CN109053374B - Ammonia removal process for ammonia-containing ethanol in aerogel production - Google Patents

Ammonia removal process for ammonia-containing ethanol in aerogel production Download PDF

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Publication number
CN109053374B
CN109053374B CN201810637880.1A CN201810637880A CN109053374B CN 109053374 B CN109053374 B CN 109053374B CN 201810637880 A CN201810637880 A CN 201810637880A CN 109053374 B CN109053374 B CN 109053374B
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Prior art keywords
ammonia
ethanol
containing ethanol
aerogel
filter
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CN109053374A (en
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陈勇
段国栋
陈世忠
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Xiangshui Huaxia Special Material Technology Development Co ltd
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Xiangshui Huaxia Special Material Technology Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/88Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention discloses an ammonia removal process for ammonia-containing ethanol in aerogel production, which sequentially comprises the following steps: (1) neutralizing: pumping ammonia-containing ethanol to a neutralization tank, adding sulfuric acid under the condition of stirring, and adjusting the pH value; (2) and (3) filtering: separating solid and liquid of the ethanol neutralized and adjusted in the step (1) through an industrial filter; (3) distillation and condensation: and (3) evaporating and condensing the filtrate obtained in the step (2) through an evaporator, and recovering to obtain ethanol meeting the conditions.

Description

Ammonia removal process for ammonia-containing ethanol in aerogel production
Technical Field
The invention relates to an ethanol impurity removal treatment process, in particular to an ammonia removal process for ammonia-containing ethanol in aerogel production.
Background
Aerogel composite materials and products thereof are novel revolutionary heat-insulating materials which are developed rapidly in recent years due to extremely low heat conductivity, wide temperature adaptability, excellent fireproof flame retardance and the like, a large amount of ethanol is used as a solvent in the production process of aerogel materials, the storage and transportation of the large amount of ethanol are caused due to the use of the large amount of ethanol, the safety risk is increased, the production cost of the aerogel materials is increased, and the ethanol is recycled, so that the aerogel composite materials and the products thereof become necessary choices of enterprises. However, ammonia is also used as a catalyst in the aerogel production process, so that ammonia molecules exist in the final ethanol, and the ammonia has great influence on the sol-gel reaction which is a front-stage process of aerogel production, so that the ethanol cannot be directly and completely recycled, and the product cost is directly increased.
Aiming at the problems, the invention provides an ammonia removal process for ammonia-containing ethanol in aerogel production, so that the ammonia-containing ethanol can be recycled, the ethanol consumption and transportation in the production process of aerogel materials can be reduced, and the aerogel production cost can be reduced.
Disclosure of Invention
In order to achieve the purpose, the invention provides the following technical scheme: an ammonia removal process for ammonia-containing ethanol in aerogel production is characterized by sequentially comprising the following steps:
(1) neutralizing: pumping ammonia-containing ethanol to a neutralization tank, adding sulfuric acid under the condition of stirring, and adjusting the pH value;
(2) and (3) filtering: separating solid and liquid of the ethanol neutralized and adjusted in the step (1) through an industrial filter;
(3) distillation and condensation: and (3) evaporating and condensing the filtrate obtained in the step (2) through an evaporator, and recovering to obtain qualified ethanol.
Further, preferably, in the step (1), the concentration of the sulfuric acid for neutralization is 50 to 98%, and the pH is adjusted to 5.0 to 6.0.
Further, preferably, the filtration mode in the step (2) is suction filtration or pressure filtration, wherein the vacuum degree is-0.06 to-0.04 MPa.
Preferably, in the step (3), the ethanol concentration obtained by condensation is 85-95% by adopting reduced pressure distillation as an evaporation mode.
Further, preferably, the filter membrane used for vacuum filtration or pressure filtration is a PP melt-blown non-woven fabric and PA filter cloth composite layer.
Compared with the prior art, the invention has the beneficial effects that:
the method realizes the recycling of the ammonia-containing ethanol by using a neutralization distillation method on the premise of not introducing other impurities, reduces the ethanol consumption and transportation in the production process of the aerogel material, and reduces the production cost of the aerogel.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An ammonia removal process for ammonia-containing ethanol in aerogel production is characterized by sequentially comprising the following steps:
(1) neutralizing: pumping ammonia-containing ethanol to a neutralization tank, adding 50% sulfuric acid under stirring, adjusting pH to 5.5, and continuing stirring for 10 min;
(2) and (3) filtering: and (3) carrying out solid-liquid separation on the ethanol neutralized and adjusted in the step (1) through an industrial filter press with a filter membrane being a PP melt-blown non-woven fabric and PA filter cloth composite layer.
(3) Distillation and condensation: and (3) evaporating and condensing the filtrate obtained in the step (2) through an alcohol evaporator, and recovering to obtain qualified ethanol.
Example 2
An ammonia removal process for ammonia-containing ethanol in aerogel production is characterized by sequentially comprising the following steps:
(1) neutralizing: pumping ammonia-containing ethanol to a neutralization tank, adding 98% sulfuric acid under stirring, adjusting pH to 5.5, and continuing stirring for 10 min.
(2) And (3) filtering: and (2) performing solid-liquid separation on the ethanol neutralized and adjusted in the step (1) by a filter membrane of a suction filter machine with a PP melt-blown non-woven fabric and PA filter cloth composite layer, wherein the vacuum degree is-0.06 to-0.04 MPa.
(3) Distillation and condensation: and (3) evaporating and condensing the filtrate obtained in the step (2) through an alcohol evaporator, and recovering ethanol meeting the conditions by assisting in vacuum of-0.02 MPa.
The method realizes the recycling of the ammonia-containing ethanol by using a neutralization distillation method on the premise of not introducing other impurities, reduces the ethanol consumption and transportation in the production process of the aerogel material, and reduces the production cost of the aerogel.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (1)

1. An ammonia removal process for ammonia-containing ethanol in aerogel production is characterized by sequentially comprising the following steps:
(1) neutralizing: pumping ammonia-containing ethanol to a neutralization tank, adding sulfuric acid under the condition of stirring, and adjusting the pH value;
(2) and (3) filtering: separating solid and liquid of the ethanol neutralized and adjusted in the step (1) through an industrial filter;
(3) distillation and condensation: evaporating and condensing the filtrate obtained in the step (2) through an evaporator, and recovering to obtain ethanol meeting the conditions;
in the step (1), the concentration of the sulfuric acid for neutralization is 50-98%, and the pH is adjusted to 5.0-6.0;
the filtration mode in the step (2) is suction filtration or filter pressing, wherein the vacuum degree of the suction filtration is-0.06 to-0.04 MPa;
in the step (3), reduced pressure distillation is adopted as an evaporation mode, and the concentration of the ethanol obtained by condensation is 85-95%;
the filter membrane used for vacuum filtration or filter pressing is a PP melt-blown non-woven fabric and PA filter cloth composite layer.
CN201810637880.1A 2018-06-20 2018-06-20 Ammonia removal process for ammonia-containing ethanol in aerogel production Active CN109053374B (en)

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CN109053374B true CN109053374B (en) 2021-09-14

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109851474A (en) * 2019-01-15 2019-06-07 安徽中航名坤新材料科技有限公司 A kind of method of fiber size pigment and ammonium ion in removal alcoholic solution
CN109678665A (en) * 2019-01-15 2019-04-26 安徽中航名坤新材料科技有限公司 A kind of method of ammonium ion in removal alcoholic solution

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101497554A (en) * 2008-01-25 2009-08-05 气体产品与化学公司 Method for removing ammonia from a methanol containing stream
CN102816047A (en) * 2012-08-07 2012-12-12 南通市振兴精细化工有限公司 Technology for removing ammonia in ammoniacal smell ethanol in tetramethylpiperidinol
CN106132874A (en) * 2014-03-21 2016-11-16 赢创罗姆有限公司 From alcoholic solution, the method removing ammonia is separated in the presence of carbonate compound
CN107827760A (en) * 2017-12-08 2018-03-23 烟台国邦化工机械科技有限公司 The device and process of cholamine are reclaimed in a kind of ammonia, water, alcohol mixture

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2241132T3 (en) * 1997-03-31 2005-10-16 Battelle Memorial Institute PROCEDURE FOR THE ELIMINATION OF AMMONIA FROM A FLUID.

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101497554A (en) * 2008-01-25 2009-08-05 气体产品与化学公司 Method for removing ammonia from a methanol containing stream
CN102816047A (en) * 2012-08-07 2012-12-12 南通市振兴精细化工有限公司 Technology for removing ammonia in ammoniacal smell ethanol in tetramethylpiperidinol
CN106132874A (en) * 2014-03-21 2016-11-16 赢创罗姆有限公司 From alcoholic solution, the method removing ammonia is separated in the presence of carbonate compound
CN107827760A (en) * 2017-12-08 2018-03-23 烟台国邦化工机械科技有限公司 The device and process of cholamine are reclaimed in a kind of ammonia, water, alcohol mixture

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