morpholine, thus increasing the difficulty of the treatment of this type of wastewater. Theref...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C07D295/03C07D295/023C02F101/32C02F103/36
CPCC02F9/00C07D295/03C07D295/023C02F1/048C02F2301/08C02F2209/08C02F2101/32C02F1/44C02F2103/36C02F1/26
Inventor 李昱学吴健张聪颖刘宝现王宁宁李海龙尚永华
Owner WANHUA CHEM GRP CO LTD
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