GB2267844A - Interchangeable reactor vessel assemblage for automated laboratory reactors - Google Patents

Abstract

There is disclosed an interchangeable reactor vessel assemblage which is adapted to be used with existing, commercially available, computer automated laboratory reactors. The disclosed assemblage includes a plurality of reactor vessels of different sizes to accommodate a variety of chemical reaction masses or volumes but which are provided with uniform attachment means. A reactor vessel of pre-selected size is inserted into a jacket which serves to circulate oil around the reactor vessel to maintain the reaction temperature at a pre-determined level. The entire assemblage is provided with means enabling it to be removably secured to the mounting frame of an existing laboratory reactor. <IMAGE>

Description

TITLE OF THE INVENTION INTERCHANGEABLE REACTOR VESSEL ASSEMBLAGE FOR AUTOMATED LABORATORY REACTORS BACKGROUND OF THE INVENTION This invention relates to a novel, interchangeable reactor vessel assemblage which can be used with automated laboratory reactors.

In the field of process chemistry, the commercial manufacture of new chemical products typically progresses from laboratory reactions which are then scaled-up to pilot plant capacities before further scale-up to commercial quantities in a factory process. These scale-up operations generally include an evaluation of the process conditions involved such as time, temperature, pressure, reaction pH, reaction mass, rate of reaction and the like to optimize factory processes that are safe, economical and cost-effective.

During such scale-up evaluations, commercially available, computer automated laboratory reactors are often used such as those disclosed in U.S.

Patents 3,994,164 and 4,456,389 as well as Swiss Patent CH657702 A5. These computerized laboratory reactors typically include a jacketed module reaction vessel in which the chemical reactants are placed, means to stir the chemical reactants and means to control the temperature of the chemical reaction. Although such computerized laboratory reactors are efficient, the reaction mass or volume that they can accommodate through interchangeable reaction module vessels having capacities of from about 1 to about 2 liters. Thus, these computerized laboratory reactors cannot accommodate reactions masses significantly less than 1 liter.

It would be desireable to be able to utilize these computerized laboratory reactors to accommodate reaction masses significantly less than 1 liter as the ability to evaluate lower volumes of chemical reactants would be more economical, require less preparation and, in the case of potentially volatile reactions, would be much safer.

SUMMARY OF THE INVENTION It has now been found that these desireable goals can be achieved by employing the novel interchangeable reactor vessel assemblage of the invention which is adapted for use with commercially available, computer automated laboratory reactors. In general, the interchangeable reactor vessel assemblage of the invention comprises: a first plug unit adapted to be secured to the support frame of an existing automated laboratory reactor; a jacket having an inlet port and outlet port and means to removably secure it to said first plug unit;'a second plug unit; a plurality of reactor vessels each of which has means to removably secure them to said second plug unit; and, means to removably secure said first plug unit to said second plug unit.

The first and second plug units are preferably in the form of T-shaped plugs having external threads on their elongated body sections.

Each of the T-shaped plugs has a plurality of channels formed within them which are aligned to communicate with each other when assembled. These channels serve to accommodate the means by which the plugs are secured to each other as well as accommodate the passage therethrough of a stirring or mixing rod and provide additional ports which can accommodate calibration units or through which chemicals can be added to or withdrawn from the reactor vessel.

The jacket surrounds the selected reactor vessel and is the means through which heated or cooled oil is circulated to maintain the reaction temperature in the reactor vessel at a desired level. The neck of the jacket is internally threaded so that it can be screwed onto the first plug unit.

Each of the reactor vessels comprise a body section and a neck section. The body section of each of the reactor vessels are of different sizes to accommodate different masses or volumes of chemical reactants of from about- 50 ml to about 750 ml.

However, the neck section of each of the different sized reactor vessels are all the same size and each is internally threaded so that they can be screwed onto the second plug unit.

Assembly of the interchangeable reactor vessel assemblage of the invention includes threadably securing a reactor vessel of pre-selected size to the second plug unit; aligning the channels in the second plug unit with those in the first plug unit and securing the first and second plug units to each other; threadably securing the jacket to the first plug unit; and, securing the entire assembly to the support frame of an existing, computer automated laboratory reactor.

DETAILED DESCRIPTION OF THE INVENTION The interchangeable reactor vessel assemblage of the invention will become more apparent from the ensuing description when considered together with the accompanying drawing wherein like reference numerals denote like parts and wherein: Fig. 1 is a diagrammatic elevation view of a typical, commercially available, computer automated laboratory reactor; Fig. 2 is an enlarged, sectional view of a jacketed, interchangeable reaction vessel module vessel used with the laboratory reactor of Fig. 1; Fig. 3 is an exploded, elevation view, part in section and part in phantom, of the interchangeable reactor vessel assemblage of the invention; and; Fig. 4 is a view taken substantially on the line 4-4 of Fig. 3 showing the mating channels and ports of the plug members utilized in the assemblage of the invention.

The main components of a typical, commercially available, computer automated laboratory reactor shown in Fig. 1 comprise a temperature control unit 10, a chiller unit 11, a small electric motor 12 to which there is secured a stirring or mixing rod 13 having a mixing blade 14 at its lower end and a thermostatic head 15 to which there is attached a changeable reactor vessel module 16.

As shown in Fig. 2, the reactor vessel module 16 is a single, integral unit which can be manufactured from any suitable material such as metal or glass and which consists of an outer jacket 17 having an outlet port 18 and an inlet port 19 and a reactor vessel 20.

Outer jacket 17 and reactor vessel 20 are joined in an upper neck portion 21 which is fitted with a gasket 22 to form a seal when the reactor vessel module is secured to the thermostatic head 15.

In operation, the chemical reactants to be monitored are charged to the reactor vessel module 16 which is then secured to thermostatic head 15.

Thermostatic head 15 has a channel formed in it (not shown) to accommodate stirring or mixing rod 13 which is contained within the reactor vessel 20. Outlet port 18 and inlet port 19 are connected to the temperature control unit 10 by means of insulated, flexible conduits (not shown). Temperature control unit 10 is also connected to chiller unit 11 by insulated conduit means (not shown). After the reactor vessel module 16 is in place, heated or cooled oil is supplied from the temperature control unit 10 to circulate through outer jacket 17 by means of inlet and outlet ports 19 and 18 until the desired reaction temperature is obtained whereupon stirring or mixing rod 13 is actuated by electric motor 12 to rotate mixing blade 14.The chiller unit 12 contains a reservoir of cold oil and this cold oil is supplied to the temperature control unit 10 to mix with and maintain the oil being circulated through jacket 17 at a pre-determined temperature.

The interchangeable reactor vessel assemblage of the invention illustrated in Figs. 3 and 4 comprises two separate sub-assemblies; i.e., a jacket assembly and a reactor vessel assembly.

The jacket assembly comprises a T-shaped plug 23 and a jacket 27. Elongated body 24 of T-shaped plug 23 carries external threads 25 and the shoulder 26 of T-shaped plug 23 is used to secure it to the existing support frame of a laboratory reactor by seating jacket 27 onto jacket support 27a and seating support disc 47 into recess 26a of shoulder 26. Jacket support 27a is carried by the frame 50 of an existing laboratory reactor and is secured to support disc 47 means such as threaded bolts 48 and nuts 48a. Jacket 27 is an elongated member having a neck portion 28 that carries internal threads 29 and which is provided with integrally formed outlet and inlet ports 30 and 31, respectively.

The reactor vessel assembly also comprises a T-shaped plug 32 and a reactor vessel 36. The elongated body 33 of T-shaped plug 32 carries external threads 34 and its shoulder 35 is used to secure it to T-shaped plug 23 as described hereinbelow. The reactor vessel 36 has a body portion 37 and a neck portion 38 that carries internal threads 39.

As can be seen more clearly in Fig. 4, T-shaped plug 23 and T-shaped plug 32 each have formed therein a plurality of internal, common channels 40, 41, 42, 43, 44, 49a, 49b, 49c and 4.9d which are aligned with each other when the two sub-assemblies are assembled. Channel 40 serves to receive stirring or mixing rod 13 while channels 49a, 49b, 49c and 49d serve to receive conventional compression posts such as 45 and 46 shown in Fig. 3 which are used to assemble the sub-assemblies. Channels 41 and 43 serve as ports through which materials can be added to or withdrawn from reactor vessel 36. Channels 42 and 44 are used to accommodate calibration units or other measuring devices inserted into reactor vessel 36.

To assemble the interchangeable reactor vessel assemblage of the invention, a reactor vessel 36 of a size appropriate for the chemical reaction to be evaluated and monitored is first selected. All of the reactor vessels 36 are provided with neck portions 38 having the same diameter and with the same internal threads 39. Hence, only the dimensions or sizes of the body portion 37 of these reactor vessels 36 vary in capacity to accommodate reaction masses or volumes that can range from about as low as 50 ml to as much as about 750 ml. Depending upon the size of the reactor vessel 36 selected an appropriate sized mixing blade 14 is fitted to the end of stirring and mixing rod 13.

Mixing rod 13 is then threaded through common channel 40 in T-shaped plug 32. Reactor vessel 36 is screwed onto T-shaped plug 32. Mixing rod 13 is passed through common channel 40 of T-shaped plug 23 and T-shaped plug 32 is then secured to T-shaped plug 23 by means of conventional compression posts such as 45 and 46 inserted through common channels 48a, 48b, 48c and 48d.

Next, jacket 27 .is threadably secured to T-shaped plug 23 and the assemblage is connected to the existing support frame 50 by means of support disc 47 and jacket support 27a as described above and mixing rod 13 is secured to electric motor 12 (Fig. 1).

Finally, inlet port 31 and outlet port 30 are connected to the insulated flexible conduits leading to and from the temperature control unit 10 and the assemblage is ready to be run.

If desired before start up, one or more calibration or other probes can be inserted into the reactor vessel 36 through common channels 41, 42, 43 and 44 in T-shaped plugs 23 and 32.

During assembly, the various components of the invention assemblage are provided with conventional gaskets or O-rings suitable to provide air-tight seals such as between reactor vessel 36 and T-shaped plug 32, T-shaped plug 32 and T-shaped plug 23, the entry and exit ports of channel 40 and the stirring or mixing rod 13, and the like.

Operation of the invention assemblage is the same as that described above for commercial, computer automated laboratory reactors with heated or cooled oil being circulated from the temperature control unit 10 through jacket 27 by means of its inlet and outlet ports 31 and 30, respectively.

While any suitable materials can be used to manufacture the various components of the interchangeable reactor vessel assemblage of the invention, those that are inert to chemical reactants and are capable of being manufactured to close tolerances are preferred. For example, for jacket 27 and reactor vessel'36, glass is preferably employed whereas an inert, moldable plastic such as Teflons (i.e., polytetrafluoroethylene) is preferred for T-shaped plugs 23 and 32.

Although the interchangeable reactor vessel assemblage of the invention has been described with particularity and in some detail, it should be understood that modifications can be made therein without departing from the scope of the invention defined in the claims.

Claims (6)

WHAT IS CLAIMED IS

1. An interchangeable reactor vessel assemblage for use with automated laboratory reactors, said assemblage comprising: (a) a first plug unit adapted to be secured to the existing support frame of said automated laboratory reactor; (b) a jacket having an inlet port and an outlet port and means to removably secure it to said first plug unit; (c) a second plug unit; (d) a plurality of reactor vessels each of which has means to removably secure them to said second plug units; and, (e) means to removably secure said first plug unit to said second plug unit.

2. The assemblage of Claim 1 wherein said first plug unit has a plurality of channels formed therein and an elongated body carrying external threads.

3. The assemblage of Claim 1 wherein said jacket has a neck section carrying internal threads enabling it to be removably secured to said first plug unit.

4. The assemblage of Claim 1 wherein said second plug unit has a plurality of channels formed therein and an elongated body portion carrying external threads.

5. The assemblage of Claim 1 wherein said plurality of reaction vessels each have a body portion and a uniform neck portion carrying internal threads enabling each of said reaction vessels to be removably secured to said second plug unit.

6. An interchangeable reactor vessel assemblage for use with automated laboratory reactors, said assemblage comprising: (a) a first plug unit having a plurality of channels formed therein, adapted to be secured to the existing support frame of an automated laboratory reactor; (b) a jacket having a body portion, an inlet port and an outlet port formed in said body portion and a neck section carrying internal threads capable of being screwed onto said first plug unit; (c) a second plug unit having a plurality of channels which are capable of being aligned with the channels in said first plug and an elongated body carrying external threads; (d) a plurality of reactor vessels each of which has a body portion of different size and a uniform neck portion carrying internal threads capable of being screwed onto said second plug unit; and, (e) means to removably secure said first plug unit to said second plug unit.