CN207951455U - A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device - Google Patents
A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device Download PDFInfo
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- CN207951455U CN207951455U CN201820215572.5U CN201820215572U CN207951455U CN 207951455 U CN207951455 U CN 207951455U CN 201820215572 U CN201820215572 U CN 201820215572U CN 207951455 U CN207951455 U CN 207951455U
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- synthesis reactor
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Abstract
The utility model discloses a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction devices, including carbon disulfide head tank, synthesis reactor, pipe bundle condenser, cooling medium supply pipe and cooling medium discharge duct；The pipe bundle condenser is located at the top of synthesis reactor, and the carbon disulfide head tank is connected to the feed inlet at the top of synthesis reactor by carbon disulfide commissioning pipe；Synthesis reactor chuck is arranged in the synthesis reactor periphery；The advantageous effect of the present apparatus is, removes device with one reaction heat of chuck of synthesis reactor, quickly moves the heat that reaction generates, it is ensured that technological parameter within the limits prescribed, ensure that safety in production, reduce safety accident to greatest extent；Maintenance of equipment simultaneously, clean and maintenance workload are few, easy to use；Reaction temperature reduces by 10 DEG C than the prior art；The reaction time is significantly shortened, product economy benefit is improved.
Description
Technical field
The utility model belongs to chemical equipment technical field more particularly to a kind of high-molecular chelating agent aminodithioformic acid
Polyethyleneimine synthetic reaction device.
Background technology
Heavy metal pollution has become whole world great environmental problem.Selecting, smelting, processing and the production of country's heavy metal at present
In the plurality of heavy metal pollutant emission to environment generated in product manufacturing activities, serious environmental pollution is caused.In recent years, with
Polyethyleneimine is that skeleton synthesizes high-molecular chelating agent aminodithioformic acid polyethyleneimine in processing effluent containing heavy metal ions
Using increasing in industry, achievement in research continuously emerges, and representative research mainly has：
Sichuan University's sieve bodyguard loyalty etc. is in patent《A kind of heavy metal chelant of novel synthesis》In, selection molecular weight is
The aqueous solution of the polyethyleneimine 50% of 30000-120000, CS2, NaOH are Material synthesis heavy metal chelant；Tianjin is auspicious
Its army of chemical science and technology Development Co., Ltd Zhu etc. is sent out in patent《A kind of chelating agent having while handling contents of many kinds of heavy metal ion》
In, it proposes, using the polyethyleneimine of degree of polymerization 6-20 as raw material, the sodium hydroxide solution of 5%-40% to be added, carbon disulfide is added dropwise
A kind of heavy metal ion chelating agent is synthesized；Tsinghua University Wang Weis etc. are in patent《Macromolecule weight for stabilization of dangerous waste materials
Metal-chelator and preparation method thereof》In, use molecular weight for 5000 or more polyethyleneimine, under alkaline condition with CS2
The method of the macromolecular heavy metal chelating agent of synthetic fluid or crystal.Moriya etc. is in United States Patent (USP) (Removal of
Heavy Metals from Waste Water, U S Pat：4731187) in, by the DTC of low molecular weight and vulcanized sodium, more sulphur
Change after sodium is mixed in a certain ratio and is used for wastewater treatment；Moriya etc. is in United States Patent (USP) (Metal Scavengers for
Treating Waste Water, U S Pat：5387365) in, crosslinking agent is introduced, it is advanced before amine is reacted with CS2
The crosslinking of row polyamines and epoxychloropropane, obtained high-molecular chelating agent can generate larger alumen ustum when in use.William etc.
In United States Patent (USP) (Polymeric Dithiocarbamate Acid Salt C ompositions and Method of
Use, U S Pat：5500133) in, the dissolubility of trapping agent is improved, synthesis is a kind of water-soluble high molecular weight branched
DTC derivatives, after being crosslinked with epoxychloropropane and introducing branched structure, then react with carbon disulfide, contain in obtained product
There are multiple DTC groups.All there is some shortcomingss, such as reaction time to grow (General reactions 4-5 hours) for the above research, product
Chelate heavy metal ion energy force difference, production cost is high, reaction heat cannot remove and cause synthetic reaction dangerous in time in building-up process
Property is big etc..
It is existing using polyethyleneimine, sodium hydroxide solution, carbon disulfide as the poly- second of Material synthesis aminodithioformic acid
Alkene imines synthesis technology mainly has following deficiency：
1, reaction heat cannot remove in time, and reaction temperature is higher, cause carbon disulfide loss too big；
2, the reaction time is long, and the reaction time is even up to 18 hours in some synthesis technologies；
3, polyethyleneimine, sodium hydroxide solution, carbon disulfide, the proportioning of water are unreasonable, and especially carbon disulfide is excessive
Too much, other than increasing cost, excessive carbon disulfide without reacting or occurring side reaction or be lost from reaction system completely；
4, react insufficient, sometimes reaction finishes, and black fine particle is will appear in solution influences product appearance and use；
5, product bin stability is poor.
Utility model content
It cannot remove, react in time to solve reaction heat present in existing aminodithioformic acid polyethyleneimine synthesis
The problems such as temperature is high, the reaction time is long, product cost is high has made intensive studies synthesis synthetic reaction equipment, this practicality is new
Type provides a kind of device that can quickly move reaction heat, and specific technical solution is as described below：
A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device, including carbon disulfide are high-order
Slot, synthesis reactor, pipe bundle condenser, cooling medium supply pipe and cooling medium discharge duct；The pipe bundle condenser is located at synthesis reactor
Top, the carbon disulfide head tank is connected to the feed inlet at the top of synthesis reactor by carbon disulfide commissioning pipe；The synthesis
Synthesis reactor chuck is arranged in kettle periphery；
The cooling medium supply pipe is branched off into cooling medium first supply pipe and cooling two pipes of medium second supply pipe
Road, the lower part of the chuck of the cooling medium first supply pipe connection synthesis reactor, the cooling medium second supply pipe are connected to
The lower part of pipe bundle condenser side wall；
It is drawn from the first discharge pipe of cooling medium of synthesis reactor chuck top extraction and from pipe bundle condenser side wall upper part
The second discharge pipe of cooling medium imports the cooling medium discharge duct；
The synthesis reactor top connects pipe bundle condenser bottom by synthesis reactor feed back pipe, and the synthesis reactor bottom setting is closed
At kettle discharge port, the pipe branch connected after synthesis reactor discharge port is at two, wherein a branch pipe(tube) connects with condenser feed pipe
It connects, another branch pipe(tube) is connected to filter and finished pot.
Preferably, transfer tube is set after the synthesis reactor discharge port, before filter, power is provided for the transmission of material.
Preferably, valve is set on the synthesis reactor feed back pipe and glass regards cup, two are especially convenient for observing response material
Nitric sulfid flows back situation to judge response situation in kettle.
Preferably, online temperatuer detector is arranged in the synthesis reactor top.
Preferably, liquid level gauge is set in the carbon disulfide high position groove sidewall, for observing liquid level situation in slot, in time
Adjust the flow for the carbon disulfide being added.
Preferably, in tubulation in the cooling medium first supply pipe upper chuck inlet and cooling medium second supply pipe
Cooling medium inlet valve is respectively set at condenser inlet；In cooling medium the first discharge pipe upper chuck exit and cooling medium
Cooling medium outlet valve is respectively set at second discharge pipe upper tube array condensator outlet.
Preferably, valve is set in carbon disulfide head tank exit on carbon disulfide head tank and synthesis reactor connecting pipe
Door；Valve is respectively set on two laterals that synthesis reactor discharge port and transfer tube rear are connected.
Preferably, double-layered stirrer is set inside synthesis reactor, and the stirrer bottom is turbine agitator, and top is
Dasher is used for heat and mass transfer enhancement, promotes the progress of reaction.
A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device provided by the utility model
It has the following advantages：
1. one reaction heat of chuck using synthesis reactor removes device, the heat that reaction generates quickly is moved, it is ensured that technique is joined
Number within the limits prescribed, ensure that safety in production, reduce safety accident to greatest extent；Maintenance of equipment, clean and maintenance simultaneously
Workload is few, easy to use；
2, reaction temperature reduces by 10 DEG C than the prior art；
3, the reaction time is significantly shortened, according to the data provided in domestic existing open source literature, the domestic prior art
Reaction time is generally 8 hours, and some technological reaction time is up to 18 hours, and this technology is anti-including charging time
It is only 2 hours or so between seasonable；
4, carbon disulfide is cooled down using external pipe bundle condenser, cooling medium identical with synthesis reactor, reduces other objects
The trouble that the preparation of material is brought；
5, product yield improves 3% or more；Product economy benefit improves 3% or more；
6, the blender that synthesis reactor uses stirs for bilayer, and bottom stirring sheet stirs for turbine type, and top stirring sheet is paddle
Formula stirs, heat and mass transfer enhancement, promotes the progress of reaction.
Description of the drawings
The Figure of description for constituting the part of the utility model is used to provide a further understanding of the present invention, this
The illustrative embodiments and their description of utility model do not constitute the improper limit to the utility model for explaining the utility model
It is fixed.
Fig. 1 is a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction provided by the utility model
Structure drawing of device；
Wherein, 1- carbon disulfide head tank, 2- synthesis reactors, 3- pipe bundle condensers, 4- cool down medium supply pipe, and 5- coolings are situated between
Matter discharge pipe, 6- transfer tubes, 7- filters, 8- finished pots；11- carbon disulfide commissioning pipes, 12- liquid level gauges, 21- synthesis reactors folder
Set, 22- synthesis reactor discharge ports, 23- synthesis reactor feed back pipes, 31- condenser feed pipes, 41- cool down medium first supply pipe, 42-
Cooling medium second supply pipe, 51- cool down the first discharge pipe of medium, and 52- cools down the second discharge pipe of medium.
Specific implementation mode
It is noted that described further below be all exemplary, it is intended to provide further instruction to the utility model.It removes
Non- otherwise indicated, all technical and scientific terms used herein has the ordinary skill with the utility model technical field
The normally understood identical meanings of personnel.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the utility model.As used herein, unless the context clearly indicates otherwise, otherwise singular
Form is also intended to include plural form, additionally, it should be understood that, when in the present specification use term "comprising" and/or
When " comprising ", existing characteristics, step, operation, device, component and/or combination thereof are indicated.
Embodiment 1：
As background technology is introduced, cannot be removed in time for reaction heat exists in the prior art, reaction temperature is inclined
The problems such as height, carbon disulfide loss is big, and the reaction time is long, reaction is insufficient, the utility model provide a kind of high-molecule chelated
Agent aminodithioformic acid polyethyleneimine synthetic reaction device, as shown, including carbon disulfide head tank 1, synthesis reactor 2,
Pipe bundle condenser 3, cooling medium supply pipe 4 and cooling medium discharge duct 5；The pipe bundle condenser 3 is located at the upper of synthesis reactor 2
Side, the carbon disulfide head tank 1 are connected to the feed inlet at 2 top of synthesis reactor by carbon disulfide commissioning pipe 11；The synthesis
2 periphery setting synthesis reactor chuck 21 of kettle；
The cooling medium supply pipe 4 is branched off into cooling medium first supply pipe 41 and cooling 42 liang of medium second supply pipe
A pipeline, the cooling medium first supply pipe 41 connect the lower part of the chuck of synthesis reactor 2, the cooling medium second supply pipe
42 are connected to the lower part of 3 side wall of pipe bundle condenser；
Draw from the first discharge pipe of cooling medium 51 of 21 top of synthesis reactor chuck extraction and from 3 side wall upper part of pipe bundle condenser
The second discharge pipe of cooling medium 52 gone out imports the cooling medium discharge duct 5；
2 top of the synthesis reactor connects 3 bottom of pipe bundle condenser, 2 bottom of the synthesis reactor by synthesis reactor feed back pipe 23
Synthesis reactor discharge port 22 is set, and the pipe branch connected after synthesis reactor discharge port 22 is at two, wherein a branch pipe(tube) and condensation
Device feed pipe 31 connects, and another branch pipe(tube) is connected to filter 7 and finished pot 8.
In synthesis reactor 2, polyethyleneimine is reacted with sodium hydroxide, carbon disulfide, generates target product.The reaction
For exothermic reaction, if heat of reaction cannot remove and will appear that reaction temperature is higher, short time interior reaction temperature is rapidly heated in time
Situations such as, cause carbon disulfide largely to lose, or even safety accident occur.
After carbon disulfide is added dropwise by carbon disulfide head tank 1 to synthesis reactor 2, by cooling medium supply pipe 4 respectively to
Synthesis reactor chuck 21, pipe bundle condenser 3 are passed through cooling medium, and synthesis reactor chuck 21 quickly removes reaction by being passed through cooling medium
The heat of generation, operating personnel are by adjusting carbon disulfide rate of addition controlling reaction temperature.
In pipe bundle condenser 3, tube side walks reaction mass, and shell side walks cooling medium.
After the synthesis reactor discharge port 22, transfer tube 6 is set before filter 7, power is provided for the transmission of material.
Valve is set on the synthesis reactor feed back pipe 23 and glass regards cup, is convenient for observing response material especially carbon disulfide
The situation that flows back is to judge response situation in kettle.
Online temperatuer detector is arranged in 2 top of the synthesis reactor.
Liquid level gauge 12 is set in 1 side wall of carbon disulfide head tank, for observing liquid level situation in slot, adjustment in time is added
Carbon disulfide flow.
It is cold in tubulation on the 41 upper chuck inlet of cooling medium first supply pipe and cooling medium second supply pipe 42
Cooling medium inlet valve is respectively set in 3 inlet of condenser；In cooling 51 upper chuck exit of the first discharge pipe of medium and cooling Jie
Cooling medium outlet valve is respectively set in 52 upper tube array condenser of the second discharge pipe of matter, 3 exit.
Valve is set in 1 exit of carbon disulfide head tank on carbon disulfide head tank 1 and 2 connecting pipe of synthesis reactor；
Valve is respectively set on two laterals that synthesis reactor discharge port 22 and 6 rear of transfer tube are connected.
Double-layered stirrer is set inside synthesis reactor 2, and the stirrer bottom is turbine agitator, and top is stirred for paddle
Device is mixed, heat and mass transfer enhancement is used for, promotes the progress of reaction.
Embodiment 2：
Synthetic reaction carries out in 3000L enamel stills (synthesis reactor 2).
Cooling medium used is the ethylene glycol of freezing, and inlet temperature is -5 DEG C~-10 DEG C.
Operating process is as follows：
1,180kg carbon disulfide is pressed onto carbon disulfide head tank 1 from basin with compressed air, confirms that carbon disulfide is high-order
Slot top aqueous layer height is not less than 10mm, otherwise needs to keep the skin wet to head tank.
2, with vacuum by 1280kg deionized waters, 355kg mass concentrations be 32% industrial NaOH, 195Kg polyethyleneimine
Amine is pumped into synthesis reactor, and charging finishes, and continues stirring 20 minutes.
3, it first passes through cooling medium first supply pipe 41 and is passed through the freezing second two that temperature is -5 DEG C~-10 DEG C to synthesis reactor 2
When kettle temperature degree to be synthesized reaches 10 DEG C, carbon disulfide is added dropwise in alcohol since carbon disulfide head tank 1；When 2 temperature of synthesis reactor reaches
At 20 DEG C, the ethylene glycol of freezing is passed through to pipe bundle condenser 3 by cooling medium first supply pipe 42, cooling medium first is supplied
42 upper feeding valve opening of pipe is one third.Carbon disulfide rate of addition is adjusted, 18-25 DEG C of dropping temperature, curing are controlled
Carbon control adds in 60 minutes.Carbon disulfide turn on agitator and transfer tube 6 simultaneously is added dropwise, transfer tube is by bottom in synthesis reactor
Material be transferred to synthesis reactor top, keep material concentration in kettle almost the same, react synchronous and carry out, prevent from being layered above and below in kettle,
Extent of reaction gap is excessive.
Carbon disulfide finishes, and is passed through the charging of the ethylene glycol of freezing in cooling medium first supply pipe 42 to pipe bundle condenser
Valve opening is adjusted to 2/3rds.The freezing ethylene glycol being passed through to synthesis reactor is closed, the freezing second two in synthesis reactor chuck is utilized
The reaction was continued 20 minutes as cooling medium for alcohol, and reaction temperature is no more than 28 DEG C at this time.
4, the freezing ethylene glycol valve for leading to condenser is closed, condenser lower end valve is closed, will be synthesized with compressed air
Enter finished pot 8, sampling analysis, packaging and storage after material is filtered by filter 7 in kettle.
Product index testing result obtained is as follows：
In the synthetic reaction that the present apparatus occurs,
1,98% or more carbon disulfide conversion ratio；
2, it is reacted in 3000L enamel stills (synthesis reactor 2), domestic pharmaceutical industry industry carbon disulfide time for adding at least 4 is small
When, this technology control adds in 60 minutes；
3, carbon disulfide finishes, and using the freezing ethylene glycol in synthesis reactor chuck as cooling medium, the reaction was continued, with state
The interior existing operation of the same industry is compared, the technical program energy saving 5% or more；
4, using external pipe bundle condenser, compared with the identical cooling medium cooling carbon disulfide of synthesis reactor, domestic pharmaceutical industry
Industry carbon disulfide conversion ratio is usually no more than 90%, and the loss ratio country of the present invention prior art reduces by 5% or more.
The above descriptions are merely preferred embodiments of the present invention, is not intended to limit the utility model, for this
For the technical staff in field, various modifications and changes may be made to the present invention.It is all in the spirit and principles of the utility model
Within, any modification, equivalent replacement, improvement and so on should be included within the scope of protection of this utility model.
Claims (8)
1. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device, which is characterized in that including two
Nitric sulfid head tank, synthesis reactor, pipe bundle condenser, cooling medium supply pipe and cooling medium discharge duct；The pipe bundle condenser
Positioned at the top of synthesis reactor, the carbon disulfide head tank is connected to the charging at the top of synthesis reactor by carbon disulfide commissioning pipe
Mouthful；Synthesis reactor chuck is arranged in the synthesis reactor periphery；
The cooling medium supply pipe is branched off into cooling medium first supply pipe and cooling medium two pipelines of second supply pipe, institute
The lower part of the chuck of cooling medium first supply pipe connection synthesis reactor is stated, it is cold that the cooling medium second supply pipe is connected to tubulation
The lower part of condenser side wall；
The first discharge pipe of cooling medium drawn from synthesis reactor chuck top and the cooling drawn from pipe bundle condenser side wall upper part
The second discharge pipe of medium imports the cooling medium discharge duct；
The synthesis reactor top connects pipe bundle condenser bottom by synthesis reactor feed back pipe, and synthesis reactor is arranged in the synthesis reactor bottom
Discharge port, the pipe branch connected after synthesis reactor discharge port is at two, wherein a branch pipe(tube) is connect with condenser feed pipe, separately
One branch pipe(tube) is connected to filter and finished pot.
2. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 1
It sets, which is characterized in that transfer tube is set after the synthesis reactor discharge port, before filter, power is provided for the transmission of material.
3. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 2
It sets, which is characterized in that valve is set on the synthesis reactor feed back pipe and glass regards cup, is returned for observing response material carbon disulfide
Situation is flowed to judge response situation in kettle.
4. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 3
It sets, which is characterized in that online temperatuer detector is arranged in the synthesis reactor top.
5. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 4
It sets, which is characterized in that liquid level gauge is set in the carbon disulfide high position groove sidewall, for observing liquid level situation in slot.
6. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 5
It sets, which is characterized in that in tubulation on the cooling medium first supply pipe upper chuck inlet and cooling medium second supply pipe
Cooling medium inlet valve is respectively set at condenser inlet；In cooling medium the first discharge pipe upper chuck exit and cooling medium
Cooling medium outlet valve is respectively set at second discharge pipe upper tube array condensator outlet.
7. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 6
It sets, which is characterized in that valve is set in carbon disulfide head tank exit on carbon disulfide head tank and synthesis reactor connecting pipe
Door；Valve is respectively set on two laterals that synthesis reactor discharge port and transfer tube rear are connected.
8. a kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction dress according to claim 7
It sets, which is characterized in that double-layered stirrer is set inside synthesis reactor, and the stirrer bottom is turbine agitator, and top is
Dasher.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820215572.5U CN207951455U (en) | 2018-02-07 | 2018-02-07 | A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device |
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| CN201820215572.5U CN207951455U (en) | 2018-02-07 | 2018-02-07 | A kind of high-molecular chelating agent aminodithioformic acid polyethyleneimine synthetic reaction device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124624A (en) * | 2019-05-27 | 2019-08-16 | 济南大学 | A kind of preparation method of the dithiocar-bamate adsorbent based on corn stalk fiber element |
| CN110433757A (en) * | 2019-08-22 | 2019-11-12 | 安徽比特海新材料股份有限公司 | A kind of polymeric kettle of polymethylphenyl siloxane fluid automatic charging |
| CN115645815A (en) * | 2022-10-20 | 2023-01-31 | 乐尔环境科技有限公司 | Composite chelating agent for treating fly ash and preparation method thereof |
-
2018
- 2018-02-07 CN CN201820215572.5U patent/CN207951455U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124624A (en) * | 2019-05-27 | 2019-08-16 | 济南大学 | A kind of preparation method of the dithiocar-bamate adsorbent based on corn stalk fiber element |
| CN110433757A (en) * | 2019-08-22 | 2019-11-12 | 安徽比特海新材料股份有限公司 | A kind of polymeric kettle of polymethylphenyl siloxane fluid automatic charging |
| CN115645815A (en) * | 2022-10-20 | 2023-01-31 | 乐尔环境科技有限公司 | Composite chelating agent for treating fly ash and preparation method thereof |
| CN115645815B (en) * | 2022-10-20 | 2023-12-08 | 乐尔环境科技有限公司 | Composite chelating agent for treating fly ash and preparation method thereof |
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