CN113773511A - Method for recycling electrostatic acid - Google Patents

Method for recycling electrostatic acid Download PDF

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Publication number
CN113773511A
CN113773511A CN202110838865.5A CN202110838865A CN113773511A CN 113773511 A CN113773511 A CN 113773511A CN 202110838865 A CN202110838865 A CN 202110838865A CN 113773511 A CN113773511 A CN 113773511A
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CN
China
Prior art keywords
acid
electrostatic
neutralization
electrostatic acid
ammonium salt
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Pending
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CN202110838865.5A
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Chinese (zh)
Inventor
刘锐
杨剑
胡显智
郑继海
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Anhui Jintong Fine Chemical Co ltd
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Anhui Jintong Fine Chemical Co ltd
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Priority to CN202110838865.5A priority Critical patent/CN113773511A/en
Publication of CN113773511A publication Critical patent/CN113773511A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

The invention discloses a method for recycling electrostatic acid, and relates to the technical field of electrostatic acid treatment. According to the method for the regeneration and recycling treatment of the electrostatic acid, caustic soda and deionized water are added into a stainless steel neutralization kettle, the mixture is uniformly stirred to reach a proper concentration, and then the electrostatic acid is slowly added for neutralization; and adding the neutralized mixed solution into a cationic ammonium salt preparation tank, performing ion neutralization, uniformly stirring, and standing to form a copolymer of fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid, fatty acid methyl ester sulfonic acid and cationic ammonium salt, so that the original black solution with strong corrosivity is converted into two substances with clear boundaries, namely a clear water body at the upper layer and a black macromolecular precipitate at the lower layer, the treated wastewater reaches the discharge standard, and the problems of high treatment cost of the electrostatic acid and the like in the prior art are solved.

Description

Method for recycling electrostatic acid
Technical Field
The invention relates to the technical field of electrostatic acid treatment, in particular to a method for electrostatic acid regeneration and recycling treatment.
Background
The anionic surfactant is a main surfactant type in China, main products comprise alkyl benzene sulfonate, fatty alcohol sulfate, fatty alcohol ether sulfate, fatty acid methyl ester sulfonate and the like, and a typical production process comprises sulfonation and sulfation of sulfur trioxide. At present, the core equipment of sulfonation and sulfation is a falling film sulfonation reactor, and a tail gas treatment device, namely an electrostatic demister, of the sulfonation and sulfation reactor recovers a mixture of sulfur trioxide and a liquid material in the production process, namely electrostatic acid, and the main components of the electrostatic acid comprise: the raw material, the sulfonated product, the super-sulfonated substance and the sulfuric acid are produced, so that the mixture is dark brown or black, contains a certain amount of sulfuric acid and cannot be sold as a conventional product, and a factory usually stores the sulfuric acid as waste in a centralized way and then entrusts a dangerous waste treatment mechanism to treat the sulfuric acid. The presence of electrostatic acids not only increases the storage capacity of hazardous wastes, but also carries a significant risk of environmental pollution. Thus, electrostatic acids have become a major problem affecting the normal production of sulfonation/sulfation plants.
Through search, in order to solve the above problems, there are related patents, such as chinese patent, with application numbers: 91101234.6, application date is: 23 days 2 and 23 days of 1991, and the date of authorized bulletin: 2013, 6 and 5, disclose a treatment method of electrostatic acid, which mainly recovers sodium alkyl benzene sulfonate in the sodium alkyl benzene sulfonate through the working procedures of neutralization, salting out, bleaching and the like, although part of surfactant can be recovered by the method, the recovery purpose of the electrostatic acid in the production process of fatty alcohol sulfonate, fatty alcohol ether sulfonate and fatty acid methyl ester sulfonate cannot be realized, high-concentration salt-containing wastewater is generated, the discharge standard cannot be reached, and various dangerous chemicals such as sodium hypochlorite, potassium permanganate and the like are used in the process, so that the finished product is high.
As another example, the chinese patent has an application number: 201210206624.X, application date is: day 16, 6 month 2012, and the date of authorized bulletin: 2013, 6 and 5 days, a comprehensive utilization method of main bath type continuous sulfonation waste acid is disclosed, the waste acid generated when the formula alkylbenzene is sulfonated by fuming sulfuric acid is disclosed, the prior fuming sulfuric acid sulfonation process belongs to a rejected process due to low sulfonation rate and large waste acid generation amount, and an advanced sulfur trioxide film type sulfonation technology is generally adopted in the industry at present, so that the sulfonation yield is high, the product color is light, the generated electrostatic acid is small, meanwhile, the components of the electrostatic acid are different from those of the electrostatic acid generated by the fuming method, the active ingredient content is high, and the sulfuric acid content is low.
Disclosure of Invention
1. Technical problem to be solved by the invention
The invention provides a method for recycling electrostatic acid, aiming at the problems of high treatment cost of the electrostatic acid in the prior art, which comprises the steps of adding caustic soda and deionized water into a stainless steel neutralization kettle, slowly adding the electrostatic acid for neutralization, adding a neutralized mixed solution into a cationic ammonium salt preparation tank, carrying out ion neutralization, uniformly stirring, and standing to form fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and a copolymer of fatty acid methyl ester sulfonic acid and cationic ammonium salt, thereby realizing the recovery of the electrostatic acid.
2. Technical scheme
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a method for electrostatic acid regeneration and resource treatment comprises the following steps:
firstly, adding caustic soda and deionized water into a stainless steel neutralization kettle, and uniformly stirring to a proper concentration;
step two, slowly adding electrostatic acid for neutralization;
step three, adding the neutralized mixed solution into a cationic ammonium salt preparation tank for ion neutralization;
and step four, uniformly stirring the mixed liquid, and standing for more than 1 hour to realize the recovery of the electrostatic acid.
In the second step, 10-30% caustic soda and 40-60% electrostatic acid are neutralized, active ingredients such as fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and fatty acid methyl ester sulfonic acid are neutralized into an anionic surfactant, and sulfuric acid is neutralized into inorganic salt and is dissociated in the mixed solution.
According to a further technical scheme, the neutralization mass ratio of the electrostatic acid to the caustic soda is 1: 1.0-2.0.
According to the further technical scheme, in the third step, the concentration of the cationic ammonium salt is 10% -20% to form a copolymer of fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and fatty acid methyl ester sulfonic acid with the cationic ammonium salt, so that an original black solution with strong corrosivity is converted into two types of substances with clear boundaries, wherein the upper layer is a clear water body, and the lower layer is a black macromolecular precipitate, so that the treated wastewater reaches the discharge standard.
According to a further technical scheme, an electronic neutralization method is utilized, and the treatment mass ratio of the cationic ammonium salt is 1: 1.0-2.0.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
(1) according to the method for recycling the electrostatic acid, after caustic soda and deionized water are added into a stainless steel neutralization kettle, the electrostatic acid is slowly added for neutralization, the neutralized mixed solution is added into a cationic ammonium salt preparation tank for ion neutralization, and the mixed solution is stirred uniformly and then stands to form fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and a copolymer of fatty acid methyl ester sulfonic acid and cationic ammonium salt, so that the electrostatic acid is recovered;
(2) according to the method for recycling the electrostatic acid, the adopted caustic alkali is used for neutralization, the caustic sodium (10-30%) and the electrostatic acid (40-60%) are neutralized, active ingredients such as fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and fatty acid methyl ester sulfonic acid are neutralized into an anionic surfactant, sulfuric acid is neutralized into inorganic salt, and the inorganic salt is dissociated in a mixed solution;
(3) according to the method for electrostatic acid regeneration recycling treatment, cationic ammonium salt (10% -20%) is added into a formula for ion neutralization, fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and a copolymer of fatty acid methyl ester sulfonic acid and cationic ammonium salt can be formed, so that an original black solution with strong corrosivity is converted into two types of substances with clear upper layers and black macromolecular precipitates at lower layers, and the treated wastewater reaches the discharge standard.
Detailed Description
For a further understanding of the present invention, the following detailed description is provided.
Example 1
The method for the regeneration and resource treatment of the electrostatic acid comprises the following steps:
firstly, adding caustic soda and deionized water into a stainless steel neutralization kettle, and uniformly stirring to a proper concentration;
step two, slowly adding electrostatic acid for neutralization;
step three, adding the neutralized mixed solution into a cationic ammonium salt preparation tank for ion neutralization;
and step four, uniformly stirring the mixed liquid, and standing for more than 1 hour.
In the embodiment, 10-30% caustic soda and 40-60% electrostatic acid are adopted for neutralization, wherein active ingredients such as fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and fatty acid methyl ester sulfonic acid are neutralized into an anionic surfactant, and sulfuric acid is neutralized into inorganic salt and is dissociated in the mixed solution. The neutralization mass ratio of the electrostatic acid to the caustic soda is 1: 1.0-2.0.
In the third step, the concentration of the cationic ammonium salt is 10-20% to form a copolymer of fatty alcohol sulfonic acid, fatty alcohol ether sulfonic acid and fatty acid methyl ester sulfonic acid with the cationic ammonium salt, so that the black solution which originally has strong corrosivity is converted into two types of substances with clear limits, namely a clear water body at the upper layer and a black macromolecular precipitate at the lower layer, and the treated wastewater reaches the discharge standard. By using an electron neutralization method, the treatment mass ratio of the cationic ammonium salt is 1: 1.0-2.0.
The present invention and its embodiments have been described above schematically, without limitation to the description, and the actual structure is not limited to this. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.

Claims (5)

1. The method for the regeneration and resource treatment of the electrostatic acid is characterized by comprising the following steps:
firstly, adding caustic soda and deionized water into a stainless steel neutralization kettle, and uniformly stirring to a proper concentration;
step two, slowly adding electrostatic acid for neutralization;
step three, adding the neutralized mixed solution into a cationic ammonium salt preparation tank for ion neutralization;
and step four, uniformly stirring the mixed liquid, and standing for more than 1 hour.
2. The method for recycling electrostatic acid as claimed in claim 1, wherein in the second step, 10-30% caustic soda and 40-60% electrostatic acid are neutralized.
3. The method for electrostatic acid regeneration and resource treatment according to claim 2, characterized in that: the neutralization mass ratio of the electrostatic acid to the caustic soda is 1: 1.0-2.0.
4. The method for electrostatic acid regeneration and resource treatment according to claim 2, characterized in that: in the third step, the concentration of cationic ammonium salt is 10-20%.
5. The method for electrostatic acid regeneration and resource treatment according to claim 4, wherein: by using an electron neutralization method, the treatment mass ratio of the cationic ammonium salt is 1: 1.0-2.0.
CN202110838865.5A 2021-07-23 2021-07-23 Method for recycling electrostatic acid Pending CN113773511A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114573136A (en) * 2022-01-18 2022-06-03 天津天智精细化工有限公司 Electrostatic demisting and washing method for fatty alcohol ether sulfonated tail gas

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Publication number Priority date Publication date Assignee Title
GB494616A (en) * 1936-09-23 1938-10-28 Ig Farbenindustrie Ag Improvements in the manufacture and production of sulphonation products
CN102070274A (en) * 2009-11-19 2011-05-25 陈丰 Method and device for treating sulfonated wastewater by using calcium salt precipitation method
CN102994173A (en) * 2012-12-08 2013-03-27 青岛科技大学 Method for preparing biodiesel and co-producing triacetin
CN103548824A (en) * 2013-11-11 2014-02-05 浙江赞宇科技股份有限公司 Method for preparing pesticide adjuvant by using electrostatic defogging liquid for producing AES (Alcohol Ether Sulfate)
CN104451714A (en) * 2014-12-05 2015-03-25 浙江赞宇科技股份有限公司 Production process and production device for preparing industrial additives from electrostatic acid and application thereof
CN106000265A (en) * 2016-07-06 2016-10-12 凯瑞环保科技股份有限公司 Process device and method for producing cation exchange resin through sulfonation of sulfur trioxide
CN106854167A (en) * 2015-12-08 2017-06-16 中国石油天然气股份有限公司 Method for producing petroleum sulfonate
CN109750301A (en) * 2017-11-06 2019-05-14 南风化工集团股份有限公司 A method of metal cleaner is produced using sulfonation black sulfonic acid
CN114573136A (en) * 2022-01-18 2022-06-03 天津天智精细化工有限公司 Electrostatic demisting and washing method for fatty alcohol ether sulfonated tail gas

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Publication number Priority date Publication date Assignee Title
GB494616A (en) * 1936-09-23 1938-10-28 Ig Farbenindustrie Ag Improvements in the manufacture and production of sulphonation products
CN102070274A (en) * 2009-11-19 2011-05-25 陈丰 Method and device for treating sulfonated wastewater by using calcium salt precipitation method
CN102994173A (en) * 2012-12-08 2013-03-27 青岛科技大学 Method for preparing biodiesel and co-producing triacetin
CN103548824A (en) * 2013-11-11 2014-02-05 浙江赞宇科技股份有限公司 Method for preparing pesticide adjuvant by using electrostatic defogging liquid for producing AES (Alcohol Ether Sulfate)
CN104451714A (en) * 2014-12-05 2015-03-25 浙江赞宇科技股份有限公司 Production process and production device for preparing industrial additives from electrostatic acid and application thereof
CN106854167A (en) * 2015-12-08 2017-06-16 中国石油天然气股份有限公司 Method for producing petroleum sulfonate
CN106000265A (en) * 2016-07-06 2016-10-12 凯瑞环保科技股份有限公司 Process device and method for producing cation exchange resin through sulfonation of sulfur trioxide
CN109750301A (en) * 2017-11-06 2019-05-14 南风化工集团股份有限公司 A method of metal cleaner is produced using sulfonation black sulfonic acid
CN114573136A (en) * 2022-01-18 2022-06-03 天津天智精细化工有限公司 Electrostatic demisting and washing method for fatty alcohol ether sulfonated tail gas

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Publication number Priority date Publication date Assignee Title
CN114573136A (en) * 2022-01-18 2022-06-03 天津天智精细化工有限公司 Electrostatic demisting and washing method for fatty alcohol ether sulfonated tail gas

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Application publication date: 20211210