CN102853668A

CN102853668A - Experimental vacuum furnace

Info

Publication number: CN102853668A
Application number: CN2012103444255A
Authority: CN
Inventors: 熊利芝; 何则强; 刘志雄
Original assignee: Jishou University
Current assignee: Jishou University
Priority date: 2012-09-18
Filing date: 2012-09-18
Publication date: 2013-01-02

Abstract

The invention relates to an experimental vacuum furnace. The experimental vacuum furnace consists of an experimental furnace body, a temperature controller, a vacuum acquiring and detecting instrument and a gas charging system. A reactor in the experimental furnace body has high sealability, and a sampler and a condenser are arranged in the reactor. The sampler consists of an iron handle, a graphite crucible, a connecting rod and an extratubal magnet. During an experiment, a sample is sent to a designated area by using the magnetic force of the magnet to ensure that the sample reacts at a constant temperature and under a relatively constant pressure, and the reaction time can be accurately controlled. The condenser is arranged on a suitable part of the experimental furnace body to ensure that the steam of a hot volatile substance generated by reaction is fully condensed on a gathering device, and is prevented from being condensed on a narrow part of a pipeline to block the pipeline and influence the experiment. The experimental vacuum furnace is vacuum equipment which can maintain the constant temperature and the constant low pressure of a system and can accurately control the reaction time.

Description

A kind of experiment vacuum drying oven

Technical field

Vacuum equipment.

Background technology

Vacuum equipment commonly used generally is sample to be added in the crucible that fixes first, vacuumizes heating again, can keep the constant pressure of system in experimentation, but to the accurate aspect of the reaction temperature of reaction and the control of time relatively a little less than.Carrying out theoretical research, particularly the control of reaction time and reaction temperature there is requirement, such as the research of dynamics aspect, vacuum equipment commonly used can not satisfy the needs of this type of experiment.

Summary of the invention

This experiment is comprised of experiment body of heater, temperature controller, vacuum acquisition and detecting instrument and gas charging system with vacuum drying oven, it is characterized in that: 1) reactor in the experiment body of heater has good sealing, generally is quartz ampoule or high-purity corundum pipe.2) the sample presentation device in the reactor is comprised of iron handle, crucible, connecting rod and the outer magnet of pipe, and connecting rod connects crucible and irony handle, and it is the elongated plates that is processed by nonmagnetic substance high temperature resistant, that rigidity is arranged, and width is slightly less than the diameter of reactor.Magnet can be placed on crucible the needed position of experiment exactly to the magnetic force that the irony handle produces, to guarantee the constant of reaction temperature and to improve the accuracy in reaction time.3) condenser that condenser is comprised of several thinner graphite flakes in the reactor, graphite flake is circular, diameter is slightly less than the diameter of reactor, three apertures are respectively arranged on each graphite flake, a hole is at the graphite flake center, for the anchor stone ink sheet is used, be passage at its symmetrical locational two apertures, when the anchor stone ink sheet, make the passage on the two adjacent graphite flakes be " ten " word cross-like, and two adjacent graphite flakes distance about 5mm of being separated by had so both increased the condensation area of condensing zone, was conducive to again the abundant condensation of hot volatile materials, prevent hot volatile materials in the condensation of equipment narrow positions and blocking pipe affects the stove internal gas pressure; Condenser need be installed in suitable location in the reactor, to guarantee that hot volatile materials is than total condensation; Collect product and be convenient to analyzing and testing.4) the installation of TC is in the middle of experiment body of heater, and the bottom is near reactor, so that Accurate Determining and control reaction temperature.5) gas charging system is comprised of air accumulator and flowmeter, and flowmeter disposes the two-stage glass rotors, and the gas flow that is filled with in the stove is carried out the thickness adjusting, is beneficial to keep the required constant pressure of experiment.

In the process of experiment, the centre bit of experiment body of heater is equipped with a flat-temperature zone, and the size of flat-temperature zone is relevant with experimental temperature, and experimental temperature is higher, and the flat-temperature zone is less.The temperature at each position of reactor is the highest with the flat-temperature zone temperature, and left and right sides temperature constantly reduces centered by it, and the closer to fire door, temperature is lower.In order to improve the accuracy of experiment, reduce experimental error, for different reaction temperatures, need the different parts of reactor is carried out temperature measuring, to determine the particular location of flat-temperature zone, preheating zone and cooling zone.

This experiment has the following advantages with vacuum drying oven: 1, condenser is installed in reactor, prevents hot volatile materials condensation and blocking pipe in pipeline, be conducive to the constant pressure of maintenance system, also be conducive to product is carried out analyzing and testing simultaneously.2, utilize magnetic force, outside sealing system, carry out the pressure and temperature that the sample presentation operation does not affect system, be conducive to the constant pressure and temperature of the system that keeps.3, the temperature at each position differs in the reactor, (temperature is the highest at the body of heater middle part one flat-temperature zone, being convenient to sample reacts), from fire door distance more close to temperature lower, when flat-temperature zone temperature 750-1200 ℃, fire door place temperature is 250-400 ℃, the temperature of reactor end is not higher than 50 ℃, the flat-temperature zone that in reactor, has sample to react like this, preheating zone before the specimen reaction and the cooling zone behind the specimen reaction, be conducive to more accurately control " beginning " and " end " of reaction, reduce experimental error.4, gas charging system is equipped with the flowmeter that thickness is regulated, and is convenient to the accuracy controlling to system pressure.5, device structure is simple, and requirement on machining accuracy is not high, and cost is low.6, easy to operate, test completely at every turn, as long as open successively reactor, take out sample presentation device and condenser, from crucible, reaction residues is taken out, from condenser, take out product and get final product; If begin new experiment, can install equipment by opposite order.

Four, description of drawings:

Fig. 1 is the experimental provision schematic diagram, and 1 is experiment body of heater, the 2nd among the figure, temperature controller, the 3rd, vavuum pump, the 4th, air accumulator, the 5th, flowmeter, the 6th, pressure gauge, the 7th, connecting rod, the 8th, crucible, the 9th, iron handle, the 10th, magnet, the 11st, thermocouple, the 12nd, condenser, the 13rd, flat-temperature zone, the 14th, preheating zone, the 15th, zinc collecting region, the 16th, cooling zone, the 17th, reactor.

Five, the specific embodiment:

Below in conjunction with accompanying drawing this equipment is described in further detail.

Present embodiment comprises being comprised of experiment body of heater, temperature controller, vacuum acquisition and detecting instrument and gas charging system sees Fig. 1.Comprise experiment body of heater 1, temperature controller 2, vavuum pump 3, air accumulator 4, flowmeter 5, pressure gauge 6, connecting rod 7, crucible 8, iron handle 9, magnet 10, thermocouple 11, condenser 12, flat-temperature zone 13, preheating zone 14, zinc collecting region 15, cooling zone 16 and reactor 17.

Experiment is as follows with the vacuum drying oven experimental procedure:

As shown in Figure 1, open reactor 17, the iron handle 9, connecting rod 7 and the crucible 8 that link together in the taking-up sample presentation device, raw material is put into crucible 8, put it in the reactor, terminal near reactor, from the other end condenser is fixed on suitable location, the good seal reactor vacuumizes that to be heated to experiment temperature required again, and the regulation and control system pressure by flowmeter 5 is to testing required pressure, utilize the magnetic force mobile crucible of magnet, after sample delivered to preheating zone preheating certain hour, deliver to again the flat-temperature zone, at once be designated as reaction zero constantly.Passed through needed certain hour when reaction, utilized the magnetic force of magnet that sample is pushed into the low-temperature space cooling, reaction finishes, and stops simultaneously the experimental furnace heating.The weighing of reacted sample slag and analyzing and testing are taken off in blow-on after the experimental furnace cooling; And take off product weighing and analyzing and testing from condenser.

This experiment is that a kind of steady temperature, constant low pressure that can maintenance system can more accurately be controlled again the vacuum equipment in reaction time with vacuum drying oven, is suitable for the research experiment of thermodynamics and kinetics aspect under the vacuum.

Claims

1. an experiment is comprised of experiment body of heater (1), temperature controller (2), vacuum acquisition and detecting instrument (3 and 6) and gas charging system (4 and 5) with vacuum drying oven, it is characterized in that:

(1) reactor (17) in the experiment body of heater requires to have good sealing, generally is quartz ampoule or high-purity corundum pipe, and pipe range is about 3 times of body of heater;

(2)Sample presentation device in the reactor is comprised of iron handle (9), crucible (8), connecting rod (7) and the outer magnet (10) of pipe; Connecting rod (7) connects crucible (8) and irony handle (9), and it is the elongated plates that is processed by nonmagnetic substance high temperature resistant, that rigidity is arranged, and width is slightly less than the diameter of reactor; Magnet (10) can be placed on crucible the needed position of experiment exactly to the magnetic force that irony handle (9) produces;

(3)Condenser in the reactor (12) is comprised of several thinner graphite flakes, graphite flake is circular, diameter is slightly less than the diameter of reactor, three apertures are respectively arranged on each graphite flake, a hole is anchor stone ink sheet usefulness at the graphite flake center, is passage at its symmetrical locational two apertures, when the anchor stone ink sheet, make the passage on the two adjacent graphite flakes be " ten " word cross-like, and be separated by distance about 5mm of two adjacent graphite flakes; Condenser need be installed in suitable location in the reactor, to guarantee that hot volatile materials is than total condensation;

(4)Thermocouple (11) is installed in the middle of experiment body of heater, and the bottom is near reactor.

2. test vacuum drying oven claimed in claim 1, its gas charging system is comprised of air accumulator (4) and flowmeter (5), its feature is: flowmeter (5) disposes the two-stage glass rotors, and the gas flow that is filled with in the stove is carried out the thickness adjusting, to keep the required constant pressure of experiment.