CN114405425A - Disposable normal pressure/near normal pressure flexible reactor for laboratory - Google Patents
Disposable normal pressure/near normal pressure flexible reactor for laboratory Download PDFInfo
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Classifications
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- 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
- B01J19/0053—Details of the reactor
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- 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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- 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
- B01J19/28—Moving reactors, e.g. rotary drums
-
- 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
- B01J19/28—Moving reactors, e.g. rotary drums
- B01J19/285—Shaking or vibrating reactors; reactions under the influence of low-frequency vibrations or pulsations
-
- 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
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00011—Laboratory-scale plants
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- 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
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
Abstract
The invention discloses a laboratory normal pressure/near normal pressure cavity-shaped flexible reactor which is made of flexible materials, has a functional layer structure and a sealable interface, can use a manual tool or a motor tool to stir and mix materials in the modes of rolling, extruding, kneading and the like, and can realize the temperature control of the materials in the reactor in the modes of an interlayer or an externally attached heat insulation layer or a heat transfer layer, light irradiation, microwave irradiation, heat conduction and the like. The reactor is particularly suitable for reaction systems which are difficult to carry out conventional stirring and mixing of materials with small feed liquid volume (such as milliliter and hundred milliliter grades) and high solid content materials, high viscosity materials, non-Newtonian fluid materials and the like, and solves the problems of laboratory mixing and reaction of the materials. The reactor is a disposable container, has the advantages of simple and convenient use, convenient management, safety, environmental protection, low comprehensive cost and the like compared with the conventional reactor in a laboratory, and has obvious technical and use values.
Description
Technical Field
The invention belongs to the technical field of reactors for laboratories, and particularly relates to a disposable normal pressure/near normal pressure flexible reactor for laboratories.
Background
At present, the glass reactor is a normal/near normal pressure reactor commonly used in laboratories, such as a flask, a microchannel reactor, and the like. The disadvantages of such reactors are: the reaction device is complicated, and in actual operation, one or more functional devices are matched with the reactor for use, such as: the reaction device is not easy to move once being erected, and the more functional devices occupy more space, the larger the space is, the reaction device is not favorable for observing the reaction; in order to have good mixing effect, the reactor has minimum material addition amount, resources are wasted, and the 'three wastes' in a laboratory are increased by redundant chemical materials; special materials, such as high-solid-content materials, high-viscosity materials, non-Newtonian fluid materials and the like, are difficult to uniformly mix in the conventional stirring reactor due to adhesion, dead angles and the like; the sealing performance is poor, and the reaction with special environmental requirements such as no water, no oxygen and the like can not be met; after the first reaction is finished, the reactor needs to be cleaned by water and a chemical solvent, and a large amount of waste liquid is generated; glassware is broken easily, easily causes the injury to the experimenter.
Materials such as high solid content, high viscosity, elastoplasticity, non-Newtonian fluids and the like which are difficult to stir and mix in a conventional reactor in a laboratory are adopted, if a mechanical mixing method is adopted, for example, when a kneader, a screw extruder and other equipment are adopted, the lower limit requirement of loading and the dead volume of the equipment are generally more than 1L due to the running of the equipment, which is far beyond the experimental feeding amount of milliliters and hundred milliliters required by the laboratory, not only is a large amount of chemicals wasted, but also the experimental investment is increased, and the safety level of the experimental process and the total amount of waste materials are also improved; materials with high viscosity and equipment dead angles also increase the cleaning difficulty of mechanical equipment, generate more waste liquid and increase the treatment investment of three wastes; adhesion of materials, insufficient stirring, dead space and dead volume of equipment, etc., and also cause non-uniform mixing of materials and insufficient reaction.
In addition, for the laboratory-level reaction process which often needs accurate metering, the insufficient mixing of materials can directly lead to the full utilization of the materials, and further the analysis of the experimental process and the stability, reliability and accuracy of the experimental results are influenced. At this time, the development of a reactor which has strong material applicability, high operability, safety, environmental protection and low comprehensive use cost becomes a problem with great technical significance and use value.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above problems occurring in the prior art.
Therefore, the invention aims to provide a disposable atmospheric/near-atmospheric flexible reactor for a laboratory.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions: a disposable normal pressure/near normal pressure flexible reactor for laboratory use comprises,
the reactor is made of flexible materials, has a functional layer structure and a sealable interface, is in a cavity shape, and is used for reaction systems which are difficult to stir and mix conventionally, such as high-solid-content materials with feed liquid volume of milliliter and hundred milliliter grades, high-viscosity materials, non-Newtonian fluid materials and the like.
As a preferable scheme of the laboratory disposable normal pressure/near normal pressure flexible reactor, the invention comprises the following steps: the flexible material is one or more of a flexible polymer film material, a metal film material and a composite film material, and comprises a silicon rubber, a fluorine-containing high polymer material, a polyolefin high polymer material and a multilayer composite film material coated with aluminum, copper and alloy; in specific applications, suitable flexible reactor materials can be selected according to the characteristics of the physical system and the regulation requirements of the reaction process, such as: the acid-base corrosive substance adopts fluorine-containing polymer material; the catalytic reaction or the catalyst preparation adopts a multi-layer composite film material coated with aluminum, copper and alloy; the conventional system can meet the requirements by adopting silicon rubber and polyolefin high polymer materials, and is not limited to the example;
the composite film material can be a blended composite film, or a laminated film composite of multiple film materials, and complex characteristics such as corrosivity, strong oxidizing property, hygroscopicity, light-shielding reaction, high-temperature reaction and the like need multiple materials to be compounded to form a film, or multiple films with specific properties are sequentially laminated to form a film. The film-coating material can be added with fiber and silk thread to improve the mechanical strength of the film, and the reactor needs to be rolled, extruded and kneaded with high strength in the reaction process to uniformly mix materials, so that the structure of the reactor can be kept from being damaged.
As a preferable scheme of the laboratory disposable normal pressure/near normal pressure flexible reactor, the invention comprises the following steps: the functional layer structure is characterized in that the wall of the flexible reactor is sequentially divided into a material contact layer, a strength layer, an interlayer material contact layer, an interlayer material contact layer, a strength layer and an external surface layer from inside to outside;
each functional layer can be composed of one or more physical structure layers, and one physical structure layer can also have the functions of a plurality of functional layers. The reactor can be directly contacted with a heating body for heating, and can also be used in a sleeved mode. The multilayer structure of suit, the reactor need carry out high strength roll, extrude, rub and make material misce bene to the reaction process, when damaged appears in inside reactor layer, outside suit layer can play the effect of holding, buffering and protection.
The interlayer provides temperature regulation, isolation and protection effects for the reaction system through a storage medium, the medium is gas or liquid in a closed state or fluid which flows and circulates with the outside through a pipeline, the medium isolation and protection material in the interlayer can be inert gas, such as nitrogen, or material with the property opposite to that of the internal material, such as alkaline absorbent when the internal material is strong acid; the temperature adjusting material can be cooling water which circularly flows with the outside or heat conducting oil used for heating.
As a preferable scheme of the laboratory disposable normal pressure/near normal pressure flexible reactor, the invention comprises the following steps: the sealable interface is a chain clamping, a bone blowing self-sealing, a sealing port with a cover or a hot melting sealing port. The sealing port can be connected with a breather valve, gas generated in the reactor can be discharged through the breather valve, but outside gas cannot enter the reactor. And (3) hot melting and sealing, namely, after all reaction materials are added, the cavity is hot melted and sealed, the reactor is completely in a sealed state in the reaction process, and has no material circulation or exchange with the outside, so that the pollution of the outside materials and the loss of the inside materials are avoided, and the materials are taken out after the reaction is finished. Threaded interfaces may be designed for connecting connections between multi-toe structures or reactors. The sealing port convenient for feeding can be designed, if the sealing port is sealed by a rubber plug, the sealing performance of the sealing port is not damaged after the syringe is used for feeding. The number of sealable interfaces is at least 1.
As a preferable scheme of the laboratory disposable normal pressure/near normal pressure flexible reactor, the invention comprises the following steps: the cavity is flat, cylindrical and spherical, and has a regular shape or an irregular shape with a multi-toe structure. The multi-toe structure is marked with scales and can be used for quantitatively storing materials in advance, in the multi-step reaction, the materials stored in the multi-toe structure in advance can be directly added into the cavity by carrying out the next step of reaction after the reaction of each step is finished, and the phenomenon that air enters when materials are added every time, the anhydrous and oxygen-free environment is damaged, and the materials are polluted is avoided. The multi-toe structure and the cavity can be integrally connected and separated by a film material, the materials are added into the cavity by breaking the diaphragm, and the multi-toe structure can also be in threaded connection, so that the multi-toe structure is not limited to the connection mode, and the sealing property of the reactor is ensured.
As a preferable scheme of the laboratory disposable normal pressure/near normal pressure flexible reactor, the invention comprises the following steps: the wall of the container is completely transparent or is provided with a transparent window. The reaction condition in the reaction kettle can be conveniently observed through full transparency or arrangement of an observation window; fully opaque reactors are used in the maturation process.
As a preferred embodiment of the application of the disposable atmospheric/near atmospheric flexible reactor for the laboratory according to the present invention, wherein: the application is that high solid content materials, high viscosity materials and non-Newtonian fluid materials with the material liquid volume of milliliter or hundred milliliter grades are added into the flexible reactor, and the materials are stirred and mixed in a manual or mechanical rolling, extruding, kneading, vibrating and ultrasonic mode to react.
As a preferred embodiment of the application of the disposable atmospheric/near atmospheric flexible reactor for the laboratory according to the present invention, wherein: the actual liquid charge of the flexible reactor does not exceed 50% of the volume, preferably the liquid charge does not exceed 30% of the maximum volume; the total volume does not exceed 100L, preferably not 1L; leaving sufficient space for facilitating the migration and mixing of the reactor materials during mixing operations such as rolling, extrusion, kneading, vibration and the like.
As a preferred embodiment of the application of the disposable atmospheric/near atmospheric flexible reactor for the laboratory according to the present invention, wherein: the use pressure of the reactor is normal pressure or the internal and external pressure difference of the reactor is less than 10Kpa, a breathing valve can be arranged on the reactor to control the internal and external pressure difference of the reactor, and the phenomenon that the mixing operation such as rolling, extrusion, kneading, vibration and the like cannot be carried out on the reactor due to overlarge pressure is avoided.
As a preferred embodiment of the application of the disposable atmospheric/near atmospheric flexible reactor for the laboratory according to the present invention, wherein: after the reaction of the flexible reactor is finished and the product is detected to be qualified, the product can be stored in the reactor, and the reactor is used as a product package. Avoiding the waste of products and packages.
The invention has the beneficial effects that:
the normal pressure/near normal pressure flexible reactor is particularly suitable for reaction systems which are difficult to stir and mix conventionally, such as high-solid-content materials with small feed liquid volume (such as milliliter and hundred milliliter grades), high-viscosity materials, non-Newtonian fluid materials and the like, can use a manual tool or a motor tool to stir and mix materials by rolling, extruding, kneading and other forms, solves the problem of uneven mixing caused by material adhesion, wrapping, insufficient stirring and the like, and solves the problem of realizing laboratory mixing and reaction of corresponding materials.
The reactor is made of flexible materials, and is foldable, movable, retractable and convenient to use and store; the wall of the reactor can be fully transparent or provided with a transparent observation window, so that the state of the internal materials can be observed conveniently, and the reactor can also be fully opaque and is suitable for light-proof and radiation-proof reactions; the reactor can realize temperature control of materials in the reactor through an interlayer or an insulating layer or a heat transfer layer attached to the outside, light irradiation, microwave irradiation, heat conduction and other forms.
The reactor is a disposable container, does not need to be cleaned specially, avoids the generation of a large amount of cleaning waste liquid, can also avoid the influence of incomplete cleaning of appliances on the experiment, and has lower comprehensive cost; accurate mixed/reaction material metering can be realized, the reaction is strictly quantitative according to the sample requirement at every time, the product can be fully transferred from the reaction kettle by means of extrusion, scraping, replacement and the like to be effectively utilized, and the waste and the pollution of residual materials are greatly avoided.
The reactor is a closed reactor, can be completely isolated from the outside, and creates an oxygen-free and water-free environment.
The reactor disclosed by the invention is simple in reaction device, does not need to be connected with a complex functional device, can be operated on the reactor for feeding, mixing and temperature control, and can be directly placed on an experimental platform for operation.
The reactor is made of flexible material with toughness, is not easy to break and is friendly to operators.
The reactor can be used as a container, and samples/products qualified in detection after the reaction can be stored in the reactor, can be refrigerated, can be transported for a long distance, and can be used as product packages.
In general, the reactor is used as a disposable reactor and as a packaging container after completion of the reaction without transferring the reaction product, as compared with a conventional laboratory reactor. The reactor has the advantages of simple structure, convenient management, simple and convenient use, safety, environmental protection, low comprehensive cost and the like, and has obvious technical and use values.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The invention is suitable for mixing and reaction operation in a laboratory, and is suitable for reaction with special reaction environment requirements such as no water, no oxygen and the like; the method is suitable for the reaction of materials with special physical properties such as volatility, toxicity and flammability; the method is particularly suitable for reaction systems which are difficult to stir and mix conventionally, such as high-solid-content materials, high-viscosity materials, non-Newtonian fluid materials and the like with small material liquid volumes (such as milliliter and hundred milliliter grades). In specific application, a proper flexible reactor material and structure can be selected according to the characteristics of a real system and the regulation and control requirements of a reaction process.
Example 1:
the laboratory of this embodiment is with disposable ordinary pressure/nearly ordinary pressure flexible reactor is the cuboid, long 100mm, wide 75mm, and wall thickness is 0.15mm, and the volume is 0.5L, and the reactor wall only has one deck physical structure layer, and it has had material contact function concurrently, and anti extrusion, kneading, roll the function to and with external isolation protect function, the wall is all made by polyethylene film flexible material, and is fully transparent, presss from both sides the chain and seals.
The added materials are as follows: 1.0g of anhydrous magnesium chloride, 3ml of anhydrous ethanol and 10ml of methyl silicone oil, wherein the total volume of the materials is less than 50 percent of the volume of the reactor.
The method comprises the following specific operation steps: raw materials are weighed in a glove box (the glove box is dried in advance), the reactor can be placed on an electronic balance to be directly weighed, the reactor is sealed before feeding, the reactor is dried and is filled with no gas, 10ml of methyl silicone oil is accurately measured, 1.0g of anhydrous magnesium chloride is accurately measured, 3ml of anhydrous ethanol is accurately measured, the anhydrous magnesium chloride is sequentially added into the reactor, the reactor is sealed, the reactor is moved out of the glove box, the reactor is flatly placed on an experiment platform, the temperature is sensed by touching the reactor with hands to indicate that the reaction has occurred in the reactor, the materials in the reactor are well dispersed, the caking phenomenon does not exist, and no water enters a reactor system.
The materials in the reactor are mixed on the operation platform, and can be directly kneaded and extruded manually, or can be scraped on the outer wall of the reactor by means of tools, such as a scraping plate with a smooth surface, so that the liquid can be driven to a position with solids, or the solids can be driven to a place with the liquid, or the materials can be paved in the reactor, or scattered materials can be driven together to form a cluster. The materials in the reaction kettle gradually become molten along with the reaction, and finally become high-viscosity materials with extremely poor fluidity.
In the mixing operation process, the material mixing reaction condition in the reactor can be observed by naked eyes at any time, and the part which is not fully mixed can be kneaded, rolled and scraped at fixed points for mixing. The reactor can be moved to a microscope for magnifying observation in order to clearly observe the dispersion of the solid in the liquid.
When magnesium chloride powder cannot be seen in the reactor, and materials are completely changed into a milky molten state from a solid-liquid mixture without agglomeration, the product is characterized by XRD, the strong diffraction peak of anhydrous magnesium chloride disappears, which indicates that magnesium chloride and ethanol generate a complex, the ratio of magnesium alkoxide to magnesium alkoxide is 1.5-2.8, and also indicates that the reactor has good sealing property, and a good water-free environment is created. After the reaction is finished, the materials can be extruded for the next operation.
When materials are mixed, the reactor can be sleeved, damage of the outer layer reactor cannot affect the inner layer reactor, a buffer protection effect is achieved, the reactor with fibers and silk threads added in the film-coated material can be selected, and the mechanical strength of the film is enhanced.
Example 2:
the laboratory of this embodiment is with disposable ordinary pressure/nearly ordinary pressure flexible reactor is the polydactyly structure, and the wall thickness is 0.15mm, and the reaction cavity volume is 0.5L, and toe structure volume is 10ml, and the reactor wall only has one deck physical structure layer, has material contact function concurrently, anti extrusion, rub, roll the function to and keep apart the protect function with the external world. The reactor is completely transparent, is provided with a sealing port with a cover and is provided with a connecting port with a toe structure, and all reactor parts are made of fluorine-containing high polymer materials.
The added materials are as follows: 1.0g of anhydrous magnesium chloride, 3ml of anhydrous ethanol and 10ml of methyl silicone oil, wherein the total volume of the materials is less than 50 percent of the volume of the reactor.
The method comprises the following specific operation steps: weighing raw materials in a glove box (the glove box is dried in advance), placing a reactor cavity on an electronic balance, accurately weighing 1.0g of anhydrous magnesium chloride in the cavity, respectively weighing 3ml of anhydrous ethanol and 10ml of methyl silicone oil in a toe structure, sealing, removing a reactor from the glove box, flatly placing the reactor on an experiment platform, firstly connecting the toe structure filled with the methyl silicone oil with the reaction cavity, adding the materials into the reaction cavity, uniformly mixing the materials with the anhydrous magnesium chloride by rolling and rubbing, then connecting the toe structure filled with the anhydrous ethanol with the reaction cavity, adding the materials into the reaction cavity for reaction, touching the reactor by hands to feel that temperature indicates that the reaction has occurred in the reactor, directly observing that solid materials in the reactor are in a normal state and have no caking phenomenon, and indicating that no water enters the reactor system.
The materials in the reactor are mixed on the operation platform, and can be directly kneaded and extruded manually, or can be scraped on the outer wall of the reactor by means of tools, such as a scraping plate with a smooth surface, so that the liquid can be driven to a position with solids, or the solids can be driven to a place with the liquid, or the materials can be paved in the reactor, or scattered materials can be driven together to form a cluster. The materials in the reaction kettle gradually become molten along with the reaction, and finally become high-viscosity materials with extremely poor fluidity.
In the mixing operation process, the material mixing reaction condition in the reactor can be observed by naked eyes at any time, and the part which is not fully mixed can be kneaded, rolled and scraped at fixed points for mixing. The reactor can be moved to a microscope for magnifying observation in order to clearly observe the dispersion of the solid in the liquid.
When magnesium chloride powder cannot be seen in the reactor, materials are completely changed into milky white glue from a solid-liquid mixture and are free of agglomeration, the product is characterized by XRD, the strong diffraction peak of anhydrous magnesium chloride disappears, the fact that magnesium chloride and ethanol generate a complex is shown, the ratio of magnesium alkoxide to magnesium alkoxide is 1.5-2.8, the fact that the reactor is good in sealing performance is also shown, and a good water-free environment is created. After the reaction is finished, the materials can be extruded to be subjected to the next operation, or the materials can be stored in a reactor and taken out when being used.
Example 3:
the laboratory disposable normal pressure/near normal pressure flexible reactor of the embodiment is flat, the volume is 0.5L, the sandwich structure is adopted, and the flip cover is sealed; a toe structure connecting port is arranged, the connecting port is sealed by a flip cover and is provided with a spiral connector. The wall of the device is provided with a breather valve and an observation window. The wall of the vessel is sequentially from inside to outside: the surface of the material contact layer is coated with titanium, and the thickness of the material contact layer is 0.02 mm; the strength layer is made of fluorine-containing polymer material and has the thickness of 0.06 mm; the interlayer is used for circulating a solvent to control the temperature of the material; the strength layer is made of fluorine-containing polymer materials, fibers and silk threads are added to enhance mechanical strength, the strength layer is directly contacted with the outside, the thickness of the strength layer is 0.08mm, the two strength layers are directly contacted with the interlayer material, and an inlet and an outlet are formed in the wall surface of the device and connected with the interlayer. The toe structure is made of fluorine-containing polymer materials, and the volumes of the toe structure are respectively 10ml and 2 ml.
Adding materials: 1.5g of spherical magnesium chloride, 4.5ml of n-hexane (dehydrated by 4A molecular sieve), 10ml of titanium tetrachloride and 0.5ml of diisobutyl phthalate, wherein the total material volume is less than 50 percent of the volume of the reactor.
The method comprises the following specific operation steps: the raw materials were weighed in a glove box (glove box was dried beforehand), the reactor was placed on an electronic balance and 1.5g of anhydrous magnesium chloride was accurately weighed into the reactor, and 4.5ml of n-hexane (dehydrated with 4A molecular sieves) was accurately weighed into the reactor. 10ml of titanium tetrachloride and 0.5ml of diisobutyl phthalate were measured in the toe structure. Sealing the opening, removing the reactor from the glove box, and flatly placing the reactor on an experimental platform. The interlayer is connected with cooling liquid, the temperature is reduced to-10 to-15 ℃ and maintained for 15 minutes, then the titanium tetrachloride toe structure is connected with a reactor, materials are slowly added into a reaction kettle, the temperature is kept for 30 minutes at-10 to-15 ℃, the materials are mixed in a kneading mode, a folding mode and the like, and the cooling liquid is emptied after the temperature is kept, so that the temperature of the materials is raised to the normal temperature. And then connecting the diisobutyl phthalate toe structure with a reaction kettle, adding the material into the kettle, controlling the pressure in the reactor (the internal and external pressure difference is less than 10Kpa) through a breathing valve, and slowly heating the reaction kettle to 120 +/-2 ℃ by connecting the interlayer with heat conduction oil and keeping the temperature for 3 hours. And (4) evacuating the heat conducting oil after the heat preservation is finished, cooling the kettle to normal temperature, and washing for 2-3 times by using normal hexane.
The obtained product is characterized by XRD, and the ICP-MS is used for testing the contents of titanium and magnesium, so that the indexes such as apparent density, isotacticity and the like can meet the use requirements.
Titanium tetrachloride and spherical magnesium chloride are forbidden to contact with water, and both substances can react with water, so that the experiment fails. The reactor can create an anhydrous environment without introducing nitrogen for protection, the temperature of the reactor can be controlled by arranging the sandwich structure, the operation is simple, and the structural material of the functional layer is selected according to actual needs.
Example 4:
the laboratory disposable normal pressure/near normal pressure flexible reactor is a cuboid, 200mm in length and 150mm in width, 0.15mm in wall thickness and 1L in volume, has a multilayer structure, is provided with a chain-sandwiched seal, is sequentially provided with a material contact layer from inside to outside, and is made of an aluminum-coated composite film material; the strength layer is made of polyethylene materials, added fibers and silk threads are added to the polyethylene materials to enhance the mechanical strength; and the outer surface layer is made of polyethylene material.
The added materials are as follows: 200g of titanium dioxide, 10g of glass fiber, 100ml of deionized water, 3g of vanadium pentoxide, 0.8g of sodium carboxymethylcellulose and 8g of starch, wherein the volume of the total material is less than 50% of the volume of the reactor.
The method comprises the following specific operation steps: accurately weighing 200g of titanium dioxide, 10g of glass fiber and 100ml of deionized water in a reactor, flatly placing the reaction kettle on an experimental platform, scraping the outer wall of the reactor by using a scraping plate with a smooth surface or rolling the materials by using a grinding rod to mix the materials, and also directly manually kneading, extruding, folding and mixing the materials; after the materials are uniformly mixed, accurately weighing 3g of vanadium pentoxide, 0.8g of sodium carboxymethylcellulose and 8g of starch, adding the materials into a reaction kettle, scraping the materials on the outer wall of the reactor by using a scraper with a smooth surface or rolling the materials by using a grinding rod to mix the materials, or directly manually kneading, extruding, folding and mixing the materials, taking out the materials after the materials are detected to be qualified, and putting the materials into a ceramic forming machine for pressure forming.
The materials in the reactor are mixed on the operation platform, and can be directly kneaded and extruded manually, or can be scraped on the outer wall of the reactor by means of tools, such as a scraping plate with a smooth surface, so that the liquid can be driven to a position with solids, or the solids can be driven to a place with the liquid, or the materials can be paved in the reactor, or scattered materials can be driven together to form a cluster. The materials in the reaction kettle gradually become molten along with the reaction, and finally become high-viscosity materials with extremely poor fluidity.
In the mixing operation process, the material mixing reaction condition in the reactor can be observed by naked eyes at any time, and the part which is not fully mixed can be kneaded, rolled and scraped at fixed points for mixing. The reactor can be moved to a microscope for magnifying observation in order to clearly observe the dispersion of the solid in the liquid.
Example 5:
the laboratory disposable normal pressure/near normal pressure flexible reactor is a cuboid, 100mm in length and 75mm in width, 0.15mm in wall thickness and 0.5L in volume, has a multilayer structure, is sealed by a clamping chain, sequentially comprises a material contact layer from inside to outside, and is made of an aluminum-coated composite film material; the strength layer is made of silicon rubber materials, fibers and silk threads added with the silicon rubber materials to enhance the mechanical strength; and the outer surface layer is made of silicon rubber.
The added materials are as follows: 20g of titanium dioxide, 1g of glass fiber, 10ml of deionized water, 0.3g of vanadium pentoxide, 0.08g of sodium carboxymethyl cellulose and 0.8g of starch, wherein the volume of the total material is less than 50% of the volume of the reactor.
The method comprises the following specific operation steps: accurately weighing 20g of titanium dioxide, 1g of glass fiber and 10ml of deionized water in a reactor, flatly placing the reaction kettle on an experimental platform, scraping the outer wall of the reactor by using a scraping plate with a smooth surface or rolling the materials by using a grinding rod to mix the materials, and also directly manually kneading, extruding, folding and mixing the materials; after the materials are uniformly mixed, accurately weighing 0.3g of vanadium pentoxide, 0.08g of sodium carboxymethylcellulose and 0.8g of starch, adding the materials into a reaction kettle, scraping the materials on the outer wall of the reactor by using a scraper with a smooth surface or rolling the materials by using a grinding rod to mix the materials, or directly manually kneading, extruding, folding and mixing the materials, taking out the materials after the materials are qualified, and putting the materials into a ceramic forming machine for compression forming.
The materials in the reactor are mixed on the operation platform, and can be directly kneaded and extruded manually, or can be scraped on the outer wall of the reactor by means of tools, such as a scraping plate with a smooth surface, so that the liquid can be driven to a position with solids, or the solids can be driven to a place with the liquid, or the materials can be paved in the reactor, or scattered materials can be driven together to form a cluster. The materials in the reaction kettle gradually become molten along with the reaction, and finally become high-viscosity materials with extremely poor fluidity.
In the mixing operation process, the material mixing reaction condition in the reactor can be observed by naked eyes at any time, and the part which is not fully mixed can be kneaded, rolled and scraped at fixed points for mixing. The reactor can be moved to a microscope for magnifying observation in order to clearly observe the dispersion of the solid in the liquid.
The normal pressure/near normal pressure flexible reactor is particularly suitable for reaction systems which are difficult to stir and mix conventionally, such as high-solid-content materials with small feed liquid volume (such as milliliter and hundred milliliter grades), high-viscosity materials, non-Newtonian fluid materials and the like, can use a manual tool or a motor tool to stir and mix materials by rolling, extruding, kneading and other forms, solves the problem of uneven mixing caused by material adhesion, wrapping, insufficient stirring and the like, and solves the problem of realizing laboratory mixing and reaction of corresponding materials.
The reactor is made of flexible materials, and is foldable, movable, retractable and convenient to use and store; the wall of the reactor can be fully transparent or provided with a transparent observation window, so that the state of the internal materials can be observed conveniently, and the reactor can also be fully opaque and is suitable for light-proof and radiation-proof reactions; the reactor can realize temperature control of materials in the reactor through an interlayer or an insulating layer or a heat transfer layer attached to the outside, light irradiation, microwave irradiation, heat conduction and other forms.
The reactor is a disposable container, does not need to be cleaned specially, avoids the generation of a large amount of cleaning waste liquid, can also avoid the influence of incomplete cleaning of appliances on the experiment, and has lower comprehensive cost; accurate mixed/reaction material metering can be realized, the reaction is strictly quantitative according to the sample requirement at every time, the product can be fully transferred from the reaction kettle by means of extrusion, scraping, replacement and the like to be effectively utilized, and the waste and the pollution of residual materials are greatly avoided.
The reactor is a closed reactor, can be completely isolated from the outside, and creates an oxygen-free and water-free environment.
The reactor disclosed by the invention is simple in reaction device, does not need to be connected with a complex functional device, can be operated on the reactor for feeding, mixing and temperature control, and can be directly placed on an experimental platform for operation.
The reactor is made of flexible material with toughness, is not easy to break and is friendly to operators.
The reactor can be used as a container, and samples/products qualified in detection after the reaction can be stored in the reactor, can be refrigerated, can be transported for a long distance, and can be used as product packages.
Generally, compared with a conventional reactor in a laboratory, the reactor serving as a disposable reactor has the advantages of simple structure, convenience in management, simplicity and convenience in use, safety, environmental friendliness, low comprehensive cost and the like, and has obvious technical and use values.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. The utility model provides a laboratory is with disposable ordinary pressure/nearly ordinary pressure flexible reactor which characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
the reactor is made of flexible materials, has a functional layer structure and a sealable interface, is in a cavity shape, and is used for reaction systems which are difficult to stir and mix conventionally, such as high-solid-content materials with feed liquid volume of milliliter and hundred milliliter grades, high-viscosity materials, non-Newtonian fluid materials and the like.
2. The laboratory disposable atmospheric/near atmospheric flexible reactor of claim 1, wherein: the flexible material is one or more of a flexible polymer film material, a metal film material and a composite film material, and comprises a silicon rubber, a fluorine-containing high polymer material, a polyolefin high polymer material and a multilayer composite film material coated with aluminum, copper and alloy;
the composite film material is a blended composite film or a laminated film composite of multiple layers of film materials, and the mechanical strength of the film is improved by adding fibers and silk threads into the film material.
3. The laboratory disposable atmospheric/near atmospheric flexible reactor of claim 1, wherein: the functional layer structure is characterized in that the wall of the flexible reactor is sequentially divided into a material contact layer, a strength layer, an interlayer material contact layer, an interlayer material contact layer, a strength layer and an external surface layer from inside to outside;
the interlayer provides temperature regulation, isolation and protection effects for the reaction system through a storage medium, and the medium is gas or liquid in a closed state or fluid which flows and circulates with the outside through a pipeline.
4. The laboratory disposable atmospheric/near atmospheric flexible reactor of claim 1, wherein: the sealable interfaces are chain clamping, bone blowing self-sealing, sealing ports with covers or sealing ports sealed by hot melting, and the number of the sealable interfaces is at least 1.
5. The laboratory disposable atmospheric/near atmospheric flexible reactor of claim 1, wherein: the cavity is flat, cylindrical and spherical, and has a regular shape or an irregular shape with a multi-toe structure.
6. The laboratory disposable atmospheric/near atmospheric flexible reactor of claim 1, wherein: the wall of the container is completely transparent or is provided with a transparent window.
7. The use of a disposable atmospheric/near atmospheric flexible reactor for a laboratory according to claims 1 to 6, wherein: the application is that high solid content materials, high viscosity materials and non-Newtonian fluid materials with the material liquid volume of milliliter or hundred milliliter grades are added into the flexible reactor, and the materials are stirred and mixed in a manual or mechanical rolling, extruding, kneading, vibrating and ultrasonic mode to react.
8. The use of claim 7, wherein: also comprises the following steps of (1) preparing,
the total volume of the flexible reactor is not more than 1L, and the actual liquid loading is not more than 50% of the volume.
9. The use of claim 7, wherein: also comprises the following steps of (1) preparing,
the reactor is used at normal pressure or the pressure difference between the inside and the outside of the reactor is less than 10 KPa.
10. The use of claim 7, wherein: also comprises the following steps of (1) preparing,
after the reaction of the flexible reactor is finished and the product is detected to be qualified, the product can be stored in the reactor, and the reactor is used as a product package.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4039580A1 (en) * | 1990-12-12 | 1992-06-17 | Boehringer Mannheim Gmbh | Reagent storage system for mixing non-storable components - contains liq. transfer device connected to discharge openings of dry reagent container and liq. reagent |
| US5494190A (en) * | 1994-12-29 | 1996-02-27 | Minnesota Mining And Manufacturing Company | Method and combination for dispensing two part sealing material |
| US20050078552A1 (en) * | 2003-10-14 | 2005-04-14 | Jean-Pascal Zambaux | Flexible mixing bag for mixing solids, liquids and gases |
-
2022
- 2022-01-04 CN CN202210002894.2A patent/CN114405425A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4039580A1 (en) * | 1990-12-12 | 1992-06-17 | Boehringer Mannheim Gmbh | Reagent storage system for mixing non-storable components - contains liq. transfer device connected to discharge openings of dry reagent container and liq. reagent |
| US5494190A (en) * | 1994-12-29 | 1996-02-27 | Minnesota Mining And Manufacturing Company | Method and combination for dispensing two part sealing material |
| US20050078552A1 (en) * | 2003-10-14 | 2005-04-14 | Jean-Pascal Zambaux | Flexible mixing bag for mixing solids, liquids and gases |
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