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A method for stripping and recovering pentamethylenediamine from a solid phase containing pentamethylenediamine

A technology of pentamethylenediamine and China Steam, which is applied in organic chemistry, calcium/strontium/barium oxide/hydroxide, calcium/strontium/barium sulfate, etc., which can solve the separation and purification pressure, large water consumption, and recovery rate Low-level problems, to achieve high-efficiency recycling, high recovery rate, and solve the effect of refractory solid waste

Active Publication Date: 2020-10-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the most used method is to wash with water in the process of solid-liquid separation. This method has disadvantages: (1) the water consumption is large, and the recovery rate is low. The experimental results show that it is fully washed 4 times, and the recovery rate is only 90%. (2) Wash the solid phase with water, and a large amount of water-soluble impurities in the solid phase will also be washed down and returned to the washing liquid, causing pressure for subsequent separation and purification

Method used

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  • A method for stripping and recovering pentamethylenediamine from a solid phase containing pentamethylenediamine
  • A method for stripping and recovering pentamethylenediamine from a solid phase containing pentamethylenediamine

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Effect test

Embodiment 1

[0039] According to the process route reported in the patent CN107043331A, a vacuum rake drying device is used to extract pentamethylenediamine, and residual pentamethylenediamine is recovered for the remaining solid residue after extraction. Analysis of the residual solid residue composition shows that the water-insoluble salts in the solid residue are mainly calcium sulfate and calcium carbonate, as well as pigments and miscellaneous proteins, wherein the mass content of pentamethylenediamine is 0.5%, and the pigment content is 32% expressed by T430nm. Take 1kg of this solid residue into the screen of the solid residue stripping tank. The tank body is kept warm to 180°C through heat transfer oil, and steam at 190-200°C is passed into the tank from the bottom. L / h, the top steam condenses the gas phase through the glass condenser tube, and collects the condensate. After the steam was introduced for 40min, 200mL of pentamethylenediamine aqueous solution was obtained, and the m...

Embodiment 2

[0041] According to the chromatographic separation process route of pentamethylenediamine reported in patent CN106861236A, this method can also be used to recover pentamethylenediamine for resins saturated with adsorbed pentamethylenediamine. The composition of the resin after adsorption saturation was tested: the mass fraction of pentamethylenediamine was 80 mg / g wet resin, and the inorganic salt contained 105 mg / g wet resin in terms of ash content. Take 1kg of this wet resin into the screen of the solid slag stripping tank, heat the tank body to 140°C through an electric heating belt, use 160-170°C water vapor to pass into the tank from the bottom, and control the gas phase outlet flow through a valve at the top opening It is 0.6L / h, and the top steam is condensed through the glass condenser tube. After the steam was introduced for 20min, 200mL of pentamethylenediamine aqueous solution was obtained, and the mass concentration of pentamethylenediamine tested by high performan...

Embodiment 3

[0042] Example 3: The production method of the solid phase containing pentamethylenediamine in the process of preparing pentamethylenediamine by biological method

[0043] Take 10L of fermentation broth of lysine sulfate, phosphate, and carbonate respectively, use lysine decarboxylase to catalyze, and then use sodium alkali, potassium alkali, calcium alkali, magnesium alkali, barium alkali or their respective The oxides are adjusted to make the pH greater than 11.0, and after solid-liquid separation, one or more of calcium sulfate, calcium carbonate, calcium phosphate, calcium hydroxide, magnesium carbonate, magnesium hydroxide, and barium sulfate can be obtained. Wet precipitation of inorganic salts. In addition to these insoluble inorganic salts, the precipitation also contains complex components such as some bacterial cells, insoluble proteins, etc., or insoluble substances in the cell fermentation process or the medium used. The wet precipitation also contains pentamethylen...

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Abstract

The invention discloses a method for recovering pentane diamine through steam stripping from a solid phase containing the pentane diamine. The method is characterized in that hot water vapors are usedfor contacting the solid phase containing the pentane diamine, the pentane diamine in the solid phase is extracted through the water vapors, an aqueous solution containing the pentane diamine or thewater vapors containing the pentane diamine are obtained, and then purification is further conducted to obtain the pentane diamine or pentane diamine dicarboxylate; and meanwhile, residual solid slagcan be recycled or highly utilized. The method has the beneficial effects that one-step separation of the pentane diamine from salt, pigment and protein can be realized, the recovery rate is up to 98%, the recovered pentane diamine is high in purity, chromatographic purity can be up to 99.5%, and the recovered pentane diamine can be directly used for subsequent distillation or salting with dicarboxylic acid to prepare a nylon monomer.

Description

technical field [0001] The technology belongs to the field of biochemical industry, and specifically relates to a method for stripping and recovering pentamethylenediamine from a solid phase containing pentamethylenediamine. Background technique [0002] At present, the main varieties of the polyamide market in the world are polyamide 6 and polyamide 66, which are produced by chemical methods using petroleum as raw materials. However, the sustainability and environmental friendliness of raw materials are poor. Hexamethylenediamine, the raw material monomer for the synthesis of polyamide 66, has been monopolized by a few foreign companies for a long time. China is completely dependent on imports. There has been no obvious breakthrough until now, which greatly limits the development of China's polyamide industry. 1,5-Pentanediamine can be produced from biomass through green bio-methods. Pentamethylenediamine and adipic acid can be polymerized to obtain nylon 56, which is consi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/86C07C211/09C07C209/84C01F11/06C01F11/46
CPCC01F11/06C01F11/46C07C209/84C07C209/86C07C211/09
Inventor 应汉杰杨朋朋温庆仕林晨光王森吴菁岚朱晨杰陈勇柳东欧阳平凯
Owner NANJING UNIV OF TECH
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