CN113264956A - Microwave-induced gas-phase synthesis method of methyl silicate - Google Patents
Microwave-induced gas-phase synthesis method of methyl silicate Download PDFInfo
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Abstract
A microwave-induced gas-phase synthesis method of methyl silicate comprises the following steps: firstly, preprocessing an inner grinder of the reaction equipment; secondly, adding silicon powder with a preset weight from a feeding port, conveying the silicon powder into a mixing cavity, and feeding the silicon powder into a mixing module; driving a rotating motor connected with the inner grinding part to enable the inner grinding part to rotate relative to the outer grinding part; fourthly, conveying the ground particles into a pretreatment cavity for pretreatment; fifthly, conveying the pretreated materials into a reaction cavity for microwave-induced gas-phase synthesis of methyl silicate; and sixthly, collecting the gas-phase product and condensing to obtain the methyl silicate.
Description
Technical Field
The invention relates to the field of chemical synthesis, in particular to a microwave-induced gas-phase synthesis method of methyl silicate.
Background
Methyl silicate generally refers to tetramethoxysilane, which is mainly used in the fields of silicone synthesis, heat-resistant paints and adhesives. The methyl silicate is widely used in industries such as industrial casting, liquid adhesives, municipal construction engineering, various vehicles, motor turbines, precision instruments, military manufacturing, microelectronic components and dies manufacturing and the like. Therefore, the methyl silicate compound can be widely applied to various industries as a high polymer material with good performance and high use value. With the development of chemical industry, the demand for methyl silicate compounds is very strong.
The synthesis method of the methyl silicate generally comprises the following steps: 1) the silicon tetrachloride method is characterized in that silicon tetrachloride and methanol directly react, and methyl silicate with higher purity is obtained through a further rectification purification method. However, the method has high raw material consumption and long production period. The product quality is unstable, more neutralizing agent is consumed for neutralization, the cost is increased, and the environmental pollution is great. 2) The direct method is a method in which silicon powder and methanol are directly reacted to produce methyl silicate. The direct method has the advantages of high atom utilization rate, environmental protection and easy separation of products due to no generation of byproducts such as hydrogen chloride and the like, and becomes a synthesis method of methyl silicate which is concerned at present. However, the direct method for preparing methyl silicate has the problems of low silicon powder conversion rate and low reaction rate. The prior art has already applied the microwave to assist the reaction and add Cu catalyst method in the direct method gas phase synthesis process, has relatively raised the speed and conversion rate of the reaction. However, the existing synthesis method has the improvement on the application of microwaves for assisting the reaction and the addition of a Cu catalyst, so that the conversion rate and the reaction rate of the silicon powder of the existing process for synthesizing methyl silicate by gas phase by the direct method are not yet satisfactory, and therefore, the conversion rate and the reaction rate of the silicon powder of the gas phase synthesis method for inducing methyl silicate by microwaves are required to be further improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: there is a need to further improve the silicon powder conversion rate and reaction rate of the microwave-induced methyl silicate gas-phase synthesis process.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a microwave-induced gas-phase synthesis method of methyl silicate comprises the following steps:
firstly, preprocessing an inner grinder of the reaction equipment;
secondly, adding silicon powder with a preset weight from a feeding port, conveying the silicon powder into a mixing cavity, and feeding the silicon powder into a mixing module;
driving a rotating motor connected with the inner grinding part to enable the inner grinding part to rotate relative to the outer grinding part;
fourthly, conveying the ground particles into a pretreatment cavity for pretreatment;
fifthly, conveying the pretreated materials into a reaction cavity for microwave-induced gas-phase synthesis of methyl silicate;
and sixthly, collecting the gas-phase product and condensing to obtain the methyl silicate.
Specifically, the inner grinder is pretreated by surface roughening and precleaning.
In particular, the surface roughening is achieved by a sand blasting process.
Specifically, the pre-cleaning includes plasma treatment.
Specifically, the plasma treatment is a hydrogen-containing plasma treatment.
Specifically, the gases used for the plasma treatment are argon and hydrogen.
Specifically, the ratio of argon to hydrogen is 4: 1.
specifically, the roughness of the grinding disc of the inner grinder is controlled to be 0.5-3mm after the inner grinder is pretreated.
The reaction equipment used by the microwave-induced methyl silicate gas-phase synthesis method comprises: the device comprises a feeding port, a mixing cavity, a gliding channel, a pretreatment cavity and a reaction cavity.
Specifically, the pretreatment cavity comprises a material bearing cavity, a material inlet positioned above the material bearing cavity and a material outlet positioned below the material bearing cavity; one side of the upper part of the material bearing cavity is provided with a hydrogen inlet, and the other side of the upper part of the material bearing cavity is provided with a hydrogen outlet.
The microwave-induced methyl silicate gas-phase synthesis method provided by the invention has the beneficial effects that: the conversion rate and the reaction rate of the silicon powder of the gas-phase synthesis method of microwave-induced methyl silicate are improved.
Drawings
Fig. 1 is a flow chart of a gas-phase synthesis method of microwave-induced methyl silicate provided by the invention.
Fig. 2 is a schematic structural diagram of a reaction apparatus used in the microwave-induced methyl silicate gas-phase synthesis method provided by the invention.
Fig. 3 is a schematic structural diagram of a reaction equipment pretreatment cavity used in the microwave-induced methyl silicate gas-phase synthesis method provided by the invention.
Fig. 4 is a schematic structural diagram of a mixing module of reaction equipment used in the gas-phase synthesis method of microwave-induced methyl silicate provided by the invention.
Detailed Description
The present invention will be described in further detail with reference to a method for the microwave-induced gas-phase synthesis of methyl silicate.
The present invention will now be described in more detail with reference to the accompanying drawings, in which preferred embodiments of the invention are shown, it being understood that one skilled in the art may modify the invention herein described while still achieving the beneficial results of the present invention. Accordingly, the following description should be construed as broadly as possible to those skilled in the art and not as limiting the invention.
In the interest of clarity, not all features of an actual implementation are described. In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail. It will of course be appreciated that in the development of any such actual embodiment, numerous implementation-specific details must be set forth in order to achieve the developer's specific goals.
In order to make the objects and features of the present invention more comprehensible, embodiments of the present invention are described in detail below with reference to the accompanying drawings. It is to be noted that the drawings are in a very simplified form and are intended to use non-precision ratios for the purpose of facilitating and clearly facilitating the description of the embodiments of the invention.
In order to more clearly describe the gas-phase synthesis method of microwave-induced methyl silicate provided by the present application, a reaction device used in the synthesis method is described first.
As shown in fig. 2, the reaction apparatus includes: the device comprises a feeding port 1, a mixing cavity 2, a gliding channel 3, a pretreatment cavity 4 and a reaction cavity 5. Wherein, pan feeding mouth 1 is installed in the top of mixing chamber 2 to have the diameter that reduces gradually towards mixing chamber 2 direction. The feed inlet 1 is used for receiving solid powder raw materials and conveying the raw materials into the mixing cavity 2. The addition of the Cu catalytic substance and the full mixing of the silicon powder and the Cu catalyst can be realized through the mixing in the mixing cavity 2. The reaction materials passing through the mixing cavity 2 enter a pretreatment cavity 4 for pretreatment through a gliding channel 3, and then enter a reaction cavity 5 for direct reaction to prepare methyl silicate, wherein a microwave transmitting device for applying microwaves is arranged around the outer wall of the reaction cavity 5; reactant methanol gas enters the reaction cavity 5 through the gas inlet pipe 6 of the reactor to participate in reaction; the methyl silicate after the reaction is subjected to subsequent necessary condensation and collection via a product discharge pipe 7.
As shown in fig. 3, the pre-treatment chamber 4 comprises a material carrying chamber 42, and a material inlet 41 located above the material carrying chamber 42 and a material outlet 43 located below the material carrying chamber 42. A hydrogen inlet 45 is arranged on one side of the upper part of the material bearing cavity 42, and a hydrogen outlet 44 is arranged on the other side of the upper part of the material bearing cavity 42, so that the flowing circulation of hydrogen is realized. Two sets of material bearing plates 47 connected to the inner wall of the material bearing cavity 42 through a pivotable electric shaft 48 are arranged in the middle of the material bearing cavity 42, when the material bearing plates 47 need to bear materials, the electric shaft 48 is controlled by an external control device to rotate, so that the material bearing plates 47 are in a horizontally extending position (solid line position in fig. 3), and when the material bearing plates 47 do not need to bear materials, the electric shaft 48 rotates, so that the material bearing plates 47 are in a downward opening state (dotted line position in fig. 3). At least one pair of stirring devices 46 is disposed above the flat extension position of the material bearing plate 47, and each stirring device has a rotary driving member 461, a rotary output shaft 462 of the rotary driving member, and a plurality of stirring blades 463 disposed on the rotary output shaft 462, so that when the material bearing plate 47 bears the material powder, the material powder can be sufficiently stirred, and the material powder can be sufficiently contacted with the pretreatment hydrogen.
As shown in fig. 4, the mixing chamber 2 is provided with a mixing module 21 and a protective gas circulation device. Wherein, protective gas circulating device includes: the gas cylinder (argon cylinder), the transmission pipeline, the gas pump, the flowmeter and other components are protected, so that gas protection is provided in the mixing process, and the probability of oxidation or passivation of the powder material is reduced. The mixing module 21 is arranged in the mixing cavity 2, and the mixing module 21 is directly and/or indirectly detachably and mechanically connected with the inner wall of the mixing cavity 2 through the outer edge or the bottom of the outer grinding part 211. The concrete connection mode can be bolt connection with the inner wall of the mixing cavity 2 through a connecting piece with a specific shape. The mixing module 21 includes an outer grinding part 211 and an inner grinding part 212.
The outer grinding part 211 includes two half cylinders having the same structure and forming an integral cylindrical structure. And the inner wall of the plate cylinder extends towards the direction of the circle center. After the two semi-cylinders are combined, a circular opening is formed in the center of the corresponding grinding sheet P combination.
The number of the polishing sheet P provided in the outer polishing section 211 is n, and n is preferably 5 to 8.
The material of the outer grinding part 211 is pure copper (purity is 4N), so that substances of other components are prevented from being added into the raw material powder in the grinding process. Preferably, the outer surface of the abrasive sheet P has a concave-convex structure. Thereby improving the polishing efficiency of the polishing sheet P and the addition efficiency of Cu substance.
The inner grinding portion 212 has a central rod 2121 and a plurality of disc-shaped grinding discs 2122 axially distributed along the central rod and concentric with the central rod, and the plurality of grinding discs 2122 are fixed on the central rod 2121 at predetermined intervals to form a string structure. The inner polishing portion 212 is made of pure copper (purity 4N). Thereby avoiding the addition of substances of other components to the raw material powder during the grinding process.
The polishing disk 2122 has a substantially disk-like shape, and a patterned shape is provided on a surface thereof, and specifically the patterned shape includes a macroscopic concave-convex pattern and a rough pattern on the concave-convex pattern. The concave-convex pattern is a main body shape portion of a patterned shape formed by a patterning method such as etching. The roughness pattern 2 on the concave-convex pattern is obtained by a roughening process such as sand blasting. When the powder passes through the grinding disk 2122 and the grinding disk P arranged at a proper interval, grinding is performed between the concave-convex structure of the grinding disk P and the patterned shape of the grinding disk 2122, the rough pattern on the surface of the patterned shape is subjected to a large stress in friction because of having a large number of tip protrusions, and the tip protrusions of the rough pattern are detached during the grinding process because the adhesion force of the rough pattern protrusions themselves is lowest in the entire system. Since the polishing disk 2122 and the polishing sheet P are made of pure copper, the above-mentioned sharp protrusions of the coarse pattern formed of pure copper fall off from the polishing disk 2122 during the polishing process and form fine particles, which are then subsequently polished and mixed with silicon powder to form a mixture of a small amount of Cu particles and Si particles having a more uniform composition.
The average roughness of the above-mentioned roughened pattern needs to be set at 0.5 to 3 mm. If the average roughness of the roughened pattern is less than 0.5mm, it is liable that the roughened pattern is ground flat prematurely during grinding, thereby reducing the amount of addition of Cu particles during later grinding, and if the average roughness of the roughened pattern is more than 3mm, it is liable that Cu particles of an appropriate size are hardly dropped from the roughened surface during grinding of the roughened pattern, resulting in insufficient addition of Cu particles, or Cu particles of an excessively large size are added to the reaction powder, resulting in insufficient dispersion of the catalyst distribution.
During use of the apparatus, the inner polishing portion 212 fits into the cylindrical structure formed by the combined outer polishing portions 211. The circular opening of the combined same-layer polishing pad P, the central rod 2121 and the combined outer polishing portion 211 are substantially coaxial.
And, the grinding discs 2122 and the grinding pieces P are arranged at intervals, and the number of the grinding discs 2122 is n +1, so that there can be one grinding piece P between every two grinding discs 2122 during grinding to ensure sufficient agitation and friction of the powder between the two grinding discs 2122.
Wherein, the interval setting rule between adjacent grinding sheet layers in the external grinding part is as follows:
wherein m represents the number of layers of the grinding sheets arranged from top to bottom in sequence, m is 1-n-1, and Hm～m+1The design interval between the M-th layer and the (M + 1) -th layer below the M-th layer is shown, k is a compensation constant and is 1.9-2.7, M is the maximum powder bearing weight designed by the grinding module 21, g is the gravity acceleration, R is the radius of a circle formed by the outer edge of the grinding sheet, T is the minimum rotation period designed by the inner grinding part, and muIs a friction coefficient of the abrasive sheet measured in advance.
The spacing arrangement rule between adjacent grinding disks in the internal grinding part is as follows:
wherein m represents the number of layers of the polishing sheet arranged from top to bottom, l is 1-n, and Dl～i+1The design distance between the first layer and the first +1 layer below the first layer is shown, q is a compensation constant and takes a value of 0.8-1.3, M is the maximum powder bearing weight designed by the grinding module 21, g is the gravity acceleration, r is the radius of a circle formed by the outer edge of the grinding disc, and T is the minimum rotation period designed by the inner grinding part.
The multi-layer grinding sheet and the grinding disc which are arranged according to the rule can ensure the grinding and Cu doping effects and reduce the powder blockage between the inner grinding part and the outer grinding part.
The inner grinding part 212 is driven by the rotating motor 217 to rotate, and under the action of gravity and centrifugal force caused by the rotation of the grinding discs 2122, the raw material powder gradually moves downwards through the gaps between the grinding discs 2122 and the grinding sheets P, is ground by the grinding discs 2122 and the grinding sheets P while moving downwards, finally flows out of the housing part C through the opening 214 on the bottom surface of the housing part, and flows out of the mixing module 21 and the mixing chamber 2 through the hollow opening of the fixing frame 216. The opening 214 may be further provided with a valve or other device for controlling the opening and closing, so as to control the time for grinding the powder in the grinding module 21.
The end of the central rod 2121 of the inner grinder 212, on which the grinding disk 2122 is not mounted, is connected to a rotating motor 217, and the rotating motor drives the central rod 2121 and the grinding disk 2122 to perform a rotating motion around the axis thereof. The upper top surface of the rotating electric machine 217 is fixedly attached (welded, riveted) to the bottom surface of a fixed frame 216. Central rod 2121 rotates from the center of fixed frame 216 and is fixed by a bearing or other pivotally connected component to maintain central rod 2121 in normal rotation. The fixed frame 216 further comprises a supporting portion and a hollow portion, wherein the supporting portion is used for supporting the telescopic rod 215 and the outer grinding portion 211; the hollow part is used for enabling the ground powder to pass through.
The upper surface of the rotating electric machine 217 is fixedly connected (welded, riveted) to the bottom surface of the fixed frame 216 near the center of the ring shape.
With the above arrangement, the outer grinder 211 is detachably and fixedly connected to the inner wall of the mixing chamber 2, that is, the outer grinder 211 is fixed relative to the mixing chamber 2. The inner grinder 212 is fixed to the fixing frame 216 in the vertical and horizontal directions by a rotary motor 217 fixedly connected below the center rod 2121, and only a predetermined axis can be rotated. That is, the position of inner grinder 212 is substantially fixed relative to fixed frame 216. The fixed frame 216 is connected with the outer grinder 211 through at least two telescopic rods 215 in an adjustable way, so that the relative positions of the outer grinder 211 and the inner grinder 212 in the vertical direction can be adjusted indirectly.
Example 1
Based on the reaction equipment, the application also provides a microwave-induced gas-phase synthesis method of methyl silicate, which comprises the following steps:
in a first step, the inner grinder 212 of the reaction apparatus described above is surface roughened and precleaned.
The method specifically comprises the following steps: according to a specific cycle, for example: before grinding or after grinding for a specific number of times, inner grinder 212 is detached. Firstly, the inner grinder 212 is sandblasted, and the roughness of the grinding disc 2122 of the inner grinding part 212 is controlled to be 4-5mm after sandblasting; the hydrogen plasma treatment is performed on the inner polishing portion 212 subjected to the sandblasting, and specifically includes: the inner grinding part 212 is placed in a vacuum plasma processing chamber, plasma processing is carried out under the conditions of vacuum degree of 10-3, Ar: H2 being 4:1, power being 2KW and processing time being 5 minutes, after the plasma processing, the roughness of the grinding disc 2122 is controlled to be 0.5-3mm, and then the inner grinding part 212 is arranged in the grinding module 21 for standby.
And secondly, adding silicon powder with a preset weight from a feeding port, conveying the silicon powder into a mixing cavity, and feeding the silicon powder into a mixing module.
Specifically, before the silicon powder is conveyed into the mixing cavity, the protective gas circulation device is started, the protective gas Ar gas is introduced into the mixing cavity, the mixing cavity is cleaned, and preferably, 3-5 times of Ar gas inflation-exhaust circulation can be performed on the mixing cavity through the gas conveying and exhausting device. After the protective gas purge, the silicon powder feedstock was transported into the compounding chamber, ready for milling and Cu catalyst addition.
In the third step, the rotating motor 217 connected to the inner polishing section 212 is driven, so that the inner polishing section 212 rotates relative to the outer polishing section 211.
Specifically, the telescopic rod 215 is driven to extend and retract so that the distance between the polishing pad and the polishing disc is equal. The rotation speed of the polishing part is controlled as follows:
wherein, omega is the rotation angular velocity, M' is the weight of the silicon powder added actually, R is the radius of the circle formed by the outer edge of the grinding sheet; theta is the average particle size of the added silicon powder. The grinding time is controlled to be 5-10 minutes, and the addition amount of Cu is reasonably controlled by controlling the distance between the grinding parts, the grinding rotation speed and the grinding time. The silicon powder added with the Cu particles mixed in the above way has proper particle size, addition amount and dispersibility.
And fourthly, conveying the ground particles into a pretreatment cavity for pretreatment.
Specifically, set up the material loading board into horizontal extension state after, carry the material powder and get into preliminary treatment chamber 4, let in hydrogen to preliminary treatment chamber 4 simultaneously, the flow of hydrogen is according to the total amount of silicon powder, and control is at 0.3sccm per gram silicon, starts agitating unit 46 intensive mixing powder simultaneously. The pretreatment step can not only ensure that the surface of small particle Cu which is easy to be oxidized generates reduction reaction and keeps the purity of Cu, but also can form H-dangling bonds on the surface of Si particles, thereby being beneficial to the subsequent further reaction with methanol.
And fifthly, conveying the pretreated materials into a reaction cavity for microwave-induced gas-phase synthesis of methyl silicate.
The specific reaction parameters are that the temperature of methanol entering the reactor is controlled to be 80-130 ℃; the frequency of the microwave is 2450 MHz; the power density of the microwave is controlled to be 500-2000w/kg silicon powder based on the silicon powder in the reactor; the reaction time is controlled to be 20-30 minutes.
And sixthly, collecting the gas-phase product and condensing to obtain the methyl silicate.
Effect test
The collected condensate was sampled for gas chromatography. The gas chromatography model used in the experiment is GC9890A, the model of the adopted chromatographic column is SE-30, the operation conditions are 0.3MPa of hydrogen pressure and 0.5MPa of steam (carrier gas) pressure, the temperature is raised by a program, the initial temperature is 50 ℃, the temperature is kept for 10 minutes, the temperature raising rate is 35 ℃/min, the final temperature is 200 ℃, the temperature is kept for 15 minutes, the temperature of a sample injector is 250 ℃, and the temperature of a detector is 280 ℃. The content of methyl silicate was measured.
The experimental data are as follows:
it can be seen that the gas-phase synthesis method of microwave-induced methyl silicate provided by the application improves the silicon powder conversion rate and the reaction rate of the gas-phase synthesis method of microwave-induced methyl silicate.
The microwave-induced methyl silicate gas-phase synthesis method provided by the invention has the beneficial effects that: the conversion rate and the reaction rate of the silicon powder of the gas-phase synthesis method of microwave-induced methyl silicate are improved.
The foregoing shows and describes the general principles, essential features and advantages of the invention, which is, therefore, described only as an example of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but rather that the invention includes various equivalent changes and modifications without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A microwave-induced gas-phase synthesis method of methyl silicate is characterized in that: the method comprises the following steps:
firstly, preprocessing an inner grinder of the reaction equipment;
secondly, adding silicon powder with a preset weight from a feeding port, conveying the silicon powder into a mixing cavity, and feeding the silicon powder into a mixing module;
driving a rotating motor connected with the inner grinding part to enable the inner grinding part to rotate relative to the outer grinding part;
fourthly, conveying the ground particles into a pretreatment cavity for pretreatment;
fifthly, conveying the pretreated materials into a reaction cavity for microwave-induced gas-phase synthesis of methyl silicate;
and sixthly, collecting the gas-phase product and condensing to obtain the methyl silicate.
2. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 1, characterized in that: the inner grinder is pretreated including surface roughening and precleaning.
3. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 2, characterized in that: the surface roughening is achieved by a sand blasting process.
4. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 2, characterized in that: the pre-cleaning includes plasma treatment.
5. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 4, characterized in that: the plasma treatment is a hydrogen-containing plasma treatment.
6. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 5, characterized in that: the gases used for plasma treatment are argon and hydrogen.
7. The gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 6, characterized in that: the ratio of argon to hydrogen was 4: 1.
8. the gas-phase synthesis method of microwave-induced methyl silicate as claimed in claim 2, characterized in that: the roughness of the grinding disc of the inner grinder is controlled to be 0.5-3mm after the inner grinder is pretreated.
9. Reaction equipment for use in a process for the microwave-induced gas-phase synthesis of methyl silicate according to claims 1 to 8, characterized in that: the reaction apparatus comprises: the device comprises a feeding port, a mixing cavity, a gliding channel, a pretreatment cavity and a reaction cavity.
10. The reactor apparatus as set forth in claim 9, wherein: the pretreatment cavity comprises a material bearing cavity, a material inlet positioned above the material bearing cavity and a material outlet positioned below the material bearing cavity; one side of the upper part of the material bearing cavity is provided with a hydrogen inlet, and the other side of the upper part of the material bearing cavity is provided with a hydrogen outlet.
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