CN104528910A - Synthetic process of heavy metal chelating agent - Google Patents

Synthetic process of heavy metal chelating agent Download PDF

Info

Publication number
CN104528910A
CN104528910A CN201410790054.2A CN201410790054A CN104528910A CN 104528910 A CN104528910 A CN 104528910A CN 201410790054 A CN201410790054 A CN 201410790054A CN 104528910 A CN104528910 A CN 104528910A
Authority
CN
China
Prior art keywords
heavy metal
metal chelant
organic amine
synthesis technique
intermediate product
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410790054.2A
Other languages
Chinese (zh)
Inventor
张哲�
李纪文
张斌
段会伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZIBO JINDING PHOTOELECTRIC TECHNOLOGY Co Ltd
Original Assignee
ZIBO JINDING PHOTOELECTRIC TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ZIBO JINDING PHOTOELECTRIC TECHNOLOGY Co Ltd filed Critical ZIBO JINDING PHOTOELECTRIC TECHNOLOGY Co Ltd
Priority to CN201410790054.2A priority Critical patent/CN104528910A/en
Publication of CN104528910A publication Critical patent/CN104528910A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C02F1/58Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62Heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of chelating agents, and in particular relates to a synthetic process of a heavy metal chelating agent. The method comprises the following steps: firstly, diluting organic amine for 2-10 times by using organic solvents; secondly, adding the enough amount of carbon disulfide into the diluted organic amine by controlling the reaction temperature to be between 30 and 50 DEG C to obtain an intermediate product; and thirdly, adding hydroxide powder into the intermediate product and stirring, performing solid-liquid separation to obtain the heavy metal chelating agent. Compared with the prior art, by reducing the concentration of organic amine, the intense degree of the reaction can be effectively reduced, so that the reaction temperature is increased. A test proves that the quality of the product has no difference from that of the previous product when the temperature is controlled to be between 30 and 50 DEG C; therefore, under a normal condition, normal production can be met by using common circulating water, so that equipment facilities such as refrigerating units for cooling are eliminated, the labor intensity of operation personnel is also reduced, and the cost is greatly reduced.

Description

The synthesis technique of heavy metal chelant
Technical field
The invention belongs to sequestrant technical field, particularly a kind of synthesis technique of heavy metal chelant.
Background technology
Heavy metal wastewater thereby refers to the waste water containing heavy metal of discharging in the Industrial processes such as mining and metallurgy, machinofacture, chemical industry, electronics and instrument.Heavy metal (as containing cadmium, nickel, mercury, zinc etc.) waste water is that environmental pollution is the most serious and endanger one of maximum trade effluent to the mankind.And the heavy metal in waste water generally can not decompose destruction, its location can only be shifted and change its Material Form.Such as, after chemical precipitation process, the heavy metal in waste water is transformed into insoluble chemical compound from the ionic condition of dissolving and precipitates, and transfers in mud from water; After ion exchange treatment, the metal ion in waste water is transferred on ion exchange resin; Transfer in regeneration waste liquid from ion exchange resin again after regeneration.
Wherein, often will use heavy metal chelant during chemical treatment, during heavy metal chelating in this sequestrant and waste water, can generate water-fast heavy metal chelate, this inner complex exists with the enforcement of suspension liquid in water.Therefore, in actual application, general needs adopts the method adding flocculation agent or sinking agent in suspension liquid that inner complex is settled down, thus reaches the object of separating beavy metal.
At present, how utilizing more effective, more economical method to solve the pollution of heavy metal ion to environment, is one of key factor determining heavy-metal pollution career development and growth.Therefore as the height of the price of the most important raw material heavy metal chelant of removal heavy metal, one of important factor of career development for this reason has been become.And reduce the production cost of heavy metal chelant, substantially can start with from following two aspects: the first utilizes more effectively more cheap raw material, replace the raw material that price is higher, thus reduction production cost, often technical difficulty is larger for the investigation and application of this respect, research cycle is longer, so progress is slower.It two is exactly utilize existing working condition, by strengthening management, technical renovation, changing existing technological operation parameter, reducing the consumption of energy, raw material, reducing operation easier, reducing the expenditure of human capital, to reach the object reducing production cost.
Existing production technique is first by pure organic amine material (purity>=99%) and CS 2with NaOH reaction, generate nabam salt metal chelator.Because the content of organic amine material is higher, with CS 2comparatively violent during reaction, for preventing the side reactions such as local superheating generation organic substance decomposing, need to carry out at a lower temperature reacting (usual temperature of reaction is lower than 10 DEG C).Therefore, just need the chilled brine of lower temperature to cool conversion unit, need to set up the installations and facilities such as refrigerator, saline groove, brine storage tank simultaneously.The normal production of product can be ensured, to produce 10000 tons of sequestrants per year, just need the freezing unit of 600,000 kilocalorie 2, brine storage tank 1, saline groove 1.600000 kilocalorie refrigerator assembly powers of motor are 150KW, and to produce calculating in 300 days year, only refrigerator power consumption just has 1,080,000 KWh.Running cost is higher.
In view of this, the necessary synthesis technique that a kind of lower-cost heavy metal chelant is provided.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, and a kind of synthesis technique of lower-cost heavy metal chelant is provided.
To achieve these goals, the present invention adopts following technical scheme:
The synthesis technique of heavy metal chelant, comprises the following steps:
The first step, first dilutes 2 ~ 10 times with organic solvent by organic amine;
Second step, joins in the organic amine after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction between 30 DEG C ~ 50 DEG C, obtain intermediate product;
3rd step, adds hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
One as the synthesis technique of heavy metal chelant of the present invention is improved, and described organic solvent is ethanol or methyl alcohol.
One as the synthesis technique of heavy metal chelant of the present invention is improved, and the organic amine described in second step is at least one in liquid dimethyl amine, diethylamine, quadrol and diethanolamine.
One as the synthesis technique of heavy metal chelant of the present invention is improved, and oxyhydroxide described in the 3rd step is at least one in sodium hydroxide, potassium hydroxide and ironic hydroxide.
One as the synthesis technique of heavy metal chelant of the present invention is improved, and the temperature of second step controls to be realized by recirculated water.
Relative to prior art, the present invention, by reducing the concentration (namely diluting) of organic amine, effectively can reduce the severity of reaction, makes reaction comparatively steady, thus temperature of reaction can be improved.Test shows, when control temperature is between 30 DEG C ~ 50 DEG C, and quality product and original also indifference.Therefore, under normal circumstances, just normal production can be met with common recirculated water, not only eliminate the installations and facilities such as freezing unit cooling, also reduce the labour intensity of operator, the power consumption of single freezing unit just can save 1,080,000 KWh every year, thus greatly reduces cost.
Embodiment
Below in conjunction with embodiment, the present invention and beneficial effect thereof are described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 3 times with methyl alcohol by diethylamine;
Second step, joins in the diethylamine after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction at 40 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds sodium hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
Embodiment 2
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 5 times with ethanol by quadrol;
Second step, joins in the quadrol after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction at 42 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds sodium hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
Embodiment 3
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 7 times with ethanol by diethanolamine;
Second step, joins in the diethanolamine after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction at 35 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds potassium hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
Embodiment 4
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 4 times with methyl alcohol by dimethylamine;
Second step, joins in the dimethylamine after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction at 35 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds ironic hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
Embodiment 5
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 4 times with ethanol by quadrol;
Second step, joins in the quadrol after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction at 45 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds sodium hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
Embodiment 6
The synthesis technique of the heavy metal chelant that the present embodiment provides, comprises the following steps:
The first step, first dilutes 6 times with ethanol by diethylamine, with ethanol, quadrol is diluted 5 times;
Second step, joins in the diethylamine after the dilution of the first step and quadrol by enough dithiocarbonic anhydride, control temperature of reaction between 41 DEG C ± 2 DEG C, obtain intermediate product by recirculated water;
3rd step, adds the mixed powder of potassium hydroxide and sodium hydroxide and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.

Claims (5)

1. the synthesis technique of heavy metal chelant, is characterized in that, comprises the following steps:
The first step, first dilutes 2 ~ 10 times with organic solvent by organic amine;
Second step, joins in the organic amine after the dilution of the first step by enough dithiocarbonic anhydride, control temperature of reaction between 30 DEG C ~ 50 DEG C, obtain intermediate product;
3rd step, adds hydroxide powder and stirs in intermediate product, then carries out solid-liquid separation, obtains heavy metal chelant.
2. the synthesis technique of heavy metal chelant according to claim 1, is characterized in that: described organic solvent is ethanol or methyl alcohol.
3. the synthesis technique of heavy metal chelant according to claim 1, is characterized in that: the organic amine described in second step is at least one in liquid dimethyl amine, diethylamine, quadrol and diethanolamine.
4. the synthesis technique of heavy metal chelant according to claim 1, is characterized in that: oxyhydroxide described in the 3rd step is at least one in sodium hydroxide, potassium hydroxide and ironic hydroxide.
5. the synthesis technique of heavy metal chelant according to claim 1, is characterized in that: the temperature of second step controls to be realized by recirculated water.
CN201410790054.2A 2014-12-18 2014-12-18 Synthetic process of heavy metal chelating agent Pending CN104528910A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410790054.2A CN104528910A (en) 2014-12-18 2014-12-18 Synthetic process of heavy metal chelating agent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410790054.2A CN104528910A (en) 2014-12-18 2014-12-18 Synthetic process of heavy metal chelating agent

Publications (1)

Publication Number Publication Date
CN104528910A true CN104528910A (en) 2015-04-22

Family

ID=52844604

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410790054.2A Pending CN104528910A (en) 2014-12-18 2014-12-18 Synthetic process of heavy metal chelating agent

Country Status (1)

Country Link
CN (1) CN104528910A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106824111A (en) * 2017-02-27 2017-06-13 湖南云平环保科技有限公司 The method that stalk prepares heavy metal chelant
CN110563622A (en) * 2019-09-05 2019-12-13 南通乐尔环保科技有限公司 Synthetic method of mixed heavy metal capture agent
CN110714213A (en) * 2019-10-31 2020-01-21 武汉奥邦表面技术有限公司 Cyanide-free alkaline cuprous copper electroplating complexing agent

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101050009A (en) * 2007-04-30 2007-10-10 河北理工大学 Medicament for reducing and removing heavy metal ion in wastewater in coal cutting subsidence area, and processing method
JP2008018311A (en) * 2006-07-11 2008-01-31 Nicca Chemical Co Ltd Treating agent for heavy metal-containing waste water and method for waste water treatment using the same
JP2009249399A (en) * 2008-04-01 2009-10-29 Tosoh Corp Heavy metal treatment agent and method for treating heavy metal pollutant
CN101857296A (en) * 2010-06-29 2010-10-13 湖南科技大学 Ethylenediamine-based heavy metal chelating agent and preparation method thereof
CN102070235A (en) * 2010-11-11 2011-05-25 华南理工大学 Water-soluble organic thiamine heavy metal chelating agent and preparation method thereof
CN102603046A (en) * 2012-04-05 2012-07-25 环境保护部华南环境科学研究所 Heavy metal ion complexing agent, preparation method and applications thereof
CN103143328A (en) * 2013-03-07 2013-06-12 西安科技大学 Preparation method of heavy metal chelating adsorbent
CN103466775A (en) * 2013-09-27 2013-12-25 广西博世科环保科技股份有限公司 Method for preparing heavy metal ion catching agent
CN103936980A (en) * 2014-03-12 2014-07-23 中国海洋石油总公司 Synthetic method for dithiocarbamate water purifying agent

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008018311A (en) * 2006-07-11 2008-01-31 Nicca Chemical Co Ltd Treating agent for heavy metal-containing waste water and method for waste water treatment using the same
CN101050009A (en) * 2007-04-30 2007-10-10 河北理工大学 Medicament for reducing and removing heavy metal ion in wastewater in coal cutting subsidence area, and processing method
JP2009249399A (en) * 2008-04-01 2009-10-29 Tosoh Corp Heavy metal treatment agent and method for treating heavy metal pollutant
CN101857296A (en) * 2010-06-29 2010-10-13 湖南科技大学 Ethylenediamine-based heavy metal chelating agent and preparation method thereof
CN102070235A (en) * 2010-11-11 2011-05-25 华南理工大学 Water-soluble organic thiamine heavy metal chelating agent and preparation method thereof
CN102603046A (en) * 2012-04-05 2012-07-25 环境保护部华南环境科学研究所 Heavy metal ion complexing agent, preparation method and applications thereof
CN103143328A (en) * 2013-03-07 2013-06-12 西安科技大学 Preparation method of heavy metal chelating adsorbent
CN103466775A (en) * 2013-09-27 2013-12-25 广西博世科环保科技股份有限公司 Method for preparing heavy metal ion catching agent
CN103936980A (en) * 2014-03-12 2014-07-23 中国海洋石油总公司 Synthetic method for dithiocarbamate water purifying agent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘立华等: "重金属螯合絮凝剂对废水中铅、镉的去除性能", 《环境工程学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106824111A (en) * 2017-02-27 2017-06-13 湖南云平环保科技有限公司 The method that stalk prepares heavy metal chelant
CN110563622A (en) * 2019-09-05 2019-12-13 南通乐尔环保科技有限公司 Synthetic method of mixed heavy metal capture agent
CN110714213A (en) * 2019-10-31 2020-01-21 武汉奥邦表面技术有限公司 Cyanide-free alkaline cuprous copper electroplating complexing agent

Similar Documents

Publication Publication Date Title
CN110240182A (en) The recycling processing method of rich lithium aluminium electrolyte
CN104528910A (en) Synthetic process of heavy metal chelating agent
CN103601322A (en) Integrated process of recycle of aluminum profile production wastewater and comprehensive utilization of waste residue
CN104975183A (en) Method for separating and recovering copper from acid CuCl2 etching solution
CN106495404A (en) A kind of processing method of the high salinity cupric organic wastewater of highly acidity
CN103922521B (en) Method used for chrome tanning waste water treatment and chrome recovery
CN106086407A (en) The recovery method of manganese in a kind of nickel cobalt leachate
CN104928481A (en) Method for separating recycling of Cu/Ni from nitric acid stripping solution
CN106630313A (en) Reduction circulation process method for recycling zinc elements in iron-containing waste acid
CN105776655A (en) Method for producing copper concentrates and prussian blue by means of mine copper cyanide wastewater
CN105316098A (en) Method for treating rolling waste lubricating oil with aluminum flocculant
CN104787983A (en) Treatment process for synthetic fiberboard production wastewater
CN104876367A (en) Method for comprehensively treating acid liquid obtained from waste hydrochloric acid and alkaline sludge
CN103693729B (en) Treatment method for nitric-acid-containing wastewater in adipic acid production technology
CN104495998B (en) Method for synthesizing heavy metal chelating agent
CN108101121A (en) A kind of resource recycling method of iron content waste sulfuric acid solution
CN102976434B (en) Method for treating lead-containing wastewater
CN100357176C (en) Method for recovering vitriol from waste vitrol containing metal salt
CN104787946A (en) Steel rolling waste acid complete resource recycling method
CN105923842A (en) Method for removing heavy metal ions in sewage
CN106745416B (en) Application of arsenic and fluorine in high-temperature molten copper slag treatment of contaminated acid and application method thereof
CN103496801B (en) A kind of electrolytic manganese chromate waste water processing and the method for reclaiming Cr VI
CN102295364B (en) Apparatus and process for virtuous cycle treatment of slag flushing water of gas producer
CN109112597B (en) Configuration and method for reforming oxidation line to recover oxidation liquid and protect mono-nickel salt coloring tank
CN105600836A (en) Method for recycling useful ingredients in acid pickling waste liquid

Legal Events

Date Code Title Description
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20150422