CN207632730U - A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device - Google Patents
A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device Download PDFInfo
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- CN207632730U CN207632730U CN201721650021.3U CN201721650021U CN207632730U CN 207632730 U CN207632730 U CN 207632730U CN 201721650021 U CN201721650021 U CN 201721650021U CN 207632730 U CN207632730 U CN 207632730U
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- butylperoxyisopropyl carbonate
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- hydrogen chloride
- isopropanol
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Abstract
The utility model is related to a kind of chloromethyl butylperoxyisopropyl carbonate reaction units, are a kind of continuous reacting devices for the multistage continuous stir reactor and the combination of continuous reaction rectification tower that chloro-methyl-chloroformate and isopropanol reaction are produced to chloromethyl butylperoxyisopropyl carbonate.The characteristics of reaction unit, is entered in concatenated multi-stage reacting kettle after first continuously mixing chloro-methyl-chloroformate and isopropanol from storage tank, hydrogen chloride is taken away while reaction, product pump is sent into rectifying column after the completion of multi-stage reacting kettle reacts, hydrogen chloride is removed totally by the heating of reboiler, goes rectifier unit to obtain finished product after tower reactor reaches reaction balance.The hydrogen chloride gas of tower top after condensation and removal isopropanol by entering in vacuum pump, and de-chlorine hydride absorption section obtains hydrochloric acid after being removed by vacuum pump.
Description
Technical field
The utility model is related to a kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting devices.
Background technology
Chloromethyl butylperoxyisopropyl carbonate, Chloromethyl isopropyl carbonate, molecular formula C5H9ClO3,
CAS NO：35180-01-9, density：1.15g/cm3 boiling point：147.463 DEG C, be used as organic synthesis intermediate, anti-AIDS and
Hepatitis B medicine tenofovir/tenofovir intermediate.
It is that chloro-methyl-chloroformate and isopropanol exist in acid binding agent that chloromethyl butylperoxyisopropyl carbonate traditional handicraft, which takes route,
Under reacted, reaction obtain the hydrochloride of acid binding agent while generating chloromethyl butylperoxyisopropyl carbonate, then with centrifuge or
The mode of washing removes the hydrochloride of acid binding agent, then obtains finished product by rectifying, adds alkali collection acid binding agent.This technique is because want
Additional raw materials consumption can be brought using acid binding agent, including acid binding agent and the alkali of recycling acid binding agent, and often
Waste water is generated, corresponding environmental issue is brought.
Utility model content
The chloromethyl butylperoxyisopropyl carbonate continuous reacting device and method of the utility model are according to two in reactor
A fundamental reaction device is the advantage and disadvantage combination design of multistage CSTR reactors and tower reactive distillation reactor.It is mainly in view of
The economy and operability of the chemical reaction industrial implementation of big reaction volume.It is suitble to long residence time and big reaction volume, instead
Answer rectifying reactor that can then realize successive reaction and separation in tower.
What the technical solution of the utility model was realized in：A kind of chloromethyl butylperoxyisopropyl carbonate continuous reaction dress
It sets, raw material storage tank connects multi-stage reacting kettle, and the multi-stage reacting kettle is that 2-10 grades of single reaction kettles are connected in series, each reaction kettle
One end connects vacuum pump, and whole order reaction kettle connects rectifying column, and rectifying column tower top connects vacuum pump.
Further, be condenser, bottom at the top of the rectifying column it is reboiler.
Further, the multi-stage reacting kettle is preferably 2-4 grades.
Further, the rectifying column uses packed tower or plate column.
Further, whole order reaction kettle connects rectifying column by delivery pump.
In addition, chloromethyl butylperoxyisopropyl carbonate continuous reaction method, by reaction raw materials chloro-carbonic acid chloromethane in raw material storage tank
Ester and isopropanol convey multi-stage reacting kettle according to proportioning, and the HCl gas generated in reaction process is by gas-guide tube from vacuum pumping
Walk, multistage continuous stir reactor come out reaction solution by conveying be pumped into rectifying column among, among reactive distillation column, feed from tower
To tower reactor flowing and tower reactor reboiler in generate steam counter-flow contact, by among charging hydrogen chloride and a small amount of isopropanol steam
Hair becomes gas phase, and gas phase is condensed in overhead condenser, isopropanol is cooled down, and hydrogen chloride gas is then by vacuum pumping
It walks, the reaction mother liquor of reboiler reacts after hydrogen chloride removing reaches home, and finally carries out conventional rectification process.
The beneficial effects of the utility model are：Reaction system core is to eliminate acid binding agent, using chloro-methyl-chloroformate and
Isopropanol is directly reacted, and is during the reaction taken away the hydrogen chloride gas that reaction generates using vacuum pump, keeps reaction flat
It weighs and is converted to the line of production, finally make that the reaction was complete.Using multistage continuous stir reactor and tower reactor, initial reaction section need compared with
Long residence time section is during the reaction taken away hydrogen chloride while meeting the residence time using multistage continuous stir reactor,
Reaction remaining hydrogen chloride close in system when terminal can influence the process for being reacted to terminal, the effect removed using autoclave
Fruit is simultaneously bad, at this moment, reactive distillation is carried out using a tower reactor, in the qualified reaction that bottom of tower is reached home
Liquid, and by the vapor condensation of tower top to -15 DEG C, by the isopropyl alcohol reflux of containing hydrogen chloride, incoagulability hydrogen chloride gas passes through vacuum
Pumping is walked.Qualified reaction solution can be obtained finished product using conventional rectification.
Description of the drawings
Fig. 1 is the structural schematic diagram of chloromethyl butylperoxyisopropyl carbonate continuous reacting device.
Specific implementation mode
Explanation is further explained to the utility model with reference to specific embodiment.
As shown in Figure 1, a kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device, raw material storage tank 1 connects reaction of high order
Kettle 2, the multi-stage reacting kettle are that 3 grades of single reaction kettles 21 are connected in series, and each reaction kettle one end connects vacuum pump 4, and whole grade is anti-
Kettle is answered to connect rectifying column 6 by delivery pump 5,6 tower top of rectifying column connects vacuum pump 4.It is condenser 61, bottom at the top of the rectifying column
Portion is reboiler 62.The rectifying column uses packed tower or plate column.Its reaction principle is, by reaction raw materials chlorine in raw material storage tank
Monochlorome-thylchloroformate and isopropanol convey multi-stage reacting kettle according to proportioning, the HCl gas generated in reaction process by gas-guide tube from
Vacuum pump is taken away, multistage continuous stir reactor come out reaction solution by conveying be pumped into rectifying column among, among reactive distillation column, into
Expect from the steam counter-flow contact generated into tower reactor flowing and tower reactor reboiler in tower, by hydrogen chloride among charging and a small amount of
Isopropanol evaporation becomes gas phase, and gas phase is condensed in overhead condenser, isopropanol is cooled down, and hydrogen chloride gas is then true
Empty pumping is walked, and the reaction mother liquor of reboiler reacts after hydrogen chloride removing reaches home, and finally carries out conventional rectification process.
Embodiment 1, in the rectifying column of the reaction kettle and tower combination DN800*16000 meters high of 3 concatenated 2000L
In, it is put into per hour into chloro-methyl-chloroformate 260.08kg/h, isopropanol 174.41kg/h, third-order reaction kettle temperature degree controls
40 degree, the control of rectifying column bottom temperature at 80 degree, -20 spends by tower top temperature control, system vacuum -0.07MPa, finally obtained
Crude product quality is 366.76kg/h, 63.70 kg/h of unreacted S05 residues, and the hydrogen chloride gas weight taken away from vacuum pump is
66.54 kg/h, content about 99%.
Embodiment 2, in the reactor of the reaction kettle and tower combination DN800*16000 meters high of 3 concatenated 2000L
In, it is put into per hour into chloro-methyl-chloroformate 195.06kg/h, isopropanol 130.80kg/h, third-order reaction kettle temperature degree controls
40 degree, the control of depickling column bottom temperature at 80 degree, -20 spends by tower top temperature control, system vacuum -0.07MPa, finally obtained
Crude product quality is 274.03kg/h, unreacted S05 residues 47.02kg/h, and the hydrogen chloride gas weight taken away from vacuum pump is
49.21 kg/h, content about 99%.
Claims (5)
1. a kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device, which is characterized in that raw material storage tank connects multi-stage reacting kettle,
The multi-stage reacting kettle is that 2-10 grades of single reaction kettles are connected in series, and each reaction kettle one end connects vacuum pump, whole order reaction kettle
Rectifying column is connected, rectifying column tower top connects vacuum pump.
2. chloromethyl butylperoxyisopropyl carbonate continuous reacting device according to claim 1, which is characterized in that the rectifying
It is reboiler that top of tower, which is condenser, bottom,.
3. chloromethyl butylperoxyisopropyl carbonate continuous reacting device according to claim 1, which is characterized in that the multistage
Reaction kettle is 2-4 grades.
4. chloromethyl butylperoxyisopropyl carbonate continuous reacting device according to claim 1, which is characterized in that the rectifying
Tower uses packed tower or plate column.
5. chloromethyl butylperoxyisopropyl carbonate continuous reacting device according to claim 1, which is characterized in that whole order reaction
Kettle connects rectifying column by delivery pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721650021.3U CN207632730U (en) | 2017-12-01 | 2017-12-01 | A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device |
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| CN201721650021.3U CN207632730U (en) | 2017-12-01 | 2017-12-01 | A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device |
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| CN207632730U true CN207632730U (en) | 2018-07-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805202A (en) * | 2017-12-01 | 2018-03-16 | 内蒙古圣氏化学股份有限公司 | A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device and method |
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2017
- 2017-12-01 CN CN201721650021.3U patent/CN207632730U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107805202A (en) * | 2017-12-01 | 2018-03-16 | 内蒙古圣氏化学股份有限公司 | A kind of chloromethyl butylperoxyisopropyl carbonate continuous reacting device and method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A continuous reaction device for chloromethyl isopropyl carbonate Effective date of registration: 20210324 Granted publication date: 20180720 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS Co.,Ltd. Registration number: Y2021150000028 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220518 Granted publication date: 20180720 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS CO.,LTD. Registration number: Y2021150000028 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A continuous reaction device for chloromethyl isopropyl carbonate Effective date of registration: 20220526 Granted publication date: 20180720 Pledgee: Bank of China Limited BAYANHOT branch Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS CO.,LTD. Registration number: Y2022150000044 |