CN2623327Y - High pressure reaction kettle for controlling water and solvent thermal reaction process - Google Patents
High pressure reaction kettle for controlling water and solvent thermal reaction process Download PDFInfo
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- CN2623327Y CN2623327Y CN 03218373 CN03218373U CN2623327Y CN 2623327 Y CN2623327 Y CN 2623327Y CN 03218373 CN03218373 CN 03218373 CN 03218373 U CN03218373 U CN 03218373U CN 2623327 Y CN2623327 Y CN 2623327Y
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- 238000010438 heat treatment Methods 0.000 claims abstract description 5
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Abstract
A high pressure reaction kettle for controlling water and solvent thermal reaction process belongs to the chemical equipment technical field, comprising a high pressure reaction kettle body, a kettle cover and a fastening piece, a heating furnace and a temperature controller, a magnetic force driving blender and a rotary speed controller, a pressure measuring device, a safety explosion-proof device, a valve and a pipeline which are used to sample and ventilate, and a set or a plurality of sets of inside retorts and\or outside retorts arranged inside and outside the reaction kettle. The high pressure reaction kettle of the utility model can effectively control the reaction process and crystallization, and the quality of the sample crystal produced is improved greatly compared with the prior art. In addition, by controlling the speed of the reaction process, the utility model also can conveniently control the granularity and distribution of the produced materials and can control the relative content of each phase in the materials of concomitant multiphase.
Description
(1) technical field
The utility model relates to a kind of improved autoclave structure, is specifically related to be used to control the autoclave of hydro-thermal and solvent thermal reaction process, belongs to technical field of chemical.
(2) background technology
In Chemical Manufacture and material preparation process, solvent process for thermosynthesizing all is the synthetic and preparation means of a kind of crucial material.Solvent process for thermosynthesizing has reaction condition gentleness, system good uniformity, course of reaction and is easy to outstanding advantages such as monitoring in real time and controllability are strong, in material preparation, particularly the relatively poor functional material of nano material and high temperatures is being brought into play irreplaceable huge effect in preparing.Specifically, solvent process for thermosynthesizing has the advantage of following uniqueness: 1, cost is low.Raw materials used chemical reagent commonly used or the industrial chemicals of being of this method, operation sequence is simple, helps reducing cost; 2, the various parameters in the course of reaction (temperature, pressure, concentration etc.) are easy to monitoring and control, and this makes us can easier research reaction mechanism, finds out the influence factor of most critical; 3, low in the pollution of the environment.Compare with other method, by recycling, can eliminate environmental pollution basically in the solvent process for thermosynthesizing solvent; 4, reaction system good uniformity.Liquid solvent is good pressure transmission mass transfer media, makes system temperature inside in the course of reaction, pressure, reactant concentration uniformity.This not only can guarantee the uniformity of product, and can prepare epigranular and controlled sub-micron even nano level powder; 5, the solvent heat condition can be prepared the metastable phase material that additive method is difficult to obtain down, significantly the scope of expanding function material.
Have these special advantages just because of solvent process for thermosynthesizing, this method is applied to contain in the preparation of oxygen system and non-oxide laminate material and has obtained immense success in recent years.Wherein hydrothermal condition down in batches the synthesis of molecular sieve technology industrialization and under hydrothermal condition the growing high quality quartz crystal be the exemplary of this method successful Application in actual production.Aspect the material scientific research, to be applied to prepare with boron nitride, gallium nitride be the success of the important nitride material of a class of representative to solvent thermal process in recent years, makes people see the dawn of low-cost this class material of preparation in enormous quantities.Along with the increase of the material system of studying, improved solvent process for thermosynthesizing such as pure hot method, the hot method of ammonia constantly occur, and the material category of preparation is also more and more.In this respect, existing in the world great deal of research results report, the work of a large amount of systems has been done by domestic Xu Ruren seminar.
For the research work that adapts to continuous development and the needs of Chemical Manufacture, people have carried out continuous improvement to used special equipment one autoclave of solvent process for thermosynthesizing, and its performance is improved constantly.Comprehensive, modern autoclave develops towards condition of work extramalization (for example operating temperature is up to 800-1000 ℃, and it is thousands of to atmospheric pressure up to ten thousand that operating pressure reaches), capacity maximization (being upgraded to hundreds of liters even nearly kilolitre from milli the earliest), functional diversities (stirring, change atmosphere, sampling and quick cooling etc. at any time) direction gradually.But solvent process for thermosynthesizing also has the shortcoming that is difficult to overcome: lack effective in-situ monitoring means, be difficult to realize preparing as required material etc. " orientation ".
(3) summary of the invention
The utility model provides a kind of autoclave that is used to control hydro-thermal and solvent thermal reaction process at the shortcoming of prior art, so that the controllability of intensified response process, and on big as far as possible degree, realize preparing as required material " orientation ".
The autoclave that is used to control hydro-thermal and solvent thermal reaction process of the present utility model comprises kettle, kettle cover and the securing member of autoclave, heating furnace and temperature controller, magnetically-actuated agitator and rotational speed governor, device for pressure measurement, the safety anti-explosive device, be used to valve, the pipeline of taking a sample and ventilating, installed a cover additional or overlapped built-in retort and/or external retort more in that reactor is inside and outside, with the controllability of intensified response process.
The measurement of the stirring system of main reaction still, sealing means, pressure and temperature and control system and safety anti-explosive device all adopt the prior art of existing stirring-type autoclave.
Above-mentioned built-in retort and/or external retort amount to 1～30.Built-in retort and external retort can be installed simultaneously, also can choose wherein a kind of as required, and the retort value volume and range of product of installation is determined according to concrete material preparation process need.
After the cover of built-in retort partly passes the kettle cover of main reaction still, be connected the whole main reaction still that is positioned at of retort tank body with the main reaction still with pad and clamp nut.
External retort and main reaction still be connected with side joint with on connect two kinds: lateral connected type is after external retort two ends respectively are connected a valve, is connected with perforate on the still sidewall by steel pipe and main reaction still kettle cover again.On connect formula external retort and be connected in main reaction still top by the perforate on the kettle cover, referring to Fig. 1 and Fig. 2.
Above-mentioned built-in retort comprise tank body, cover, valve rod, valve piece, seal member and with main reaction still attaching parts, by the closely contact or add that between cover and the main reaction kettle cover gasket seal is connected of the conical section on the cover and main reaction still kettle cover.The valve rod that is positioned at main reaction still outside adopts one group of sealing or organizes compound seal more, inwardly pushes filler by clamp nut and makes its distortion realize sealing.The composition mode of filler adopts the multistage composite sealing, and this method can be used for improving significantly the sealing of common needle-valve and ball valve equally.
Above-mentioned built-in retort can be divided into two kinds of needle valve and ball-valve types again, and structure chart is seen Fig. 3 and Fig. 7 respectively.
The switching of lower channel is mentioned and the realization of screw down valve piece by rotation valve rod on the built-in retort of above-mentioned needle valve, and in this process, valve rod and valve piece integral body are done and pumped; There are two seal valve pieces and valve rod to be connected as a single entity in the tank body, be respectively applied for two passages up and down on the sealed shell of tank, between valve rod and the valve piece pad is arranged, can freely rotate, the spill steel loop is that the screw thread on the valve rod reserves the space that moves up and down, valve piece position is fixed with clip by clamp or axle, also has the spring of control valve piece pressure on the valve piece.Structure is seen Fig. 3, Fig. 4, Fig. 5, Fig. 6.
The function of each critical piece is as follows:
(1) tank body 301: be mainly used in splendid attire solid or liquid reaction raw material, the transfer screw 310 of bottom (must or go up lower channel and open simultaneously this moment valve rod and the taking-up of valve piece) temporary sealing when packing reaction raw materials in tank body is used, after tank body assembling finished and closes up and down two passages simultaneously, this screw need take off.
(2) valve rod 302: can promote simultaneously or to pressing down two valve pieces 303 and 304, so that realize the opening and closing of built-in retort by rotation valve rod 302.
(3) valve piece 303 and 304: valve piece 303 and 304 is respectively applied for the last lower channel on the sealed shell of tank among Fig. 3, and they are connected as a single entity by valve rod 3, by moving the built-in retort of opening and closing simultaneously.Fluting on the valve piece 304 vertical sides 417 is so that liquid or solid material can flow out retort when lift valve piece upwards.
(4) seal member 308: this component exposed need be born the HTHP condition of work outside the main reaction still.It is by clamp nut 309 filler to be compressed to realize sealing (filling-material structure is seen Fig. 6, and it is the enlarged drawing of part in the circle among Fig. 5).Wherein, 601 and 604 is dull and stereotyped filler pads, and their effect is to produce distortion under the pressure of housing pin 309, seals the space between valve rod and the packing sheet, forms the auxiliary seal effect; 602 and 603 is taper filler pads, and they produce distortion under the co-extruded of housing pin 309 and stainless steel packing ring 503, to the distortion extruding of valve rod place, thereby plays main sealing function; The effect of stainless steel packing ring 504 mainly is that guiding packing ring 602 and 603 pushes to center (valve rod) behind pressurized; The effect of spill stainless steel coil 503 is to produce roof pressure power with clamp nut 309, reserves enough spaces that moves up and down for the screw thread on the valve rod simultaneously.
The switching of the built-in retort of described ball-valve type is to rotate simultaneously by valve rod and valve piece, changes the switching of the relative orientation realization response jar of perforate in the valve piece.In this process, have only valve rod and valve piece simultaneously around the rotation of valve rod axis, there is not motion up and down.There are two seal valve pieces to fixedly connected in the tank body with valve rod, be respectively applied for two passages up and down on the sealed shell of tank, valve piece position is fixed with clip by clamp or axle, the spring that also has control valve piece pressure on the valve piece, on two valve pieces one or more intercommunicating pores are arranged respectively, be used to open or close built-in retort.See Fig. 7, Fig. 8, Fig. 9, Figure 10.
The function of built-in each critical piece of retort of ball-valve type:
(1) tank body 701: the same with the built-in retort of needle valve, it is mainly used in splendid attire solid or liquid reaction raw material, and the transfer screw 706 of bottom is used for temporary sealing, and after tank body assembling finished and closes up and down two passages simultaneously, this screw need take off.
(2) cover 707: its main effect is an auxiliary seal, and by it tank body 701 is fixed on the kettle cover of main reaction still.After main reaction still kettle cover is passed in coupling part on the cover, be connected with the main reaction still with clamp nut 106 with pad 107.
(3) valve rod 702: the relative orientation that can change up and down two valve pieces 703 and 704 by rotation valve rod 702 simultaneously, perforate 804 and 806 on the valve piece is aimed at or depart from last lower channel 710 and 705 on the tank body, so that realize the opening and closing of built-in retort.The difference of built-in retort of ball-valve type and the built-in retort of needle valve is, the opening or close in the closed procedure of jar, valve rod 702 does not move up and down, and is convenient to seal member and seals better.
(4) valve piece 703 and 704: they are connected as a single entity by valve rod 702, by rotating the built-in retort of opening and closing simultaneously.Spring 803 and 808 on the valve rod is used to guarantee that lower valve block 703 and 704 compresses simultaneously, in order to avoid make course of reaction restive because of revealing in the still.Need to get the duct of one or more connection on the valve piece 703 and 704, when the duct on the valve piece and the passage on the tank body were in over against the position, retort was in open mode, and reaction raw materials can flow out retort by these ducts.
(5) seal member 708: by clamp nut 709 filler 708 is compressed and realize sealing (structure is seen Fig. 9 and 10).In Figure 10,1001 and 1004 is dull and stereotyped filler pads, and their effect is to produce distortion under the pressure of housing pin 709, seals the space between valve rod 702 and the packing sheet, has the auxiliary seal effect; 1002 and 1003 is taper filler pads, and they produce distortion under the extruding of housing pin 709, expands to valve rod 702 places, plays main sealing function; The effect of stainless steel packing ring 903 mainly is that guiding packing ring 1002 and 1003 pushes to center (valve rod) behind pressurized.
External retort of the present utility model sealing hammer is positioned on the step of tank body, and sealing ring is enclosed within the sealing hammer and goes up and compress downwards, and hold-down ring is enclosed within on the sealing hammer, realizes sealing that by sealing hammer, sealing ring and hold-down ring valve is connected with pipeline by screw rod.The external retort realizes sealing by sealing hammer, sealing ring and hold-down ring, and this contacts sealing firmly than common steel to steel and gasket type sealing use is more convenient, and sealing effectiveness is better.
In the external retort parts, the effect of sealing hammer 1105 is to support sealing ring 1107 and when the sealing ring compressive deformation, guide sealing ring 1107 to extruding all around, seals the slit between sealing hammer 1105 and the tank body 1101.Sealing ring 1107 is by morphotropism filler making preferably, and its produces distortion under the co-extruded of sealing hammer 1105 and hold-down ring 1106, a main sealing function.
Be connected with high voltage bearing pipeline between external retort and the main reaction still.Because whole external retort and connected system thereof be outside the main reaction still, external retort and connecting line, interface and valve require and can use in the operating temperature of 1-1500 atmospheric pressure and room temperature to 250 ℃, so that guarantee handling safety.
Connected mode between external retort 105 and the main reaction still 101 can be as shown in Figure 1, external retort 105 is positioned over the side of main reaction still 101, by perforate on the main reaction still kettle cover and the perforate on the sidewall, be connected with the main reaction still with screw or by valve.Also can be by mode shown in Figure 2, external retort 105 is positioned over the top of main reaction still 101, two connectors all are arranged on the kettle cover of main reaction still, couple together by screw or by valve and main reaction still.
Autoclave of the present utility model can be controlled course of reaction and crystallization process effectively, and the sample crystalline quality of preparation improves significantly than prior art.In addition,, the granularity and the distribution thereof of prepared material can also be controlled easily, and the relative amount of each thing phase in the material of heterogeneous coexistence can be controlled by the control course of reaction speed of carrying out.Utilize the improved reactor of the utility model, can improve the productive rate of material effectively, reduce preparation cost significantly.
(4) description of drawings
Fig. 1 is the assembling schematic diagram of improved autoclave of the present utility model.Fig. 2 is the another kind assembling schematic diagram of improved autoclave of the present utility model.Wherein, 101 are the main reaction still, the 103rd, and heating electric furnace heating wire, the 102nd, agitator, the 104th, built-in retort, the 105th, external retort, the 107th, pad, the 106th, clamp nut, the 108th, valve.
Fig. 3 is the assembling schematic diagram of the built-in retort of needle valve.Wherein 301 is tank bodies, the 307th, and cover, the 302nd, valve rod is used to mention or depresses two valve pieces 303 and 304.Indicating 312 part requires inner wall surface to process a little tapering to improve sealing effectiveness.The 311st, the breach that mills out, clamping when tightening retort.
Fig. 4 is the assembly assumption diagram of the built-in retort of needle valve.403,409,410 and 416 is clamp, is used for fixing the position of valve piece and spring, and 404,408,411 and 415 is spring, is respectively applied for and compresses valve piece 303 and 304.406 and 413 is filler, and when compressing the valve piece downwards, pad 405 and 412 compresses two fillers respectively, prevents to reveal.Indicating 417 side among the figure needs fluting, so that reaction raw materials can spill out when opening retort.
Fig. 5 is the seal member figure of the built-in retort of needle valve.The 309th, clamp nut is used to compress filler 308 to realize sealing.
Fig. 6 is the part enlarged drawing in the circle among Fig. 5.Wherein 503 is spill steel loops, and main effect is when valve rod moves up and down, and reserves a space for screwed part, and in addition, it also pushes packing sheet 308 with clamp nut 309.601 and 604 is dull and stereotyped packing sheets, and they are out of shape under pressure and produce the auxiliary seal effect.602 and 603 is taper packing sheets, under pressure they or to center extruding, play main sealing function.504 is steel loop, and its cross section can be leg-of-mutton, also can be trapezoidal, and main effect is when tapered packing sheet 602 and 603 compressive deformations, guides them to push to the center, to improve sealing effectiveness.
Fig. 7 is the assembling schematic diagram of the built-in retort of ball-valve type.Wherein 701 is tank bodies, the 707th, and cover, the 702nd, valve rod is used to mention or depresses two valve pieces 703 and 704.710 and 705 is access openings of getting on the retort tank body.The 711st, the breach that mills out, clamping when tightening retort.The 708th, the seal member of retort is used for reaction system is isolated from the outside out.The 706th, the transfer screw rod is used for when filling with substance temporary sealing in retort, after the question response jar assembles fully, they need be taken off.
Fig. 8 is the assembly assumption diagram of the built-in retort of ball-valve type.Wherein, 804 and 806 is respectively the duct of getting on valve piece 703 and 704, and their effect is the last lower channel 710 and 705 that is used to open retort.802,805,807 and 809 is clamp, is used for fixing the position of valve piece and spring.803 and 808 is two springs, is respectively applied for and compresses valve piece 703 and 704.
Fig. 9 is the seal member figure of the built-in retort of ball-valve type.The 708th, filler, the 709th, clamp nut is used to compress filler to realize sealing.The 901st, screw thread is used for the location of valve rod 702, and 902 is the ball face sealing part, is used for the auxiliary seal of retort.
Figure 10 is the part enlarged drawing in the circle among Fig. 9.Wherein 1001 and 1004 is dull and stereotyped packing sheets, and they are out of shape under pressure and produce the auxiliary seal effect.1002 and 1003 is taper packing sheets, and they push to the center under pressure, plays main sealing function.903 is steel loop, and its cross section can be leg-of-mutton, also can be trapezoidal, and main effect is when tapered packing sheet 1002 and 1003 compressive deformations, guides them to center crimp, to improve sealing effectiveness.
Figure 11 is the structure chart of external retort.Wherein 1101 is tank bodies, the 1104th, and cover, the 1105th, sealing hammer.The 1108th, the breach that mills out, clamping when supplying to tighten retort.The 1107th, sealing ring, the 1106th, hold-down ring.Under the co-extruded of hold-down ring 1106 and sealing hammer 1105, sealing ring is to expanding all around, and the slit of blocking between sealing hammer 1105 and the tank body 1101 realizes sealing.
Figure 12 is the x-ray diffraction pattern of gallium phosphide nano material, (a) is the sample with common stirring-type reactor preparation, and sample (b) is the gallium phosphide nano material with the improved reactor preparation of the utility model.Under the situation of careful control reaction raw materials mixing velocity, the nanocrystalline crystalline perfection of gallium phosphide has obtained very big improvement.
(5) specific embodiment
Embodiment 1:
Structure such as Fig. 1, Fig. 3～5, shown in Figure 11, two built-in retort 104 of needle valve are installed along arranged in a straight line in the main reaction still, after their cover partly passes the kettle cover of main reaction still 101, be connected with the main reaction still with pad 107 and clamp nut 106, in both sides, main reaction still outside two external retort 105 are housed, after their two ends respectively connect a valve 108, be connected with perforate on the still sidewall with steel pipe and main reaction still kettle cover again.Control order, speed and beginning and the termination of course of reaction by the switching order of adjusting different retort.Among Fig. 3, built-in retort 301 is connected with cover 307 by screw thread, and inner two seal valve pieces 303 and 304 of installing of tank body 301 are respectively applied for two passages 306 up and down and 305 on the sealed shell of tank.Two seal valve pieces 303 and 304 usefulness valve rods 302 are connected as a single entity so that action simultaneously.Can freely rotate between valve rod 302 and valve piece 303 and 304.In Fig. 4, the effect of spill steel loop 402 is to reserve the space that moves up and down for the screw thread on the valve rod 302.The effect of conical surface part 401 is after built-in retort and main reaction still kettle cover fix, and the conical surface closely contacts to realize sealing with main reaction still kettle cover.In addition, in Fig. 4,403,409,410,416th, clamp or axle are used clip, are used for fixing the position of valve piece 303 and 304.405,407,412 and 414 is pad, is used to guarantee freely rotating between valve rod 302 and the valve piece 303,304.Spring 404,408,411 and 415 are used for the pressure on control valve piece 303 and 304, and realize the fine setting of two valve piece positions.Filler 406 and 413 is when the valve piece compresses downwards, the sealing usefulness between realization valve rod and the valve piece.The valve stem seal that is arranged in main reaction still outside in the built-in retort be by Fig. 5 clamp nut 309 inwardly extruding fillers 308 its distortion is realized.The composition mode of filler adopts the multistage composite sealing, sees Fig. 6.601,602,504,603,604 are combined as one group mutually in the seal member, can use one group, also can use many groups.This method can be improved the sealing of common needle-valve and ball valve significantly.External retort structure during use, is at first hammered into shape on 1105 steps that are installed in the tank body sealing as shown in figure 11, then sealing ring 1107 is enclosed within on the sealing hammer 1105 also to compress downwards again.Then, hold-down ring 1106 is enclosed within on the sealing hammer 1105 again, tightens cover 1104 at last.Because sealing ring 1107 is out of shape, thereby realize sealing to the external retort under the extruding of cover.Among Figure 11,1103 and 1109 is the screw rods that are used to be connected valve and pipeline, and 1108 is the breach that mills out, clamping when tightening retort.
Embodiment 2:
The built-in retort of ball-valve type is installed in structure such as Fig. 2, Fig. 7～10, shown in Figure 11 in the main reaction still, after the cover of the built-in retort 104 of ball-valve type partly passes the kettle cover of main reaction still 101, be connected with the main reaction still with pad 107 and clamp nut 106.Adorn 3 external retort in main reaction still outside, they evenly arrange above the main reaction still, after two ends respectively connect a valve 108, are connected with two perforates on the main reaction still kettle cover with steel pipe again.
Among Fig. 7, the built-in retort 701 of ball-valve type is connected with cover 707 by screw thread, and inner two seal valve pieces 703 and 704 of installing of tank body 701 are respectively applied for two passages 710 up and down and 705 on the sealed shell of tank.Two seal valve pieces 703 and 704 usefulness valve rods 702 are connected as a single entity so that rotate simultaneously.Can not relatively rotate between valve rod 702 and valve piece 703 and 704.In Fig. 8, the effect of conical surface part 801 is after built-in retort and main reaction still kettle cover fix, and the conical surface closely contacts to realize sealing with main reaction still kettle cover.In addition, in Fig. 8,802,805,807,809th, clamp or axle are used clip, are used for fixing the position of valve piece 703 and 704.Spring 803,808 is used for the pressure on control valve piece 703 and 704, and realizes the fine setting of two valve piece positions.804 and 806 is the intercommunicating pores on valve piece 703 and 704, is used to open or close built-in retort.
The valve stem seal that is arranged in main reaction still outside in the built-in retort of ball-valve type be by Fig. 9 clamp nut 709 inwardly extruding fillers 708 its distortion is realized.The composition mode of filler adopts the multistage composite sealing, sees Figure 10.1001,1002,903,1003,1004 are combined as one group mutually in the seal member, can use separately, also can organize to be used in combination more.
Embodiment 3:
As embodiment 1, different is that 1 built-in retort of needle valve and 1 built-in retort of ball-valve type are installed in the main reaction still, installs 1 external retort additional in main reaction still outside.
Embodiment 4
As embodiment 2, different is that 2 built-in retort of ball-valve type and 2 built-in retort of needle valve are installed in the main reaction still, installs six external retort additional in main reaction still outside.
Embodiment 5:
As embodiment 2, different is that 8 built-in retort of needle valve are installed in the main reaction still, installs 10 external retort additional in main reaction still outside.
Embodiment 6:
As embodiment 1, different is that 1 built-in retort of ball-valve type and 1 built-in retort of needle valve are installed in the main reaction still, installs 20 external retort additional in main reaction still outside.
Embodiment 7:
As embodiment 1, different is that 4 built-in retort of ball-valve type and 2 built-in retort of needle valve are installed in the main reaction still, does not install the external retort additional in main reaction still outside.
Embodiment 8:
As embodiment 2, different is that 3 built-in retort of needle valve are installed in the main reaction still, does not install the external retort additional in main reaction still outside.
Embodiment 9:
As embodiment 2, different is that 12 built-in retort of needle valve and 18 built-in retort of ball-valve type are installed in the main reaction still, does not install the external retort additional in main reaction still outside.
Embodiment 10:
As embodiment 1, different is not install built-in retort in the main reaction still additional, installs 4 external retort additional in main reaction still outside.
Embodiment 11:
As embodiment 1, different is not install built-in retort in the main reaction still additional, installs 16 external retort additional in main reaction still outside.
Embodiment 12:
As embodiment 1, different is not install built-in retort in the main reaction still additional, installs 30 external retort additional in main reaction still outside.
Embodiment 13:
As embodiment 2, different is that 30 built-in retort of needle valve are installed in the main reaction still, does not install the external retort additional in main reaction still outside.
Embodiment 14:
As embodiment 2, different is that 30 built-in retort of ball-valve type are installed in the main reaction still, does not install the external retort additional in main reaction still outside.
Embodiment 15:
As embodiment 1, different is to install 1 built-in retort of needle valve and 3 built-in retort of ball-valve type in the main reaction still additional, installs 3 external retort additional in main reaction still outside.
Embodiment 16:
As embodiment 1, different is to adorn 1 built-in retort of ball-valve type in the main reaction still, adorns 1 external retort in main reaction still outside.
In order to further specify the effect of improved autoclave of the present utility model, synthesized the gallium phosphide nano material with existing common stirring-type autoclave and the improved autoclave of the utility model respectively, reaction raw materials is gallium trichloride and sodium phosphide, and solvent is the benzene through the distillation and the deoxygenation that dewaters.
In common stirring-type autoclave, at first add benzene, again to the gallium trichloride that wherein adds 0.5 mole.Stir a little make the gallium trichloride dissolving after, add 0.6 mole sodium phosphide again, adding a certain amount of benzene at last again, to make filling rate be 80%.Behind the air in the high pure nitrogen eliminating reactor, the envelope still.The temperature of reactor is brought up to 120 ℃ of constant temperature 5 hours, stir so that 350-400 rev/min speed is lasting simultaneously, finish up to reaction.After product used benzene and deionized water suction filtration 3-5 time respectively, the vacuum drying of gained powder promptly got the gallium phosphide nano material.Its x-ray diffraction pattern is seen Figure 12 (a).
As a comparison, we utilize improved autoclave of the present utility model to prepare the gallium phosphide nano material.At first in the main reaction still, add benzene, again to the sodium phosphide that wherein adds 0.6 mole.After stirring a little, add a certain amount of benzene and make filling rate reach 80%; 0.5 mole gallium trichloride is dissolved in 50 milliliters of benzene, again the benzole soln of gallium trichloride is joined in the built-in retort (also can use the external retort), be installed in the main reaction still after built-in retort is sealed.Behind the air in the high pure nitrogen eliminating reactor, the envelope still.After the temperature of reactor brought up to 120 ℃, open the last lower channel of retort slightly, the benzole soln that makes gallium trichloride lentamente with the sodium phosphide hybrid reaction.120 ℃ of constant temperature 5 hours, continue to stir with 350-400 rev/min speed simultaneously, finish up to reaction.After product used benzene and deionized water suction filtration 3-5 time respectively, the vacuum drying of gained powder promptly got the gallium phosphide nano material.Its x-ray diffraction pattern is seen Figure 12 (b).
Clearly, the X-ray diffraction peak of sample is sharp and strong among Figure 12 (b), among Figure 12 (a) the X-ray diffraction peak of sample then wide and a little less than.This explanation utilizes improved autoclave of the present utility model can control course of reaction and crystallization process effectively, and the sample crystalline quality of preparation is more much better than commonsense method.
Claims (9)
1. be used to control the autoclave of hydro-thermal and solvent thermal reaction process, the kettle, kettle cover and the securing member that comprise autoclave, heating furnace and temperature controller, magnetically-actuated agitator and rotational speed governor, device for pressure measurement, the safety anti-explosive device is used to valve, the pipeline of taking a sample and ventilating, it is characterized in that, installed a cover additional or overlapped built-in retort and/or external retort more in that reactor is inside and outside.
2. the autoclave that is used to control hydro-thermal and solvent thermal reaction process as claimed in claim 1 is characterized in that the quantity of described built-in retort and/or external retort is respectively 1～30.
3. the autoclave that is used to control hydro-thermal and solvent thermal reaction process as claimed in claim 1, it is characterized in that, described built-in retort is divided into two kinds of needle valve and ball-valve types, comprise tank body, cover, valve rod, valve piece, seal member and with main reaction still attaching parts, by the closely contact or add that between cover and the main reaction kettle cover gasket seal is connected of the conical section on the cover and main reaction still kettle cover.
4. as claim 1 or the 3 described autoclaves that are used to control hydro-thermal and solvent thermal reaction process, it is characterized in that, the valve stem seal mode that described built-in retort is positioned at main reaction still outside adopts one group of sealing or organizes the sealed composite sealing more, inwardly pushes filler by clamp nut its distortion is realized.
5. as claim 1 or the 3 described autoclaves that are used to control hydro-thermal and solvent thermal reaction process, it is characterized in that, the switching of lower channel is mentioned with the screw down valve piece by rotation valve rod and is realized on the built-in retort of described needle valve, in this process, valve rod and valve piece integral body are done and are pumped; There are two seal valve pieces and valve rod to be connected as a single entity in the tank body, two seal valve pieces are respectively applied for two passages up and down on the sealed shell of tank, between valve rod and the valve piece pad is arranged, seal valve piece and valve rod can freely rotate, the spill steel loop is that the screw thread on the valve rod reserves the space that moves up and down, valve piece position is fixed with clip by clamp or axle, also has the spring of control valve piece pressure on the valve piece.
6. as claim 1 or the 3 described autoclaves that are used to control hydro-thermal and solvent thermal reaction process, it is characterized in that, the switching of the built-in retort of described ball-valve type is to rotate simultaneously by valve rod and valve piece, changes the switching of the relative orientation realization response jar of perforate in the valve piece.In this process, have only valve rod and valve piece simultaneously around the rotation of valve rod axis, there is not motion up and down.There are two seal valve pieces to fixedly connected in the tank body with valve rod, be respectively applied for two passages up and down on the sealed shell of tank, valve piece position is fixed with clip by clamp or axle, also has the spring of control valve piece pressure on the valve piece, on two valve pieces an intercommunicating pore is arranged respectively, be used to open or close built-in retort.
7. the autoclave that is used to control hydro-thermal and solvent thermal reaction process as claimed in claim 1, it is characterized in that, between described external retort and the main reaction still be connected with side joint with on connect two kinds: lateral connected type is after external retort two ends respectively are connected a valve, is connected with perforate on the still sidewall by steel pipe and main reaction still kettle cover again.On connect formula external retort and be connected in main reaction still top by the perforate on the kettle cover.
8. as claim 1 or the 7 described autoclaves that are used to control hydro-thermal and solvent thermal reaction process, it is characterized in that, described external retort by tank body, cover, sealing hammer, sealing ring, hold-down ring and up and down two valves form, the sealing hammer is positioned on the step of tank body, sealing ring is enclosed within the sealing hammer and goes up and compress downwards, hold-down ring is enclosed within on the sealing hammer, realizes sealing by sealing hammer, sealing ring and hold-down ring, and valve is connected with pipeline by screw rod.
9. as claim 1 or the 7 described autoclaves that are used to control hydro-thermal and solvent thermal reaction process, it is characterized in that, be communicated with high voltage bearing pipeline between described external retort and the main reaction still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03218373 CN2623327Y (en) | 2003-06-27 | 2003-06-27 | High pressure reaction kettle for controlling water and solvent thermal reaction process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03218373 CN2623327Y (en) | 2003-06-27 | 2003-06-27 | High pressure reaction kettle for controlling water and solvent thermal reaction process |
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| CN2623327Y true CN2623327Y (en) | 2004-07-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952744A (en) * | 2011-08-31 | 2013-03-06 | 中国科学院过程工程研究所 | Biomass hydrothermal pretreatment reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952744A (en) * | 2011-08-31 | 2013-03-06 | 中国科学院过程工程研究所 | Biomass hydrothermal pretreatment reactor |
| CN102952744B (en) * | 2011-08-31 | 2014-07-30 | 中国科学院过程工程研究所 | Biomass hydrothermal pretreatment reactor |
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