CN105949100B - The production technology of new dithiocarbamates heavy metal chelant - Google Patents
The production technology of new dithiocarbamates heavy metal chelant Download PDFInfo
- Publication number
- CN105949100B CN105949100B CN201610333478.5A CN201610333478A CN105949100B CN 105949100 B CN105949100 B CN 105949100B CN 201610333478 A CN201610333478 A CN 201610333478A CN 105949100 B CN105949100 B CN 105949100B
- Authority
- CN
- China
- Prior art keywords
- phpg
- mixture
- heavy metal
- glycine
- production technology
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/16—Salts of dithiocarbamic acids
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/40—Inorganic substances
- A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to a kind of production technology of new dithiocarbamates heavy metal chelant.Chemical method production D-pHPG is one pot process racemic para hydroxybenzene glycine.The accessory substance of synthesis is generally all handled as solid waste, causes the wasting of resources and environmental pollution.Present invention be characterized in that utilized in D-pHPG production process, produce the mixture of o-hydroxy glycine and D-pHPG, mixture again with CS2Reaction, generate the dithiocar-bamate of D-pHPG or o-hydroxy glycine.The present invention efficiently utilizes caused accessory substance in D-pHPG production process, while generates certain economic benefit, reduces the pollution of discarded object.
Description
Technical field
The invention belongs to chelating agent technical field and field of environment protection, especially a kind of new dithiocar-bamate
The production technology of class heavy metal chelant.
Background technology
Chemical method production D-pHPG is to hydroxyl using phenol, glyoxalic acid, sulfamic acid one pot process DL
Base phenylglycine.Accessory substance o-hydroxy glycine is produced during synthesis.D-pHPG and the sweet ammonia of o-hydroxy
The ratio of acid is about 4:1~5:1.Synthetic wastewater concentrates by MVR, extracts producing ammonium sulfate byproduct；Extract the mother liquor after ammonium sulfate, drop
Temperature separates out the mixture of D-pHPG, o-hydroxy glycine and ammonium sulfate, and this part mixes is generally all
Handled as solid waste, cause the wasting of resources and environmental pollution.
The content of the invention
The invention aims to solve above-mentioned technical problem, and provide a kind of new dithiocarbamates weight
The production technology of metal-chelator, by the D-pHPG extracted in D-pHPG synthesis mother liquid, adjacent hydroxyl
The mixture of base phenylglycine and ammonium sulfate carries out comprehensive utilization of resources, produces heavy metal chelant.
The technical solution adopted by the present invention is：The production technology of new dithiocarbamates heavy metal chelant,
It is characterized in that using in D-pHPG production process, o-hydroxy glycine and D-pHPG are produced
Mixture, mixture again with CS2Reaction, generate the aminodithioformic acid of D-pHPG or o-hydroxy glycine
Salt.
Preferably, described D-pHPG production process is using phenol, glyoxalic acid, sulfamic acid one kettle way
Racemic para hydroxybenzene glycine is synthesized, generation accessory substance is the mixing of D-pHPG, o-hydroxy glycine, ammonium sulfate
Thing.
Preferably, D-pHPG, o-hydroxy glycine, the mixture of ammonium sulfate are added in a kettle,
The liquid caustic soda of water and concentration for 30-32% is added, dissolved clarification is stirred, is warming up to 80-90 DEG C, vacuum is opened, negative pressure ammonia still process, it is small to continue 2-4
When；30-40 DEG C is cooled to afterwards, adds CS2, then 40-60 DEG C of reaction 4-8h is warming up to, vacuum is opened afterwards, and negative pressure steams not anti-
The CS answered2, cooling discharge.
Preferably, it is characterized in that described reactor reclaimed water, liquid caustic soda and D-pHPG, the sweet ammonia of o-hydroxy
The mass ratio of sour, ammonium sulfate mixture is 1:3:1.
Preferably, it is characterized in that add in a kettle the water of above-mentioned mass ratio, liquid caustic soda and D-pHPG,
The mixture of o-hydroxy glycine and ammonium sulfate, 80 DEG C are warming up to, the ammonia still process under -0.06KPa vacuum, continue 4 hours,
Sampling detection ammonium sulphate content, during less than 1%, is cooled to 30 DEG C, adds CS2, it is warming up to 60 DEG C and flows back 8 hours, open vacuum, bears
Pressure steams unreacted CS2, cooling discharge.
The present invention efficiently utilizes caused accessory substance in D-pHPG production process, while generates certain
Economic benefit, reduce the pollution of discarded object.
Embodiment
The present invention is further described below：
Embodiment 1：1 ton of water, 3 tons of liquid caustic soda and 1 ton of D-pHPG, the sweet ammonia of o-hydroxy are added in a kettle
Acid, the mixture of ammonium sulfate, are warming up to 80 DEG C, the ammonia still process under -0.06KPa vacuum, continue 4 hours, sampling detection sulfuric acid
Ammonium content, during less than 1%, 30 DEG C are cooled to, adds CS2, it is warming up to 60 DEG C and flows back 4 hours, opens vacuum, negative pressure steams unreacted
CS2, sampling detection dithiocar-bamate content is 36.5%.
Embodiment 2：1 ton of water, 3 tons of liquid caustic soda and 1 ton of D-pHPG, the sweet ammonia of o-hydroxy are added in a kettle
Acid, the mixture of ammonium sulfate, are warming up to 80 DEG C, the ammonia still process under -0.06KPa vacuum, continue 6 hours, sampling detection sulfuric acid
Ammonium content, during less than 1%, 30 DEG C are cooled to, adds CS2, it is warming up to 60 DEG C and flows back 8 hours, opens vacuum, negative pressure steams unreacted
CS2, sampling detection dithiocar-bamate content is 38.8%.
Embodiment 3：1 ton of water, 3 tons of liquid caustic soda and 1 ton of D-pHPG, the sweet ammonia of o-hydroxy are added in a kettle
Acid, the mixture of ammonium sulfate, are warming up to 90 DEG C, the ammonia still process under -0.06KPa vacuum, continue 2 hours, be cooled to 40 DEG C, add
Enter CS2, it is warming up to 60 DEG C and flows back 4 hours, opens vacuum, negative pressure steams unreacted CS2, sampling detection dithiocar-bamate
Content is 26.3%.
Embodiment 4：1 ton of water, 3 tons of liquid caustic soda and 1 ton of D-pHPG, the sweet ammonia of o-hydroxy are added in a kettle
Acid, the mixture of ammonium sulfate, are warming up to 80 DEG C, the ammonia still process under -0.06KPa vacuum, continue 2 hours, be cooled to 30 DEG C, add
Enter CS2, it is warming up to 60 DEG C and flows back 4 hours, opens vacuum, negative pressure steams unreacted CS2, sampling detection dithiocar-bamate
Content is 26.3%.
The chemical equation of reaction is as follows：
Listed above is only the specific embodiment of the present invention, and the invention is not restricted to above embodiment, can also have
Many deformations.All deformations that one of ordinary skill in the art directly can export or associate from present disclosure,
It is considered as protection scope of the present invention.
Claims (4)
1. the production technology of new dithiocarbamates heavy metal chelant, it is characterised in that be D-pHPG
Production process is using phenol, glyoxalic acid, sulfamic acid one pot process racemic para hydroxybenzene glycine, and it is pair to produce accessory substance
Hydroxyphenylglycine, o-hydroxy glycine, the mixture of ammonium sulfate, mixture again with CS2Reaction, generate the sweet ammonia of para hydroxybenzene
The dithiocar-bamate of acid or o-hydroxy glycine.
2. the production technology of new dithiocarbamates heavy metal chelant according to claim 1, its feature
It is to add D-pHPG, o-hydroxy glycine, the mixture of ammonium sulfate in a kettle, adds water and concentration is
30-32% liquid caustic soda, dissolved clarification is stirred, is warming up to 80-90 DEG C, opened vacuum, negative pressure ammonia still process, continue 2-4 hours；It is cooled to afterwards
30-40 DEG C, add CS2, then 40-60 DEG C of reaction 4-8h is warming up to, vacuum is opened afterwards, and negative pressure steams unreacted CS2, cool and
Material.
3. the production technology of new dithiocarbamates heavy metal chelant according to claim 2, its feature
The quality of the mixture of reactor reclaimed water, liquid caustic soda and D-pHPG, o-hydroxy glycine, ammonium sulfate described in being
Than for 1:3:1.
4. the production technology of new dithiocarbamates heavy metal chelant according to claim 3, its feature
It is water, liquid caustic soda and the D-pHPG, o-hydroxy glycine and ammonium sulfate for adding above-mentioned mass ratio in a kettle
Mixture, be warming up to 80 DEG C, the ammonia still process under -0.06KPa vacuum, continue 4 hours, sampling detection ammonium sulphate content, it is low
When 1%, 30 DEG C are cooled to, adds CS2, it is warming up to 60 DEG C and flows back 8 hours, opens vacuum, negative pressure steams unreacted CS2, cooling
Discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333478.5A CN105949100B (en) | 2016-05-18 | 2016-05-18 | The production technology of new dithiocarbamates heavy metal chelant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610333478.5A CN105949100B (en) | 2016-05-18 | 2016-05-18 | The production technology of new dithiocarbamates heavy metal chelant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105949100A CN105949100A (en) | 2016-09-21 |
| CN105949100B true CN105949100B (en) | 2017-12-19 |
Family
ID=56912320
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610333478.5A Active CN105949100B (en) | 2016-05-18 | 2016-05-18 | The production technology of new dithiocarbamates heavy metal chelant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105949100B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674179B (en) * | 2017-10-27 | 2020-07-17 | 天津市职业大学 | Method for preparing epoxy resin by utilizing solid waste residues generated in production of p-hydroxyphenylglycine |
| CN115254054B (en) * | 2022-07-25 | 2024-01-23 | 浙江云涛生物技术股份有限公司 | Production process of copper ion adsorption resin |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE613461A (en) * | 1959-07-31 | |||
| GB1180216A (en) * | 1966-04-25 | 1970-02-04 | Reckitt And Sons Ltd | Dithiocarbamates |
| JPS5728074A (en) * | 1980-07-28 | 1982-02-15 | Ono Pharmaceut Co Ltd | Rhodanine derivative, its preparation, and inhibitor for aldose reducing enzyme consisting essentially of it |
| FR2817259B1 (en) * | 2000-11-29 | 2003-02-21 | Cis Bio Int | METAL CHELATION COMPOUND, RADIOPHARMACEUTICAL, MANUFACTURING METHOD THEREOF AND DIAGNOSTIC KIT |
-
2016
- 2016-05-18 CN CN201610333478.5A patent/CN105949100B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105949100A (en) | 2016-09-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103922416B (en) | A kind of method of Separation and Recovery iron from red mud | |
| CN106904667B (en) | The method of recycling purification nickel cobalt from manganese-containing waste | |
| CN108275819A (en) | A kind of method of ternary precursor washes recycling | |
| CN108504868B (en) | Method for recovering metal lithium in waste lithium ion battery | |
| CN102795641B (en) | Novel method for direct extraction recovery of ammonia nitrogen from electrolyzed manganese slag | |
| CN104018184B (en) | A kind of method producing electrolytic manganese metal | |
| CN107236870B (en) | A kind of method of v-bearing steel slag carbonization vanadium extraction | |
| CN101899582A (en) | Method for extracting vanadium pentoxide from vanadium slag | |
| CN103834815B (en) | A kind of method be separated containing tungsten tantalum in the rich tungsten slag of tantalum | |
| CN101818262A (en) | Method for removing chlorine from solution of zinc sulfate | |
| CN102358645B (en) | Fully-closed circulation treatment method for water used by electrolytic manganese metal production | |
| CN104195346B (en) | Clean process method for efficiently extracting chromium in extracted vanadium tailings | |
| CN105949100B (en) | The production technology of new dithiocarbamates heavy metal chelant | |
| CN102828052B (en) | Method for separating potassium, rubidium, cesium and vitriol after extracting lithium from lepidolite | |
| CN105603220A (en) | Method for extracting vanadium and chromium step by step and removing aluminum and silicon from alkaline aqueous solution | |
| CN101781172B (en) | Novel process for efficiently and continuously synthesizing 2-naphthol | |
| CN105731710B (en) | A kind of high magnesium ammonium sulfate waste water comprehensive reutilization method of cobalt smelting | |
| CN111057847A (en) | Green method for preparing battery-grade nickel sulfate from nickel salt | |
| CN105330344A (en) | Preparation method for extracting potassium sulphate from smelting blast furnace gas ash | |
| CN103602807B (en) | Treating method of removed molybdenum slag produced from tungsten smelting processes | |
| CN103774178B (en) | A kind of additive for electrolytic manganese from manganese sulfate electrolyte system and application method thereof | |
| CN104229892A (en) | Method for efficiently extracting, separating and recovering chromium and silicon from vanadium extraction tailings | |
| CN104928476B (en) | A kind of processing method of cobalt-copper alloy Water Quenching Slag | |
| CN105329952A (en) | Refining method of titanium dioxide by-product ferrous sulfate | |
| CN107746951A (en) | Method for separating nickel in sulfate solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhu Yuntao Inventor after: Liu Fengneng Inventor after: Jiang Xiaoming Inventor after: Gao Qi Inventor after: Gui Chenqiu Inventor after: Lin Weikang Inventor before: Zhu Yuntao Inventor before: Liu Fengneng Inventor before: Jiang Xiaoming Inventor before: Gao Qi Inventor before: Gui Chenqiu Inventor before: Lin Weikang |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |