CN114213445B - Method for returning organosilicon contact body to bed - Google Patents
Method for returning organosilicon contact body to bed Download PDFInfo
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- CN114213445B CN114213445B CN202111476986.6A CN202111476986A CN114213445B CN 114213445 B CN114213445 B CN 114213445B CN 202111476986 A CN202111476986 A CN 202111476986A CN 114213445 B CN114213445 B CN 114213445B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/16—Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/584—Recycling of catalysts
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Abstract
The application provides a method for returning an organosilicon contact body to a bed, which comprises the following steps: mixing silicon powder and copper catalyst in a contact tank to form a first contact, inputting the first contact into a fluidized bed reactor, introducing methyl chloride gas into the fluidized bed reactor, reacting the silicon powder and the methyl chloride under the action of the copper catalyst to generate a crude methylchlorosilane, separating the crude methylchlorosilane by a cyclone separator, introducing the obtained methylchlorosilane into a impurity removal process, directly inputting a second contact separated by the first cyclone separator into the fluidized bed reactor for reaction, inputting a third contact and a fourth contact separated by the second cyclone separator and the third cyclone separator into a fine powder activation bed for activation, introducing nitrogen into the fine powder activation bed, removing carbon impurities from the third contact and the fourth contact by the nitrogen, and collecting and inputting the carbon impurities into the fine powder tank for reuse. The application removes carbon on the surface of the contact body, improves the reactivity and the utilization rate of silicon powder, and simultaneously improves the yield of methyl chlorosilane.
Description
Technical Field
The application relates to the technical field of organic silicon, in particular to a method for returning an organic silicon contact body to a bed.
Background
Organosilicon is widely used as a new chemical material because of its advantages such as high and low temperature resistance and corrosion resistance. Methylchlorosilanes are the most important monomers for preparing organosilicon polymers, wherein the highest amount of dimethyldichlorosilane is about 90% of methylchlorosilanes.
In the production process of the organic silicon, silicon powder and chloromethane are used as production raw materials, and copper is used as a catalyst to promote the synthesis of organic silicon monomers such as dimethyl dichlorosilane. In the reaction for producing the dimethyl dichlorosilane, silicon powder and a copper catalyst are mixed to form an active contact body, and along with the extension of the reaction time, sediment on the surface of the contact body is more and more, and the silicon copper contact body is polluted mainly because carbon-containing impurities are accumulated in the reaction process, so that the activity of the contact body is reduced, and the synthesis rate of the dimethyl dichlorosilane is reduced.
In the prior art, after a contact body is separated by a cyclone separator, the contact body directly returns to a bed to participate in reaction, carbon on the surface of the contact body cannot be effectively removed, so that the activation of the contact body is reduced, when impurities reach a certain degree, the contact body needs to be stopped for maintenance, a new reaction period can be started after the reactor is cleaned, the production efficiency of methyl chlorosilane is greatly influenced in the process, the production period is shortened, and the production cost of enterprises is increased. When the contact body is polluted seriously, the silicon powder cannot be returned to the bed for use, so that the utilization rate of the silicon powder is reduced, and meanwhile, the production efficiency of the methyl chlorosilane is also reduced.
Disclosure of Invention
The application provides a method for an organosilicon contact back-to-bed process, which is used for solving the problems of carbon deposition and activation performance reduction of the surface of the organosilicon contact.
The application provides a method for returning an organosilicon contact body to a bed, which comprises the following steps:
s1: mixing silicon powder and a copper catalyst in a contact tank to form a first contact, inputting the first contact into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable the silicon powder and the chloromethane to react under the action of the copper catalyst to generate a methylchlorosilane crude product.
S2: and sequentially inputting the methyl chlorosilane crude product into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, sequentially separating to obtain a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride, and enabling the methyl chlorosilane and the methyl chloride to enter a next impurity removing procedure.
S3: and directly conveying the second contact body separated by the primary cyclone separator to a fluidized bed reactor for reaction, and conveying the third contact body separated by the secondary cyclone separator and the fourth contact body separated by the tertiary cyclone separator to a fine powder activation bed for activation.
S4: and introducing nitrogen into the fine powder activation bed to activate the third contact body and the fourth contact body, and collecting the activated third contact body and fourth contact body in a fine powder tank and conveying the third contact body and fourth contact body to a fluidized bed reactor for recycling.
Optionally, the copper-based catalyst is one or more of cuprous oxide and cuprous chloride.
Optionally, the mass fraction of the copper-based catalyst in the first contact is 4-7%.
Alternatively, the temperature in the fluidized bed reactor is 280-310℃and the pressure is 0.28-0.31MPa.
Optionally, the fine powder activation bed is heated by heat conduction oil in a jacket, the temperature of the heat conduction oil is 240-260 ℃, the temperature in the fine powder activation bed is 100-120 ℃, and the pressure is 0.1-0.2MPa.
Optionally, the third contact body separated by the secondary cyclone separator and the fourth contact body separated by the tertiary cyclone separator are conveyed to a fine powder activation bed for activation, and the method comprises the following steps:
sampling and testing the particle sizes of the third contact body and the fourth contact body, and if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation.
Optionally, if the particle sizes of the third contact body and the fourth contact body are smaller than 30 μm, the third contact body and the fourth contact body are used as waste contact bodies to be subjected to directional conversion treatment through a contact body tank.
Optionally, the contact tank is further used for sending unreacted contact in the fluidized bed reactor into the contact tank when the fluidized bed reactor is stopped for maintenance or suddenly stopped when the fluidized bed reactor is in fault, and sending the contact in the contact tank into the fluidized bed reactor for reaction when the system resumes production and is started again.
Optionally, the flow rate of nitrogen in the fine powder activation bed is 1000Nm 3 /h。
Optionally, a filtering system is arranged behind the fine powder activation bed, and the filtering system is used for collecting and incinerating carbon impurities on the surfaces of the removed third contact body and the removed fourth contact body.
According to the method for preparing the organosilicon contact body back-to-bed process, methyl chlorosilane synthesized in the fluidized bed reactor is separated from the contact body through the cyclone separator, the obtained contact body is sent to the fine powder activation bed for impurity removal, carbon impurities deposited on the surface of the contact body are removed through nitrogen blowing, and then the contact body is re-transported to the fluidized bed reactor for reuse, so that the aim of impurity removal on the surface of the contact body is achieved, the utilization rate of silicon powder is improved, the production efficiency of the methyl chlorosilane is improved, and the production cost is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a method for returning an organosilicon contact body to a bed.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are also within the scope of the application.
Fig. 1 is a flowchart of a method for returning an organosilicon contact body to a bed, as shown in fig. 1, the method may include:
s1: and (3) stirring and mixing the silicon powder and the copper catalyst in a contact tank to form a first contact, inputting the first contact into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to react the silicon powder and the chloromethane under the action of the copper catalyst to generate a methylchlorosilane crude product.
Specifically, silicon powder and a copper catalyst are mixed in a contact tank to form a first contact with reactivity, the first contact is input into a fluidized bed reactor, and methyl chloride gas is introduced into the fluidized bed reactor at the same time, so that the silicon powder and the methyl chloride react under the action of the copper catalyst, the contact area of the silicon powder and the methyl chloride can be increased by the first contact which is uniformly mixed in advance in the contact tank, and meanwhile, the copper catalyst can better promote the reaction of the silicon powder and the methyl chloride to generate a methyl chlorosilane crude product.
S2: and sequentially inputting the methyl chlorosilane crude product into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, sequentially separating to obtain a second contact body, a third contact body, a fourth contact body and methyl chlorosilane, and enabling the methyl chlorosilane to enter a next impurity removing procedure.
Specifically, the crude methyl chlorosilane gas synthesized by the fluidized bed reactor is sequentially input into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, the crude methyl chlorosilane gas at the outlet of the fluidized bed reactor comprises methyl chlorosilane and chloromethane generated by reaction and a contact body carried along with the gas, gas-solid separation is carried out under the action of the cyclone separators, and the methyl chlorosilane and chloromethane obtained by separation are input into the next impurity removal procedure.
S3: and directly conveying the second contact body separated by the primary cyclone separator to a fluidized bed reactor for reaction, and conveying the third contact body separated by the secondary cyclone separator and the fourth contact body separated by the tertiary cyclone separator to a fine powder activation bed for activation.
Specifically, the second contact body separated by the first cyclone separator is directly conveyed to the fluidized bed reactor for recycling, because the contact body separated by the first cyclone separator is more in quantity and larger in particle size, the contact body has reactivity and can directly participate in reaction, and then the third contact body separated by the second cyclone separator and the fourth contact body separated by the third cyclone separator are conveyed to the fine powder activation bed for activation.
S4: and introducing nitrogen into the fine powder activation bed to activate the third contact body and the fourth contact body, and collecting the activated third contact body and fourth contact body in a fine powder tank and conveying the third contact body and fourth contact body to a fluidized bed reactor for recycling.
Specifically, nitrogen is introduced into a fine powder activation bed to remove impurities on the surfaces of a third contact body and a fourth contact body, the nitrogen has a certain flow velocity in the fine powder activation bed, the contact bodies have a fluid-like flowing state in the fine powder activation bed, silicon powder particles have a certain hardness, under the action of air flow, the contact body particles mutually collide and rub, carbon impurities deposited on the surface of the contact bodies fall off from the surface of the contact bodies, activated contact bodies are obtained, the carbon impurities on the surface of the contact bodies come from a small amount of carbon and carbon generated by thermal decomposition of chloromethane contained in silicon powder, and then the activated third contact body and the activated fourth contact body are collected in a fine powder tank and are conveyed to a fluidized bed reactor for recycling.
Optionally, the copper-based catalyst is one or more of cuprous oxide and cuprous chloride.
The copper catalyst has high activity and can promote the reaction of silicon powder and chloromethane.
Optionally, the mass fraction of the copper-based catalyst in the first contact is 4-7%.
When the silicon powder and the copper catalyst are mixed, the mass fraction of the copper catalyst in the contact body is 4-7%, the copper catalyst has high activity, and the reaction can be promoted by a small amount.
Alternatively, the temperature in the fluidized bed reactor is 280-310℃and the pressure is 0.28-0.31MPa.
Wherein, the temperature in the fluidized bed reactor is controlled to be 280-310 ℃, and the reaction rate of the main product of the dimethyl dichlorosilane is improved when the temperature is increased within the temperature range, but the continuous temperature increase reaction rate is in a descending trend, so that the control of the temperature to be 280-310 ℃ is beneficial to the generation of the main product of the dimethyl dichlorosilane. Proper pressurization in the fluidized bed reactor can lead to higher yield of the main product dimethyl dichlorosilane, but excessive pressure has less influence on the generated product and increases the production cost.
Optionally, a jacket is arranged outside the fine powder activation bed, the fine powder activation bed is heated by heat conduction oil in the jacket, the temperature of the heat conduction oil is 240-260 ℃, the temperature in the fine powder activation bed is 100-120 ℃, and the pressure is 0.1-0.2MPa. The method has the advantages that the yield of methylchlorosilanes can be improved by 2-3 percent after the contact is activated and returned to the bed in the contact activation process for 4-8 hours.
The third contact body and the fourth contact body are input into a fine powder activation bed, a jacket is arranged outside the fine powder activation bed, heat conduction oil is introduced into the jacket, the temperature of the heat conduction oil is controlled to be 240-260 ℃, the heat conduction oil is used as a heat conduction medium to heat the fine powder activation bed, the temperature in the fine powder activation bed is kept at 100-120 ℃, and meanwhile, the pressure is controlled to be 0.1-0.2MPa, so that carbon impurities on the surface of the contact body are beneficial to falling off from the surface of the contact body.
Optionally, the third contact body separated by the secondary cyclone separator and the fourth contact body separated by the tertiary cyclone separator are conveyed to a fine powder activation bed for activation, and the method comprises the following steps:
sampling and testing the particle sizes of the third contact body and the fourth contact body, and if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation.
Specifically, when the particle size of the third contact body and the fourth contact body is greater than or equal to 30 μm, silicon powder reacting with methyl chloride exists in the contact bodies, and the area of the silicon powder capable of participating in the reaction is reduced due to the coverage of deposited carbon impurities on the surfaces, so that the carbon impurities on the surfaces of the third contact body and the fourth contact body are required to be removed, the silicon powder with reactivity is exposed, and the silicon powder utilization rate is improved.
Optionally, if the particle sizes of the third contact body and the fourth contact body are smaller than 30 μm, the third contact body and the fourth contact body are used as waste contact bodies to be subjected to directional conversion treatment through a contact body tank.
Specifically, if the particle size of the third contact body and the fourth contact body is smaller than 30 μm, the agglomeration force among the particles is increased by the excessively fine silicon powder, the dispersibility is deteriorated, adverse effects on the heat dissipation of the system or the entrainment amount of the silicon powder along with the air flow is increased, and meanwhile, the impurity which is contained in the excessively fine contact body particles and affects the reaction of the silicon powder and the chloromethane is more, so that the reaction is not facilitated, and the third contact body and the fourth contact body are used as waste contact bodies to be subjected to directional conversion treatment through a contact body tank.
Optionally, the contact tank is further used for feeding the contact in the fluidized bed reactor into the contact tank when the fluidized bed reactor is stopped.
Specifically, the touch body tank is also used for sending unreacted touch bodies in the fluidized bed reactor into the touch body tank when the fluidized bed reactor is stopped for maintenance or the system needs emergency stopping when meeting faults, and sending the touch bodies in the touch body tank into the fluidized bed reactor for internal reaction when the system resumes the normal production cycle.
Optionally, the flow rate of nitrogen in the fine powder activation bed is 1000Nm 3 /h。
Specifically, nitrogen in the fine powder activation bed has a certain flow rate, so that the contact body has a fluid-like flowing state in the fine powder activation bed, carbon impurities on the surface of the contact body can be removed in the flowing state, if the flow rate of the nitrogen is smaller, the contact body has poor fluidity in the fine powder activation bed, the impurity removal on the surface of the contact body is not facilitated, and if the flow rate of the nitrogen is too large, a part of contact body with smaller particles is blown out, so that raw materials are wasted.
Optionally, a filtering system is arranged behind the fine powder activation bed, and the filtering system is used for collecting and burning the carbon impurities on the surfaces of the third contact body and the fourth contact body.
Specifically, the third contact body and the fourth contact body which are subjected to impurity removal by the fine powder activation bed are recycled, the removed carbon impurities are filtered and collected by a filtering system arranged behind the fine powder activation bed, and then the collected carbon impurities are subjected to incineration treatment, so that the pollution to the environment relative to direct emission is reduced.
The technical scheme of the application is illustrated in detail by specific examples.
Example 1
A method for returning an organosilicon contact body to a bed, comprising the following steps:
1) The silicon powder and the copper catalyst are mixed in a contact tank to form a first contact, wherein the mass ratio of the copper catalyst in the contact is 4% and the copper catalyst is cuprous oxide during mixing. And inputting the first contact body into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable silicon powder and chloromethane to react under the action of a copper catalyst to generate a methylchlorosilane crude product, wherein the temperature in the fluidized bed reactor is 280 ℃, and the pressure is 0.28MPa.
2) The methyl chlorosilane crude product synthesized in the fluidized bed reactor is sequentially input into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, gas-solid separation is carried out under the action of the cyclone separator, a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride are sequentially obtained through separation, and the methyl chlorosilane and the methyl chloride obtained through separation enter into the next impurity removal process.
3) And directly conveying the second contact body separated by the primary cyclone separator to a fluidized bed reactor for recycling, then sampling and testing the particle sizes of the third contact body and the fourth contact body separated by the secondary cyclone separator and the tertiary cyclone separator, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, and carrying out directional conversion treatment on the third contact body and the fourth contact body serving as waste contact bodies through a contact body tank if the particle sizes of the third contact body and the fourth contact body are smaller than 30 mu m.
4) Nitrogen is introduced into the fine powder activation bed for removing impurities, nitrogen has a certain flow velocity in the fine powder activation bed, silicon powder particles have a certain hardness, and under the action of air flow, the contact particles mutually collide and rub, so that carbon impurities deposited on the surface of the contact are separated from the surface of the contact, and the activated contact is obtained. The flow rate of nitrogen in the fine powder activation bed was 1000Nm 3 And/h, a jacket is arranged outside the fine powder activation bed, the fine powder activation bed is heated by heat conduction oil in the jacket, the temperature of the heat conduction oil is 240 ℃, the temperature in the fine powder activation bed is 100 ℃, and the pressure is 0.1MPa. A filtering system is arranged behind the fine powder activation bed, and the filtering system collects and burns carbon impurities on the surface of the blown-off contact body.
5) And collecting the activated contact body in a fine powder tank and conveying the contact body to a fluidized bed reactor for recycling.
Example 2
A method for returning an organosilicon contact body to a bed, comprising the following steps:
1) The silicon powder and the copper catalyst are mixed in a contact tank to form a first contact, wherein the mass ratio of the copper catalyst in the contact is 5% and the copper catalyst is cuprous oxide during mixing. And inputting the first contact body into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable silicon powder and chloromethane to react under the action of a copper catalyst to generate a methylchlorosilane crude product, wherein the temperature in the fluidized bed reactor is 295 ℃, and the pressure is 0.29MPa.
2) The methyl chlorosilane crude product synthesized in the fluidized bed reactor is sequentially input into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, gas-solid separation is carried out under the action of the cyclone separator, a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride are sequentially obtained through separation, and the methyl chlorosilane and the methyl chloride obtained through separation enter into the next impurity removal process.
3) And directly conveying the second contact body separated by the primary cyclone separator to a fluidized bed reactor for recycling, then sampling and testing the particle sizes of the third contact body and the fourth contact body separated by the secondary cyclone separator and the tertiary cyclone separator, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, and carrying out directional conversion treatment on the third contact body and the fourth contact body serving as waste contact bodies through a contact body tank if the particle sizes of the third contact body and the fourth contact body are smaller than 30 mu m.
4) Nitrogen is introduced into the fine powder activation bed for removing impurities, nitrogen has a certain flow velocity in the fine powder activation bed, silicon powder particles have a certain hardness, and under the action of air flow, the contact particles mutually collide and rub, so that carbon impurities deposited on the surface of the contact are separated from the surface of the contact, and the activated contact is obtained. The flow rate of nitrogen in the fine powder activation bed was 1000Nm 3 And/h, a jacket is arranged outside the fine powder activation bed, the fine powder activation bed is heated by heat conduction oil in the jacket, the temperature of the heat conduction oil is 250 ℃, the temperature in the fine powder activation bed is 112 ℃, and the pressure is 0.15MPa. A filtering system is arranged behind the fine powder activation bed, and the filtering system collects and burns carbon impurities on the surface of the blown-off contact body.
5) And collecting the activated contact body in a fine powder tank and conveying the contact body to a fluidized bed reactor for recycling.
Example 3
A method for returning an organosilicon contact body to a bed, comprising the following steps:
1) The silicon powder and the copper catalyst are mixed in a contact tank to form a first contact, wherein the mass ratio of the copper catalyst in the contact is 7% and the copper catalyst is cuprous oxide during mixing. And inputting the first contact body into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable silicon powder and chloromethane to react under the action of a copper catalyst to generate a methylchlorosilane crude product, wherein the temperature in the fluidized bed reactor is 310 ℃, and the pressure is 0.31MPa.
2) The methyl chlorosilane crude product synthesized in the fluidized bed reactor is sequentially input into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, gas-solid separation is carried out under the action of the cyclone separator, a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride are sequentially obtained through separation, and the methyl chlorosilane and the methyl chloride obtained through separation enter into the next impurity removal process.
3) And directly conveying the second contact body separated by the primary cyclone separator to a fluidized bed reactor for recycling, then sampling and testing the particle sizes of the third contact body and the fourth contact body separated by the secondary cyclone separator and the tertiary cyclone separator, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, and carrying out directional conversion treatment on the third contact body and the fourth contact body serving as waste contact bodies through a contact body tank if the particle sizes of the third contact body and the fourth contact body are smaller than 30 mu m.
4) Nitrogen is introduced into the fine powder activation bed for removing impurities, nitrogen has a certain flow velocity in the fine powder activation bed, silicon powder particles have a certain hardness, and under the action of air flow, the contact particles mutually collide and rub, so that carbon impurities deposited on the surface of the contact are separated from the surface of the contact, and the activated contact is obtained. The flow rate of nitrogen in the fine powder activation bed was 1000Nm 3 The fine powder activation bed is externally provided with a jacket, the fine powder activation bed is heated by heat conduction oil in the jacket, the temperature of the heat conduction oil is 250 ℃, the temperature in the fine powder activation bed is 120 ℃, and the pressure is 0.2MPa. A filtering system is arranged behind the fine powder activation bed, and the filtering system collects and burns carbon impurities on the surface of the blown-off contact body.
5) And collecting the activated contact body in a fine powder tank and conveying the contact body to a fluidized bed reactor for recycling.
Comparative example 1
A method for returning an organosilicon contact body to a bed, comprising the following steps:
1) The silicon powder and the copper catalyst are mixed in a contact tank to form a first contact, wherein the mass ratio of the copper catalyst in the contact is 7% and the copper catalyst is cuprous oxide during mixing. And inputting the first contact body into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable silicon powder and chloromethane to react under the action of a copper catalyst to generate a methylchlorosilane crude product, wherein the temperature in the fluidized bed reactor is 310 ℃, and the pressure is 0.31MPa.
2) The methyl chlorosilane crude product synthesized in the fluidized bed reactor is input into a first cyclone separator, a second cyclone separator and a third cyclone separator in sequence for separation, a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride are sequentially obtained by separation, gas-solid separation is carried out under the action of the cyclone separator, and the methyl chlorosilane and the methyl chloride obtained by separation enter into the next impurity removal procedure.
3) And directly conveying the second contact body, the third contact body and the fourth contact body which are separated by the cyclone separator to a fluidized bed reactor for recycling.
Experimental example 1
The schemes in examples 1 to 3 described above were compared with the scheme in comparative example 1 to obtain the results shown in table one.
List one
By comparing the schemes of the embodiments, the application has the following beneficial effects:
(1) The application realizes the aim of activating the surface of the organosilicon contact back to the bed, and compared with the prior art (comparative example 1), the product methyl chlorosilane yield is higher.
(2) Compared with the prior art (comparative example 1), the impurity removing reagent in the scheme of the application has the advantages that the contact body returns to the bed, the utilization rate of silicon powder is improved, and the production cost is reduced.
(3) In the production process of the scheme of the application, the waste contact body is discharged and treated while the contact body is activated, so that the production period is prolonged, the problem that frequent shutdown and maintenance are required due to more impurities is solved, and the production efficiency is improved.
(4) The process is convenient to operate and easy to realize industrialization.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solution of the present application, and not limiting thereof; although the application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will appreciate that; the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (6)
1. A method for returning an organosilicon contact body to a bed, comprising:
s1: mixing silicon powder and a copper catalyst in a contact tank to form a first contact, inputting the first contact into a fluidized bed reactor, and simultaneously introducing chloromethane gas into the fluidized bed reactor to enable the silicon powder and the chloromethane to react under the action of the copper catalyst to generate a methylchlorosilane crude product;
s2: sequentially inputting the methyl chlorosilane crude product into a first cyclone separator, a second cyclone separator and a third cyclone separator for separation, sequentially separating to obtain a second contact body, a third contact body, a fourth contact body, methyl chlorosilane and methyl chloride, and enabling the methyl chlorosilane and the methyl chloride to enter a next impurity removing step;
s3: directly conveying the second contact body separated by the primary cyclone separator to the fluidized bed reactor for reaction, and conveying the third contact body separated by the secondary cyclone separator and the fourth contact body separated by the tertiary cyclone separator to a fine powder activation bed for activation;
s4: introducing nitrogen into the fine powder activation bed to activate the third contact body and the fourth contact body, collecting the activated third contact body and fourth contact body in a fine powder tank, and conveying the third contact body and fourth contact body to the fluidized bed reactor for recycling, wherein the flow rate of the nitrogen in the fine powder activation bed is 1000Nm 3 /h；
Sampling and testing the particle sizes of the third contact body and the fourth contact body, if the particle sizes of the third contact body and the fourth contact body are larger than or equal to 30 mu m, conveying the third contact body and the fourth contact body to a fine powder activation bed for activation, and if the particle sizes of the third contact body and the fourth contact body are smaller than 30 mu m, taking the third contact body and the fourth contact body as waste contact bodies and carrying out directional conversion treatment through the contact body tank;
the fine powder activation bed is heated by heat conduction oil in a jacket, the temperature of the heat conduction oil is 240-260 ℃, the temperature in the fine powder activation bed is 100-120 ℃, and the pressure is 0.1-0.2MPa.
2. The method of claim 1, wherein the copper-based catalyst is one or more of cuprous oxide and cuprous chloride.
3. The method according to claim 1 or 2, characterized in that the copper-based catalyst mass fraction in the first contact is 4-7%.
4. The process according to claim 1, wherein the temperature in the fluidized bed reactor is 280-310 ℃ and the pressure is 0.28-0.31MPa.
5. The method of claim 1, wherein the contactor tank is further configured to feed the contactors within the fluidized bed reactor into the contactor tank when the fluidized bed reactor is shut down.
6. The method according to claim 1, wherein a filtration system is arranged behind the fine powder activation bed, and the filtration system is used for collecting and incinerating carbon impurities on the surfaces of the removed third contact body and the removed fourth contact body.
Priority Applications (1)
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| US4224297A (en) * | 1977-07-22 | 1980-09-23 | Wacker-Chemie Gmbh | Method for reactivating a residue containing elemental silicon |
| US4281149A (en) * | 1980-03-24 | 1981-07-28 | General Electric Company | Process for treating silicon particles within a silicone reactor system |
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| CN110075762A (en) * | 2019-05-20 | 2019-08-02 | 合盛硅业股份有限公司 | Method and apparatus organosilicon contact separation and reduce methylchlorosilane impurity |
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| DE102014225460A1 (en) * | 2014-12-10 | 2016-06-16 | Wacker Chemie Ag | Process for the direct synthesis of methylchlorosilanes in fluidized bed reactors |
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| US4224297A (en) * | 1977-07-22 | 1980-09-23 | Wacker-Chemie Gmbh | Method for reactivating a residue containing elemental silicon |
| US4281149A (en) * | 1980-03-24 | 1981-07-28 | General Electric Company | Process for treating silicon particles within a silicone reactor system |
| CN101456877A (en) * | 2008-12-08 | 2009-06-17 | 江苏宏达新材料股份有限公司 | Contact masses processing method during methylchlorosilane synthesis |
| CN110075762A (en) * | 2019-05-20 | 2019-08-02 | 合盛硅业股份有限公司 | Method and apparatus organosilicon contact separation and reduce methylchlorosilane impurity |
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