CN206897357U - A kind of autoclave of accurate temperature controlling - Google Patents
A kind of autoclave of accurate temperature controlling Download PDFInfo
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- CN206897357U CN206897357U CN201720651307.7U CN201720651307U CN206897357U CN 206897357 U CN206897357 U CN 206897357U CN 201720651307 U CN201720651307 U CN 201720651307U CN 206897357 U CN206897357 U CN 206897357U
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- flat bottom
- metal flat
- bottom container
- autoclave
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Abstract
A kind of autoclave of accurate temperature controlling is the utility model is related to, mainly includes minitype high voltage kettle, cold-hot integrated machine and metal Flat bottom container.Minitype high voltage kettle is placed in metal Flat bottom container, multiple spoilers 3 is provided with the space of metal Flat bottom container wall and autoclave, while heat-conducting medium communicates with the circulation of cold-hot integrated machine heat-conducting medium in metal Flat bottom container.It is to make heat-conducting medium mixing more uniform that it, which is acted on,.The inlet of metal Flat bottom container is connected with the liquid outlet of cold-hot integrated machine, by carrying out real-time detection to the temperature of minitype high voltage kettle and judging whether temperature is higher or lower than design temperature, cold-hot integrated machine starts cooling or heating in real time, and real-time and precise temperature control is carried out to minitype high voltage kettle.The utility model heating is more uniform, and heating real-time can be achieved, operate steadily, easy temperature control system, be less prone to failure, meanwhile, the utility model is easy to operate, and thermal loss is small, non-environmental-pollution.
Description
Technical field
Laboratory Instruments equipment technical field is the utility model is related to, specifically a kind of reaction under high pressure of accurate temperature controlling
Kettle.
Background technology
For chemical reaction process along with heat release or endothermic process, in order that reacting balance is carried out, side reaction is few, and then generates
Impurity is less, typically by strict temperature control, regulates and controls come the heat release to chemical reaction or endothermic process.Temperature control is related to
Chemically react the property of itself（Neither endothermic nor exothermic）, respective thermal effect of different reaction vessel in lab scale and amplification production process
Should.List generally relates to inhale exothermic process, at typical condition for reaction under high pressure（Such as hydrogenation reaction）, reaction under high pressure
Along with very exothermic process, if accurate temperature control can not be accomplished, the wind of reaction under high pressure process slug or even blast has been buried
Danger.Usually, in order to which heating process safe ready is carried out, minitype high voltage kettle is typically directly heated using heating mantle, Large-scale High-Pressure
Kettle is then typically heated using steam mode of heating, and heating mantle heats and steam heating have the characteristics of heating is rapid jointly,
However, steam is heated compared to heating mantle heats, heat is removed rapidly, and heating mantle can not then remove thermal source in time, and take preheating
The mode of dissipation, waste heat disperse slower.Therefore steam heating can be achieved according to temperature Real-time Feedback and accurately be adjusted, and heat
The temperature control stability for covering heating is not then high.Existing invention employs chuck（Conduction oil is full of in chuck）To carry out autoclave
Heating, can only heat, and can not freeze, and being equally faced with can not cool down and the rising of controlling reaction temperature is asked quickly
Topic, so as to realize the purpose of accurate temperature control.Therefore, under the prior art, minitype high voltage kettle and Large-scale High-Pressure kettle chemically reacted
Temperature control process is generally mutually far short of what is expected in journey, and this is steadily amplified to the risk produced greatly as laboratory safety.For preferable mould
Intend production, preferably control reaction, reduce side reaction impurity caused by chemical reaction, it would be highly desirable to a kind of new autoclave mode of heating
To meet in minitype high voltage kettle small-scale experiment the needs of to accurate temperature control.
The content of the invention
In order to solve the above problems, the utility model aims to provide a kind of accurately to be entered to minitype high voltage kettle chemical reaction process
The method of row temperature adjustment.In order to achieve the above object, the utility model uses following technical scheme：
1st, a kind of autoclave of accurate temperature controlling, including minitype high voltage kettle, cold-hot integrated machine and metal Flat bottom container,
It is characterized in that：Autoclave body 4 is placed in metal Flat bottom container 6, is provided with the space of metal Flat bottom container wall and autoclave
Multiple spoilers 3, it is to make heat-conducting medium mixing more uniform that it, which is acted on,.The inlet of metal Flat bottom container and cold-hot integrated machine 7
Liquid outlet be connected, the liquid outlet of metal Flat bottom container is connected with the inlet of cold-hot integrated machine, metal Flat bottom container height with
Autoclave body is highly suitable, and the diameter of metal Flat bottom container and the diameter ratio of autoclave body are 2:1-5:4.Cold-hot integrated machine 7
Temperature sensing table be inserted into autoclave body temperature sensing hole 1.Heat-conducting medium and cold-hot integrated machine in metal Flat bottom container 6
Heat-conducting medium circulation communicates.Heat-conducting medium heat exchange mode can also take winding pipe type heat transfer.
The autoclave of accurate temperature controlling described in the utility model, it is characterised in that：The metal Flat bottom container difference
The inlet and outlet of heat-conducting medium is installed additional in side lower end and opposite side upper end, and the position of inlet and outlet is located at water-bath respectively
1/5-1/2 and 1/2-4/5 at.
The autoclave of accurate temperature controlling described in the utility model, it is characterised in that：Kettle cover with agitating paddle 5 passes through spiral shell
Silk 2 with autoclave body is closed tightens, the temperature sensing table of cold-hot integrated machine is inserted into autoclave body temperature sensing hole（1）In.With
In the temperature detection sensor of detection autoclave body internal temperature, pass through the information obtained by the temperature sensor feedback, cold-hot integrated
Machine is automatically brought into operation accordingly to heat-conducting medium（Heating or refrigeration）.
A kind of autoclave of accurate temperature controlling disclosed in the utility model is possessed compared with prior art actively to imitate
Fruit is：The utility model employs cold-hot integrated machine to be heated to minitype high voltage kettle, using in cold-hot integrated machine to small
Type autoclave carries out temperature control, compared with traditional heating mantle heats mode, has advantages below：
（1）Because the utility model is heated using cold-hot integrated machine to minitype high voltage kettle, according to the spy on kettle cover
Temperature in temperature sensor real-time perception minitype high voltage kettle, led according to temperature in kettle higher or lower than design temperature to freeze or heat
Thermal medium, therefore, temperature can be precisely controlled, it is ensured that the accurate temperature control of exothermic reaction in minitype high voltage kettle, make reaction temperature
It is slow to spend the rate of climb, is controlled, effectively prevent the security incidents such as material spray, blast.
（2）By comparing, the minitype high voltage kettle using cold-hot integrated machine and the liter using steam-heated Large-scale High-Pressure kettle
Warm curve is similar, so as to which the course of reaction of minitype high voltage kettle preferably simulates the amplification production process of Large-scale High-Pressure kettle.
（3）Temperature fluctuation is smaller.Due to traditional heating mantle heats, not in time, temperature drift reaches 5-10 DEG C for radiating, this
Increasing substantially for impurity can be brought and gone beyond the limit, so as to which product quality can not be ensured；Pass through the utility model technology, temperature
Drift band is reduced to 1-2 DEG C, so that side reaction impurity content reduces, ensure that product quality.
Brief description of the drawings
Fig. 1 is the utility model using cold-hot integrated machine and the minitype high voltage kettle schematic diagram of Flat bottom container；
Wherein
1st, autoclave body temperature sensing hole 2, screw 3, spoiler
4th, autoclave body 5, agitating paddle
6th, the cold-hot integrated machine of inlet 7 of metal Flat bottom container.
Embodiment
The utility model is described below by specific embodiment.Unless stated otherwise, it is used in the utility model
Technological means is method known in those skilled in the art.In addition, embodiment be interpreted as it is illustrative, it is and unrestricted
The scope of the utility model, spirit and scope of the present utility model are limited only by the claims that follow.For people in the art
For member, on the premise of without departing substantially from the utility model in essence and scope, to the various changes in these embodiments or change
Fall within the scope of protection of the utility model.
Embodiment 1
Below in conjunction with the accompanying drawings, the utility model is further illustrated：
Autoclave body 4 is put into the metal Flat bottom container with spoiler 3, the inlet 6 of metal Flat bottom container with it is cold
The liquid outlet of hot all-in-one 7 is connected, and the liquid outlet of metal Flat bottom container is connected with the inlet of cold-hot integrated machine.Add reaction material
Liquid, by the kettle cover with agitating paddle 5 by screw 2 with kettle is closed tightens, the temperature sensing table of cold-hot integrated machine is added to
Autoclave body temperature sensing hole 1.Open stirring, design temperature, according to the real time and on line monitoring of autoclave body, in metal Flat bottom container
Heat-conducting medium communicates with the circulation of cold-hot integrated machine heat-conducting medium, carries out dynamic temperature regulation.
Embodiment 2
The example of the autoclave actual use of accurate temperature controlling
100g p-nitrophenyl acetamides accurately are weighed, are added in 1000ml autoclaves, add 400ml methanol and 5g palladium carbons,
Using being operated in embodiment 1, high-pressure hydrogenation is carried out.For accurate temperature controlling to 45 ± 1 DEG C, amide hydrolysis impurity is 0.04%（Impurity
Limit is≤0.1%）.
With this contrast, equally reacted using conventional heating mantle heats mode, controllable temperature is to 45 ± 5 DEG C, amide hydrolysis
Impurity is 0.21%, has exceeded the limit of impurities requirement of product.
Claims (5)
1. a kind of autoclave of accurate temperature controlling, including minitype high voltage kettle, cold-hot integrated machine and metal Flat bottom container, it is special
Sign is：Autoclave body（4）It is placed in metal Flat bottom container（6）In, it is provided with the space of metal Flat bottom container wall and autoclave
Multiple spoilers（3）, the inlet and cold-hot integrated machine of metal Flat bottom container（7）Liquid outlet be connected, metal Flat bottom container
Liquid outlet is connected with the inlet of cold-hot integrated machine, metal Flat bottom container height, cold-hot integrated machine highly suitable with autoclave body
（7）Temperature sensing table be inserted into autoclave body temperature sensing hole（1）In.
2. the autoclave of accurate temperature controlling according to claim 1, it is characterised in that：Metal Flat bottom container（6）In lead
Thermal medium and cold-hot integrated machine（7）Heat-conducting medium circulation communicate.
3. the autoclave of accurate temperature controlling according to claim 1, it is characterised in that：The diameter of metal Flat bottom container with
The diameter ratio of autoclave body is 2:1-5:4.
4. the autoclave of accurate temperature controlling according to claim 1, it is characterised in that：The metal Flat bottom container difference
The inlet and outlet of heat-conducting medium is installed additional in side lower end and opposite side upper end, and the position of inlet and outlet is located at water-bath respectively
1/5-1/2 and 1/2-4/5 at.
5. the autoclave of accurate temperature controlling according to claim 1, it is characterised in that：With agitating paddle（5）Kettle cover
Pass through screw（2）With autoclave body is closed tightens.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720651307.7U CN206897357U (en) | 2017-06-07 | 2017-06-07 | A kind of autoclave of accurate temperature controlling |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720651307.7U CN206897357U (en) | 2017-06-07 | 2017-06-07 | A kind of autoclave of accurate temperature controlling |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206897357U true CN206897357U (en) | 2018-01-19 |
Family
ID=61287168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201720651307.7U Active CN206897357U (en) | 2017-06-07 | 2017-06-07 | A kind of autoclave of accurate temperature controlling |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206897357U (en) |
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2017
- 2017-06-07 CN CN201720651307.7U patent/CN206897357U/en active Active
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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: Accurate temperature control's high -pressure batch autoclave Effective date of registration: 20190529 Granted publication date: 20180119 Pledgee: Beijing Chegongzhuang Branch of Huaxia Bank Co., Ltd. Pledgor: Beijing Mediking Pharmaceutical Group Co., Ltd. Registration number: 2019990000482 |
|
| 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: 20200724 Granted publication date: 20180119 Pledgee: Beijing Chegongzhuang Branch of Huaxia Bank Co.,Ltd. Pledgor: BEIJING MEDIKING BIOHARM Co.,Ltd. Registration number: 2019990000482 |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220602 Address after: Room 161, 16 / F, 101-2 to 16 / F, building 21, Rongda Road, Chaoyang District, Beijing 100012 Patentee after: Zhongguancun Technology Leasing Co.,Ltd. Address before: 100176 Room 203, 2nd floor, building 203, No.7, Rongchang East Street, Beijing Economic and Technological Development Zone, Daxing District, Beijing Patentee before: BEIJING MEDIKING BIOPHARM Co.,Ltd. |