CN109847547A - A kind of heavy metal chelant and preparation method thereof - Google Patents
A kind of heavy metal chelant and preparation method thereof Download PDFInfo
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- CN109847547A CN109847547A CN201910275270.6A CN201910275270A CN109847547A CN 109847547 A CN109847547 A CN 109847547A CN 201910275270 A CN201910275270 A CN 201910275270A CN 109847547 A CN109847547 A CN 109847547A
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Abstract
The invention discloses a kind of heavy metal chelants and preparation method thereof, the raw material that the heavy metal chelant preparation needs has: diethylenetriamine, carbon disulfide, distilled water, 1,2- Bromofume, powdered sodium hydroxide, dehydrated alcohol, ammonium hydroxide and ozone, equipment needed for prepared by the described heavy metal chelant have: use for laboratory ventilation equipment, split type overhead mechanical stirring equipment, use for laboratory closing biochemical test platform, laboratory universal electric furnace, Vacuum filtration device, laboratory refrigerator and gas reaction kettle.The heavy metal chelant and preparation method thereof, it is carried out in relatively closed environment, the gas for guaranteeing that volatilization property and reaction generate will not impact external environment and operator, and pass through the control to solution temperature and outside atmosphere temperature when reacting progress, improve the rate of reaction, and raw material used in this preparation method is reacted with the state of liquid or solution, is avoided the insufficient situation of hybrid reaction and is occurred.
Description
Technical field
The present invention relates to heavy metal chelant technical field, specially a kind of heavy metal chelant and preparation method thereof.
Background technique
Heavy metal chelant is also referred to as heavy metal ion releasing agent or heavy metal chelating agent, and being can be with heavy metal ion
The chemical industry medicament of strength chelating, is widely used in the industries such as Electroplating Operations, electronics industry and smelting iron and steel industry to heavy metal ion
Treatment process in, due to heavy metal element such as mercury, cadmium, lead, chromium and metalloid arsenic etc. have significant bio-toxicity, a huge sum of money
Belong to element to enter in soil and water body environment after the exit, by such as plant absorption of the producer in food chain and accumulate, then plants
Object is searched for food by first order consumer such as herbivore etc., and heavy metal element is assembled in first order consumer's body, and the first order disappears
The person of expense can be preyed on again by for example some carnivores of second level consumer, and heavy metal element again can be in the consumer's body of the second level again
Aggregation, and so on heavy metal element can largely assemble in subsequent third, fourth stage consumer's body, and the mankind are in food
The top of chain can eat a variety of animals and plants from the producer to fourth stage consumer, so heavy metal ion can be big in human body
Amount is assembled and can not be discharged, and shows that heavy metal has very strong destruction to most of protein and enzyme according to experiment, this
Sample heavy metal will accumulate in the organ of human body and destroy the function of human organ, will ultimately result in human organ failure.
As people's awareness of environmental protection continues to increase, and more and more industries will use heavy metal chelant to production now
The heavy metal generated in the process is handled, and using more heavy metal chelant, there are two main classes in actual production at present:
Xanthic acid esters and dithiocarbamate salt derivative, but existing dithiocarbamate salt derivative exists instead
Answer insufficient, reaction rate is compared with slow and the problem of to the carbon disulfide used needed for reaction volatile pollution.So needing needle
It is raw to existing dithiocarbamate salt derivative that a kind of heavy metal chelant and preparation method thereof is designed to the above problem
Production method improves.
Summary of the invention
The purpose of the present invention is to provide a kind of heavy metal chelants and preparation method thereof, to solve in above-mentioned background technique
It is proposed the problem of reaction is insufficient, and reaction rate is slower, carbon disulfide volatile pollution.
To achieve the above object, the invention provides the following technical scheme: a kind of heavy metal chelant and preparation method thereof, institute
Stating the raw material that heavy metal chelant preparation needs has: diethylenetriamine, carbon disulfide, distilled water, glycol dibromide, powder
Shape sodium hydroxide, dehydrated alcohol, ammonium hydroxide and ozone, equipment needed for prepared by the described heavy metal chelant have: use for laboratory ventilation
Equipment, split type overhead mechanical stirring equipment, use for laboratory closing biochemical test platform, laboratory universal electric furnace, vacuum filtration dress
It sets, laboratory refrigerator and gas reaction kettle.
Preferably, the heavy metal chelant the preparation method is as follows:
Preparation:
1. taking 50mL diethylenetriamine liquid in dark-brown vial, and by diethylenetriamine hydraulic seal, it is placed in reality
It tests in the refrigerator of room and saves, the temperature setting of laboratory refrigerator is 5 DEG C；
2. weighing 70g powdered sodium hydroxide using counter balance, take 200mL distilled water in 500mL beaker, by 70g
Powdered sodium hydroxide pours into, and is stirred using glass stirring rod to mixing liquid, until can not observe in solution not molten
Solve sodium hydrate solid, stand for standby use；
3. 100mL carbon disulfide is taken to seal in 250mL beaker, and with preservative film, it is placed in the refrigerator of laboratory；
4. taking 40mL1,2- Bromofume spare in 100mL beaker；
5. take 1L dehydrated alcohol and 1L ammonium hydroxide in plastic barrel respectively, tighten that bung is spare and 1 compression bottle ozone gas
It is spare；
6. split type overhead mechanical stirring equipment, laboratory universal electric furnace, Vacuum filtration device energization are placed in experiment
The exhaust duct of use for laboratory closing biochemical test platform is closed in closing biochemical test platform in room, is set by use for laboratory ventilation
It is standby to be slowly passed through the air that temperature is 10 DEG C into use for laboratory closing biochemical test platform；
Preparation process:
1. storage is had the dark-brown vial of diethylenetriamine liquid and fills the 250mL beaker of 100mL carbon disulfide
It is placed on use for laboratory closing biochemical test platform from the taking-up of laboratory refrigerator, and the 500mL for filling sodium hydroxide solution is burnt
The 100mL beaker of cup and the glycol dibromide for filling 40mL is placed on use for laboratory closing biochemical test platform；
2. 1L ammonium hydroxide has been poured into cover glass sealing container, there is cover glass sealing container to have an air inlet pipe, nozzle position
Under ammonium hydroxide liquid level, there is an escape pipe, be located on ammonium hydroxide liquid level, use for laboratory closes the exhaust duct of biochemical test platform
It is connected with there is the air inlet pipe of cover glass sealing container, has the escape pipe of cover glass sealing container to be connected with gas reaction kettle, will fill
There is the compression bottle of ozone to be connected with gas reaction kettle；
3. 1, the 2- Bromofume of 40mL and 50mL diethylenetriamine liquid are poured into 1 1000mL beaker, glass is used
Glass stirring rod quickly stirs 10s, adds 500mL distilled water, and 1000mL beaker is placed on the universal electric furnace of laboratory, and will be real
The heating temperature for testing room universal electric furnace is set as 50 DEG C, and mobile split type overhead mechanical stirring equipment enables split type overhead mechanical
It in the stirring structure insertion 1000mL beaker of mixing plant bottom end, and is contacted with mixing liquid in beaker, starts split type overhead
Mechanical stirring equipment stirs 90min, while starting split type overhead mechanical stirring equipment, is set by use for laboratory ventilation
It is standby that the air themperature being passed through is adjusted to 30 DEG C, and use for laboratory is opened after split type overhead mechanical stirring equipment starts 5min
Close the exhaust duct of biochemical test platform；
4. delaying after liquid 90min into 1000mL beaker in split type overhead mechanical stirring equipment stirring 1000mL beaker
The slow sodium hydroxide solution being added in 500mL beaker, split type overhead mechanical stirring equipment are stirred for 2h；
5. after stirring 2h, by 40mL1,2- Bromofume is added in 1000mL beaker, by the heating of laboratory universal electric furnace
Temperature setting is 95 DEG C, and the mixing speed of split type overhead mechanical stirring equipment is constant, persistently stirs 6h；
The carbon disulfide of the gas and volatilization that generate in reaction process closes the row of biochemical test platform by use for laboratory
Air piping and there is the air inlet pipe of cover glass sealing container to be passed through in ammonium hydroxide, carbon disulfide gas absorbed by ammonium hydroxide it is most of, instead
The gas and unabsorbed carbon disulfide that should be generated can enter in reaction kettle to be contacted with ozone, and oxidation occurs instead with ozone
It answers, then is discharged by the discharge structure of reaction kettle, the gas being discharged at this time is substantially free of carbon disulfide, pernicious gas also quilt mostly
Ammonium hydroxide reactive absorption dissolves and becomes innocuous substance by ozone oxidation reaction；
6. heavy metal chelant obtained in 1000mL beaker is fallen after split type overhead mechanical stirring equipment stirring 6h
Out, and using Vacuum filtration device filtered, then by the heavy metal chelant that is obtained after suction filtration down to capacity be 2L or more
In glass container, dehydrated alcohol is poured into and is washed, washing times are 3 times or more to get to heavy metal chelant.
Compared with prior art, the beneficial effects of the present invention are: the heavy metal chelant and preparation method thereof, using in phase
To the mode reacted in closed environment, guarantee the gas that there is relatively strong volatile substance and reaction to generate in raw material
External environment and operator will not be impacted, and by solution temperature and outside atmosphere when reacting progress
The control of temperature improves the rate of reaction, and raw material used in this preparation method is finally all with liquid or solution
State reacted, avoid the insufficient situation of hybrid reaction and occur.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of technical solution:
A kind of heavy metal chelant and preparation method thereof, the raw material that heavy metal chelant preparation needs have: divinyl three
Amine, carbon disulfide, distilled water, 1,2- Bromofume, powdered sodium hydroxide, dehydrated alcohol, ammonium hydroxide and ozone, the described huge sum of money
Belonging to equipment needed for prepared by chelating agent has: use for laboratory ventilation equipment, split type overhead mechanical stirring equipment, use for laboratory closing life
Change experimental bench, laboratory universal electric furnace, Vacuum filtration device, laboratory refrigerator and gas reaction kettle.
A kind of heavy metal chelant and preparation method thereof, the preparation method is as follows:
Preparation:
1. taking 50mL diethylenetriamine liquid in dark-brown vial, and by diethylenetriamine hydraulic seal, it is placed in reality
It tests in the refrigerator of room and saves, the temperature setting of laboratory refrigerator is 5 DEG C；
2. weighing 70g powdered sodium hydroxide using counter balance, take 200mL distilled water in 500mL beaker, by 70g
Powdered sodium hydroxide pours into, and is stirred using glass stirring rod to mixing liquid, until can not observe in solution not molten
Solve sodium hydrate solid, stand for standby use；
3. 100mL carbon disulfide is taken to seal in 250mL beaker, and with preservative film, it is placed in the refrigerator of laboratory；
4. taking 40mL1,2- Bromofume spare in 100mL beaker；
5. take 1L dehydrated alcohol and 1L ammonium hydroxide in plastic barrel respectively, tighten that bung is spare and 1 compression bottle ozone gas
It is spare；
6. split type overhead mechanical stirring equipment, laboratory universal electric furnace, Vacuum filtration device energization are placed in experiment
The exhaust duct of use for laboratory closing biochemical test platform is closed in closing biochemical test platform in room, is set by use for laboratory ventilation
It is standby to be slowly passed through the air that temperature is 10 DEG C into use for laboratory closing biochemical test platform；
Preparation process:
1. storage is had the dark-brown vial of diethylenetriamine liquid and fills the 250mL beaker of 100mL carbon disulfide
It is placed on use for laboratory closing biochemical test platform from the taking-up of laboratory refrigerator, and the 500mL for filling sodium hydroxide solution is burnt
The 100mL beaker of cup and the glycol dibromide for filling 40mL is placed on use for laboratory closing biochemical test platform；
2. 1L ammonium hydroxide has been poured into cover glass sealing container, there is cover glass sealing container to have an air inlet pipe, nozzle position
Under ammonium hydroxide liquid level, there is an escape pipe, be located on ammonium hydroxide liquid level, use for laboratory closes the exhaust duct of biochemical test platform
It is connected with there is the air inlet pipe of cover glass sealing container, has the escape pipe of cover glass sealing container to be connected with gas reaction kettle, will fill
There is the compression bottle of ozone to be connected with gas reaction kettle；
3. 1, the 2- Bromofume of 40mL and 50mL diethylenetriamine liquid are poured into 1 1000mL beaker, glass is used
Glass stirring rod quickly stirs 10s, adds 500mL distilled water, and 1000mL beaker is placed on the universal electric furnace of laboratory, and will be real
The heating temperature for testing room universal electric furnace is set as 50 DEG C, and mobile split type overhead mechanical stirring equipment enables split type overhead mechanical
It in the stirring structure insertion 1000mL beaker of mixing plant bottom end, and is contacted with mixing liquid in beaker, starts split type overhead
Mechanical stirring equipment stirs 90min, while starting split type overhead mechanical stirring equipment, is set by use for laboratory ventilation
It is standby that the air themperature being passed through is adjusted to 30 DEG C, and use for laboratory is opened after split type overhead mechanical stirring equipment starts 5min
Close the exhaust duct of biochemical test platform；
4. delaying after liquid 90min into 1000mL beaker in split type overhead mechanical stirring equipment stirring 1000mL beaker
The slow sodium hydroxide solution being added in 500mL beaker, split type overhead mechanical stirring equipment are stirred for 2h；
5. after stirring 2h, by 40mL1,2- Bromofume is added in 1000mL beaker, by the heating of laboratory universal electric furnace
Temperature setting is 95 DEG C, and the mixing speed of split type overhead mechanical stirring equipment is constant, persistently stirs 6h；
The carbon disulfide of the gas and volatilization that generate in reaction process closes the row of biochemical test platform by use for laboratory
Air piping and there is the air inlet pipe of cover glass sealing container to be passed through in ammonium hydroxide, carbon disulfide gas absorbed by ammonium hydroxide it is most of, instead
The gas and unabsorbed carbon disulfide that should be generated can enter in reaction kettle to be contacted with ozone, and oxidation occurs instead with ozone
It answers, then is discharged by the discharge structure of reaction kettle, the gas being discharged at this time is substantially free of carbon disulfide, pernicious gas also quilt mostly
Ammonium hydroxide reactive absorption dissolves and becomes innocuous substance by ozone oxidation reaction；
6. heavy metal chelant obtained in 1000mL beaker is fallen after split type overhead mechanical stirring equipment stirring 6h
Out, and using Vacuum filtration device filtered, then by the heavy metal chelant that is obtained after suction filtration down to capacity be 2L or more
In glass container, dehydrated alcohol is poured into and is washed, washing times are 3 times or more to get to heavy metal chelant.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (2)
1. a kind of heavy metal chelant and preparation method thereof, it is characterised in that: the original that the heavy metal chelant preparation needs
Material has: diethylenetriamine, carbon disulfide, distilled water, glycol dibromide, powdered sodium hydroxide, dehydrated alcohol, ammonium hydroxide and smelly
Oxygen, equipment needed for prepared by the described heavy metal chelant have: use for laboratory ventilation equipment, split type overhead mechanical stirring equipment,
Use for laboratory closes biochemical test platform, laboratory universal electric furnace, Vacuum filtration device, laboratory refrigerator and gas reaction kettle.
2. a kind of heavy metal chelant according to claim 1 and preparation method thereof, it is characterised in that: the heavy metal chela
Mixture the preparation method is as follows:
Preparation:
1. taking 50mL diethylenetriamine liquid in dark-brown vial, and by diethylenetriamine hydraulic seal, it is placed in laboratory
It is saved in refrigerator, the temperature setting of laboratory refrigerator is 5 DEG C；
2. weighing 70g powdered sodium hydroxide using counter balance, take 200mL distilled water in 500mL beaker, by 70g powder
Shape sodium hydroxide pours into, and is stirred using glass stirring rod to mixing liquid, until can not observe undissolved hydrogen in solution
Sodium oxide molybdena solid, stand for standby use；
3. 100mL carbon disulfide is taken to seal in 250mL beaker, and with preservative film, it is placed in the refrigerator of laboratory；
4. taking 40mL1,2- Bromofume spare in 100mL beaker；
5. take 1L dehydrated alcohol and 1L ammonium hydroxide in plastic barrel respectively, tighten that bung is spare and 1 compression bottle ozone gas is standby
With；
6. split type overhead mechanical stirring equipment, laboratory universal electric furnace, Vacuum filtration device energization are placed in use for laboratory
Close biochemical test platform in, close use for laboratory closing biochemical test platform exhaust duct, by use for laboratory ventilation equipment to
The air that temperature is 10 DEG C is slowly passed through in use for laboratory closing biochemical test platform；
Preparation process:
1. the dark-brown vial for having diethylenetriamine liquid and the 250mL beaker for filling 100mL carbon disulfide will be stored from reality
Test room refrigerator taking-up be placed in use for laboratory closing biochemical test platform on, and by fill sodium hydroxide solution 500mL beaker and
The 100mL beaker for filling the glycol dibromide of 40mL is placed on use for laboratory closing biochemical test platform；
2. 1L ammonium hydroxide has been poured into cover glass sealing container, there is cover glass sealing container to have an air inlet pipe, nozzle is located at ammonia
Under water level, there is an escape pipe, be located at ammonium hydroxide liquid level on, use for laboratory closing biochemical test platform exhaust duct with have
The air inlet pipe of cover glass sealing container is connected, and has the escape pipe of cover glass sealing container to be connected with gas reaction kettle, will be equipped with smelly
The compression bottle of oxygen is connected with gas reaction kettle；
3. 1, the 2- Bromofume of 40mL and 50mL diethylenetriamine liquid are poured into 1 1000mL beaker, stirred using glass
It mixes stick and quickly stirs 10s, add 500mL distilled water, 1000mL beaker is placed on the universal electric furnace of laboratory, and by laboratory
The heating temperature of universal electric furnace is set as 50 DEG C, and mobile split type overhead mechanical stirring equipment enables split type overhead mechanical stirring
It in the stirring structure insertion 1000mL beaker of equipment bottom end, and is contacted with mixing liquid in beaker, it is mechanical to start split type overhead
Mixing plant stirs 90min, will by use for laboratory ventilation equipment while starting split type overhead mechanical stirring equipment
The air themperature being passed through is adjusted to 30 DEG C, and opens use for laboratory closing after split type overhead mechanical stirring equipment starts 5min
The exhaust duct of biochemical test platform；
4. slowly adding after liquid 90min into 1000mL beaker in split type overhead mechanical stirring equipment stirring 1000mL beaker
Enter the sodium hydroxide solution in 500mL beaker, split type overhead mechanical stirring equipment is stirred for 2h；
5. after stirring 2h, by 40mL1,2- Bromofume is added in 1000mL beaker, by the heating temperature of laboratory universal electric furnace
95 DEG C are set as, the mixing speed of split type overhead mechanical stirring equipment is constant, persistently stirs 6h；
The carbon disulfide of the gas and volatilization that generate in reaction process closes the air-exhausting duct of biochemical test platform by use for laboratory
Road and there is the air inlet pipe of cover glass sealing container to be passed through in ammonium hydroxide, carbon disulfide gas is absorbed most of by ammonium hydroxide, and reaction produces
Raw gas and unabsorbed carbon disulfide can enter in reaction kettle to be contacted with ozone, and oxidation reaction occurs with ozone,
It is discharged again by the discharge structure of reaction kettle, the gas being discharged at this time is substantially free of carbon disulfide, and pernicious gas is also mostly by ammonia
Water reactive absorption dissolves and becomes innocuous substance by ozone oxidation reaction；
6. heavy metal chelant obtained in 1000mL beaker is poured out after split type overhead mechanical stirring equipment stirring 6h, and
It is filtered using Vacuum filtration device, then the heavy metal chelant obtained after suction filtration is held down to the glass that capacity is 2L or more
In device, dehydrated alcohol is poured into and is washed, washing times are 3 times or more to get to heavy metal chelant.
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| CN201910275270.6A CN109847547A (en) | 2019-04-08 | 2019-04-08 | A kind of heavy metal chelant and preparation method thereof |
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Application publication date: 20190607 |