WO2007029218A1 - Apparatus for low temperature reaction process - Google Patents

Apparatus for low temperature reaction process Download PDF

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Publication number
WO2007029218A1
WO2007029218A1 PCT/IE2005/000097 IE2005000097W WO2007029218A1 WO 2007029218 A1 WO2007029218 A1 WO 2007029218A1 IE 2005000097 W IE2005000097 W IE 2005000097W WO 2007029218 A1 WO2007029218 A1 WO 2007029218A1
Authority
WO
WIPO (PCT)
Prior art keywords
coolant
reaction vessel
container
temperature
contents
Prior art date
Application number
PCT/IE2005/000097
Other languages
French (fr)
Inventor
William Tully
John O'neill
Original Assignee
Pfizer Science And Technology Ireland Limited
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Pfizer Science And Technology Ireland Limited filed Critical Pfizer Science And Technology Ireland Limited
Priority to PCT/IE2005/000097 priority Critical patent/WO2007029218A1/en
Publication of WO2007029218A1 publication Critical patent/WO2007029218A1/en

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L7/00—Heating or cooling apparatus; Heat insulating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D1/00—Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators
    • F28D1/02—Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators with heat-exchange conduits immersed in the body of fluid
    • F28D1/0206—Heat exchangers immersed in a large body of liquid
    • F28D1/0213—Heat exchangers immersed in a large body of liquid for heating or cooling a liquid in a tank
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/02—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being helically coiled
    • F28D7/024—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being helically coiled the conduits of only one medium being helically coiled tubes, the coils having a cylindrical configuration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00083—Coils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/0015—Controlling the temperature by thermal insulation means
    • B01J2219/00153—Vacuum spaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00191—Control algorithm
    • B01J2219/00193—Sensing a parameter
    • B01J2219/00195—Sensing a parameter of the reaction system
    • B01J2219/002—Sensing a parameter of the reaction system inside the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00191—Control algorithm
    • B01J2219/00211—Control algorithm comparing a sensed parameter with a pre-set value
    • B01J2219/00213—Fixed parameter value
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00191—Control algorithm
    • B01J2219/00222—Control algorithm taking actions
    • B01J2219/00227—Control algorithm taking actions modifying the operating conditions
    • B01J2219/00238—Control algorithm taking actions modifying the operating conditions of the heat exchange system
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/18—Means for temperature control
    • B01L2300/1838—Means for temperature control using fluid heat transfer medium
    • B01L2300/185—Means for temperature control using fluid heat transfer medium using a liquid as fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/18—Means for temperature control
    • B01L2300/1894—Cooling means; Cryo cooling
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D3/00—Devices using other cold materials; Devices using cold-storage bodies
    • F25D3/10—Devices using other cold materials; Devices using cold-storage bodies using liquefied gases, e.g. liquid air

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Organic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A laboratory scale low temperature apparatus (1) for carrying out laboratory scale low temperature chemical reactions comprises an insulated pressure container (2) for a coolant, in this case liquid nitrogen at less than minus 1960C, and a reaction vessel (3) in the form of a silvered, vacuum jacketed borosilicate glass vessel in which low temperature reactions are carried out. An outlet (5) from the coolant container (2) is connected to an in-line heater 8 in which the coolant is heated. The in-line heater (8) is connected to a contact heat exchanger (12) in the form of a spiral coil extending into the reaction vessel (3). The temperature in the vessel (3) is monitored by a sensor (25) which provides a signal to a controller which is also connected to the in-line heater (8) to maintain the target temperature in the vessel (3).

Description

APPARATUS FOR LOW TEMPERTURE REACTION PROCESS
Introduction
The invention relates to a laboratory scale apparatus for carrying out low temperature reactions.
Some reactions require very low temperatures in order to proceed and proceed efficiently. The slightest fluctuations in temperature can have an adverse effect on the reaction yield or quality and/or slow the reaction time significantly. A limited amount of very low temperature laboratory equipment is available for operating as low as minus 1000C however what is available is complex and expensive and relies on difficult refrigerated cooling of viscous fluids that require continuous pumped circulation. There remains a need for a simple, efficient, cost effective, reliable and flexible system for carrying out routine low temperature reactions.
The object of the present invention is therefore to provide a simple apparatus or device capable of providing a stable very low temperature environment over a sustainable period of time for carrying out low temperature reactions with the flexibility to heat and cool at varying rates with a high degree of precision and avoiding the use of electrical refrigeration.
Statements of Invention
According to the invention there is provided an apparatus for carrying out very low temperature chemical reactions comprising:-
an insulated pressure container for both liquid and gaseous coolant;
a heater for vaporising the liquid coolant; a gaseous coolant outlet from the container;
an in-line heater for heating the gaseous coolant, the heater having a coolant inlet and a coolant outlet;
a conduit leading from the container outlet to the heater inlet;
a vacuum jacketed reaction vessel for carrying out a low temperature reaction;
a contact heat exchanger for directly heating or cooling the contents of the reaction vessel;
the heat exchanger having an inlet connected to the outlet of the in-line heater;
the heat exchanger having an outlet connected to an atmospheric vent;
a temperature sensor for monitoring the temperature of the contents of the reaction vessel; and
control means for receiving a signal from the temperature sensor and connected to the in-line heater for controlling the operation of the heater dependent on the temperature of the reaction vessel and the preset requirements.
In one embodiment of the invention the heat exchanger is a metal coil extending into the reaction vessel.
In another embodiment the contact heat exchanger is an insulated jacket surrounding the contents of the reaction vessel. Preferably the contents of the reaction vessel are held and controlled at a temperature of between minus 12O0C and plus 5O0C. Preferably the contents of the reaction vessel are held at a set temperature of less than minus 8O0C.
Preferably the contents of the reaction vessel can be cooled or heated at a preset rate.
Preferably the control means maintains the contents of the reaction vessel at plus or minus I0C of the preset point.
In one embodiment of the invention the conduit is vacuum insulated. Preferably the conduit is of flexible material.
Most preferably the reaction vessel has a vacuum insulated jacket.
In one embodiment of the invention the apparatus includes a pump means for delivering coolant from the container to the in-line heater.
Preferably the pump means is an evaporator for converting the liquid coolant in the container to gaseous coolant thus allowing delivery of the coolant from the container to the in-line heater.
Most preferably the insulated pressure coolant container maintains the temperature of the coolant at less than minus 196°C.
Preferably the coolant is liquid nitrogen.
In a further embodiment the operation of the pump is controlled by a control means. Brief Description of the Drawings
The invention will be more clearly understood from the following description given by way of example only with reference to the accompanying drawings in which:-
Fig. 1 is a schematic representation of an apparatus for carrying out low temperature chemical reactions according to the invention;
Fig. 2 is a perspective view of the front of the apparatus of Fig. 1 ;
Fig. 3 is a perspective view of an in-line heater of the apparatus according to the invention; and
Fig. 4 is a perspective view of a coolant container fittings of the apparatus of the invention.
Detailed Description
Referring to Fig. 1 there is illustrated a schematic representation of a laboratory scale low temperature apparatus 1 according to the invention for carrying out laboratory scale low temperature chemical reactions comprising an insulated pressure container 2 for a coolant, in this case liquid nitrogen at less than minus 196°C, and a reaction vessel 3 in the form of a silvered, vacuum jacketed borosilicate glass vessel in which low temperature reactions are carried out.
An outlet 5 from the coolant container 2 is connected by a conduit 6 to an inlet 7 of an in-line heater 8 in which the gaseous coolant is heated. The in-line heater 8 has a vacuum insulated block 9 and an outlet 10 which is connected by a flexible connector 11 to a contact heat exchanger 12, in this case in the form of a spiral coil, which extends into the reaction vessel 3 to cool the contents of the reaction vessel 3. The heat exchanger may also be an insulated jacket surrounding the contents of the reaction vessel 3. The coolant leaves the heat exchanger 12 through an outlet 13.
The conduit 6 is vacuum insulated and is of flexible material. The in-line heater 8 housing is also vacuum insulated. A vacuum is drawn on the conduit 6 by means of a vacuum pump 15.
Pump means for delivery of coolant gas from the coolant container 2 to the in-line heater 8 comprises an evaporator 20 in the coolant container 2 which imparts heat energy to the liquid nitrogen to induce gas formation and flow. The evaporator 20 is controlled by an independent controller 21.
A temperature sensor 25 extends into the reaction vessel 3 to monitor the temperature of the reaction mixture in the vessel 3. The sensor 25 produces a signal which is carried along a signal line 26 to a control means 30. The control means 30 is also connected to the in-line heater 8.
The temperature of the contents of the reaction vessel 3 is monitored by the control means 30 which has a set-point inputted by a key pad 35. The in-line heater 8 is controlled by the controller 30 to adjust heat transfer parameters to enhance and maintain the target temperature in the reaction vessel 3. The controller 30 is connected to a computer 50 at which reaction conditions may be monitored and controlled.
Figs. 2 to 4 illustrate the apparatus 1 of the invention for carrying out low temperature laboratory scale chemical reactions. The apparatus 1 may be easily moved as the coolant container 2 is set in a protection frame 41 fitted on castors and the reaction vessel 3 is attached to frame 40 which can be easily dismantled and reconstructed.
The coolant container 2 is fitted with pressure gauge 42, pressure relief device 43, and a liquid nitrogen fill point 44 fitted with a valve 45. The heater unit is held in position by clamps 46. The reaction vessel 3 has a vacuum insulated removable lid 47 which has entry points 48 that allow for charging of materials and attachment of equipment such as a stirring device 49 and a liquid dropping funnel 50.
The apparatus 1 is capable of cooling a reaction mixture to a temperature of minus
90°C in less than 1 hour, maintaining the temperature at plus or minus I0C from the set point and returning to room temperature in less than 2 hours at a predetermined cooling or heating rate. This is very advantageous for reactions where low temperatures are required for some steps while other steps require warmer temperatures in order to proceed efficiently and where temperature precision is essential.
The temperature of the gas in the low temperature coolant container 2 is approximately minus 185°C. Before entering the internal coil 12 of the reaction vessel 3 and after passing through the in-line heater 8 the temperature of the gas is approximately minus
165 to plus 2000C, depending on the heating/cooling requirements.
The invention is not limited to the embodiments hereinbefore described which may be varied in detail.

Claims

Claims
1. An apparatus for carrying out low temperature laboratory scale chemical reactions comprising:-
an insulated pressure container for both liquid and gaseous coolant;
a heater for vaporising the liquid coolant;
a gaseous coolant outlet from the container;
an in-line heater for heating the gaseous coolant, the heater having a coolant inlet and a coolant outlet;
a conduit leading from the container outlet to the heater inlet;
a vacuum jacketed reaction vessel for carrying out a low temperature reaction;
a contact heat exchanger for directly heating or cooling the contents of the reaction vessel;
the heat exchanger having an inlet connected to the outlet of the in-line heater;
the heat exchanger having an outlet connected to an atmospheric vent;
a temperature sensor for monitoring the temperature of the contents of the reaction vessel; and control means for receiving a signal from the temperature sensor and connected to the in-line heater for controlling the operation of the heater dependent on the temperature of the reaction vessel and the preset requirements.
2. An apparatus as claimed in claim 1 wherein the heat exchanger is a metal coil extending into the reaction vessel.
3. An apparatus as claimed in claim 1 wherein the contact heat exchanger is an insulated jacket surrounding the contents of the reaction vessel.
4. An apparatus as claimed in any preceding claim wherein the control means maintains the contents of the reaction vessel between minus 12O0C and plus 5O0C.
5. An apparatus as claimed in claim 4 wherein the control means maintains the contents of the reaction vessel at a temperature of less than minus 80°C.
6. An apparatus as claimed in any preceding claim wherein the control means maintains the contents of the reaction vessel at plus or minus I0C of the set point.
7. An apparatus as claimed in any of the preceding claim wherein the control means allows the contents of the reaction vessel to be heated or cooled at a preset rate.
8. An apparatus as claimed in any preceding claim wherein the conduit is vacuum insulated.
9. An apparatus as claimed in any preceding claim wherein the conduit is of flexible material.
10. An apparatus as claimed in any preceding claim wherein the reaction vessel has a vacuum insulated jacket.
11. An apparatus as claimed in any preceding claim including a pump means for delivering coolant from the container to the in-line heater.
12. An apparatus as claimed in claim 11 wherein the pump means is an evaporator for converting the liquid coolant in the container to gaseous coolant allowing delivery of the coolant from the container to the in-line heater.
13. An apparatus as claimed in any preceding claim wherein the insulated pressure coolant container maintains the temperature of the coolant at less than minus 196°C.
14. Apparatus as claimed in any preceding claim wherein the coolant is liquid nitrogen.
15. An apparatus as claimed in any of claims 11 to 15 wherein the operation of the pump is controlled by the control means.
PCT/IE2005/000097 2005-09-09 2005-09-09 Apparatus for low temperature reaction process WO2007029218A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/IE2005/000097 WO2007029218A1 (en) 2005-09-09 2005-09-09 Apparatus for low temperature reaction process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/IE2005/000097 WO2007029218A1 (en) 2005-09-09 2005-09-09 Apparatus for low temperature reaction process

Publications (1)

Publication Number Publication Date
WO2007029218A1 true WO2007029218A1 (en) 2007-03-15

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102818731A (en) * 2011-06-10 2012-12-12 中国石油天然气集团公司 Low temperature test system of low temperature stretching tests
CN103884602A (en) * 2012-12-20 2014-06-25 核工业西南物理研究院 Low-temperature stretching testing system and testing method
GB2574178A (en) * 2018-02-16 2019-12-04 Silicon Fuel Ltd Thermal Management

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4846584A (en) * 1987-12-17 1989-07-11 Pennwalt Corporation Automated calorimeter and methods of operating the same
EP0423944A1 (en) * 1989-09-28 1991-04-24 Tosoh Corporation Cooling method
WO1998057741A2 (en) * 1997-06-18 1998-12-23 Arencibia Associates, Inc. Temperature controlled reaction vessel
WO2001078890A2 (en) * 2000-04-13 2001-10-25 Arencibia Jose P Jr Temperature controlled reaction vessel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4846584A (en) * 1987-12-17 1989-07-11 Pennwalt Corporation Automated calorimeter and methods of operating the same
EP0423944A1 (en) * 1989-09-28 1991-04-24 Tosoh Corporation Cooling method
WO1998057741A2 (en) * 1997-06-18 1998-12-23 Arencibia Associates, Inc. Temperature controlled reaction vessel
WO2001078890A2 (en) * 2000-04-13 2001-10-25 Arencibia Jose P Jr Temperature controlled reaction vessel

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102818731A (en) * 2011-06-10 2012-12-12 中国石油天然气集团公司 Low temperature test system of low temperature stretching tests
CN103884602A (en) * 2012-12-20 2014-06-25 核工业西南物理研究院 Low-temperature stretching testing system and testing method
GB2574178A (en) * 2018-02-16 2019-12-04 Silicon Fuel Ltd Thermal Management
GB2574178B (en) * 2018-02-16 2022-07-13 Water Lane 6 Sf Ltd Thermal Management

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