CN210332605U

CN210332605U - Automatic continuous adding device for catalyst

Info

Publication number: CN210332605U
Application number: CN201920411798.7U
Authority: CN
Inventors: 曹华俊; 罗燚; 朱恩华; 刘凯; 张寅旭; 程刘备; 瞿龙学; 侯晓利
Original assignee: Hoshine Silicon Industry Co ltd
Current assignee: Hoshine Silicon Industry Co ltd
Priority date: 2019-03-28
Filing date: 2019-03-28
Publication date: 2020-04-17
Anticipated expiration: 2029-03-28

Abstract

The application provides an automatic continuous device that adds of catalyst includes: the first tank body, the second tank body, the delivery pump and the fluidized bed are connected in sequence; the first tank body comprises a catalyst; the second tank body comprises a mixed solution of a catalyst and chloromethane; the delivery pump is respectively connected with the second tank body and the fluidized bed; the fluidized bed comprises silicon powder, chloromethane gas and the mixed liquid. According to the method, the catalyst mixed liquid with a certain proportion is prepared in advance, then the catalyst mixed liquid is continuously introduced into the fluidized bed, the catalyst is supplemented into the fluidized bed at any time, the fluctuation range of the catalyst content is reduced, and the stability of the methyl chlorosilane reaction is improved.

Description

Automatic continuous adding device for catalyst

Technical Field

The utility model relates to an organochlorosilane technical field especially relates to an automatic device that adds in succession of catalyst.

Background

The organochlorosilane is a pillar of the whole organosilicon chemistry, and most organosilicon products are prepared by processing polymethylsiloxane prepared by hydrolyzing methylchlorosilane with a regulator, a cross-linking agent, an end capping agent and the like. The application of the composite material is in various fields of aerospace, aviation, chemical engineering, metallurgy, daily life of people and medical care. The methyl chlorosilane is generated by the reaction of methyl chloride and silicon powder, and the development process of the methyl chlorosilane is related to the development of the whole organic silicon industry, so that the improvement of the synthesis efficiency of the methyl chlorosilane is extremely important.

Methylchlorosilanes are the most important monomers for the preparation of silicone polymers. Wherein the maximum dosage of the dimethyldichlorosilane accounts for about 90 percent of the methylchlorosilane. In the fluidized bed reactor, silicon powder and a copper catalyst are mixed to form an active contact.

In the polymerization production process of batch operation, the catalyst activity is reduced along with the reaction, and then the catalyst needs to be supplemented in a reaction container at intervals, so that the fluctuation range of the catalyst content is large, and the methyl chlorosilane reaction is unstable.

SUMMERY OF THE UTILITY MODEL

The utility model provides an automatic device that adds in succession of catalyst to it is big to solve the catalyst content fluctuation range that intermittent operation leads to, and methyl chlorosilane reacts unstable problem.

In order to achieve the above object, the utility model provides an automatic continuous adding device of catalyst, include: the first tank body, the second tank body, the delivery pump and the fluidized bed are connected in sequence;

the first tank body is used for containing and conveying the catalyst;

the second tank body is used for mixing the catalyst and the chloromethane liquid to prepare a mixed liquid with the solid content of 1-5%;

the delivery pump is used for continuously introducing the mixed solution into the fluidized bed;

the fluidized bed is used for carrying out methyl chlorosilane reaction.

Optionally, in the automatic continuous catalyst adding device, the first tank is provided with a catalyst feeding pipe and a nitrogen input pipe, the catalyst feeding pipe is provided with a first valve, and the nitrogen input pipe is provided with a second valve; or/and

the vacuum-pumping device also comprises a vacuum-pumping mechanism connected with the first tank body.

Optionally, the above-mentioned automatic continuous catalyst adding apparatus includes: the upper part of the second tank body is provided with a rack, a first connecting pipe and a chloromethane liquid inlet pipe, a stirring rod is arranged in the second tank body, the lower part of the rack is connected with the stirring rod, the upper part of the rack is connected with a motor, the motor is connected with the stirring rod through a speed reducer, and the stirring rod is provided with a double-layer stirring blade; the bottom of the second tank body is connected with the delivery pump.

Optionally, in the above automatic continuous catalyst adding apparatus, a flow meter is disposed on the second connecting pipe between the delivery pump and the fluidized bed; and a pressure gauge is arranged at the upper part of the second tank body.

Optionally, the above automatic continuous catalyst adding apparatus further comprises: and the controller is connected with the flowmeter, the pressure gauge, the motor, the first valve and the second valve.

Optionally, in the automatic and continuous catalyst adding device, a third valve is arranged on the first connecting pipe, a fourth valve is arranged on the chloromethane liquid inlet pipe, and the third valve and the fourth valve are connected with the controller.

Optionally, in the automatic continuous catalyst adding device, a fifth valve and a sixth valve are respectively arranged at two ends of the second connecting pipe, and the fifth valve and the sixth valve are connected with the controller.

Optionally, in the automatic continuous catalyst adding device, the controller is a PLC programmable controller.

Compared with the prior art, the utility model has the advantages that:

the application provides an automatic and continuous catalyst adding method, which comprises the steps of preparing a catalyst mixed solution in a certain proportion in advance, continuously introducing the catalyst mixed solution into a fluidized bed, supplementing a catalyst into the fluidized bed at any time, reducing the fluctuation range of the catalyst content and improving the stability of methyl chlorosilane reaction.

Drawings

The accompanying drawings, which are described herein, serve to provide a further understanding of the invention and constitute a part of this specification, and the exemplary embodiments and descriptions thereof are provided for explaining the invention without unduly limiting it. In the drawings:

FIG. 1 is a flow diagram of a process for the automatic continuous addition of catalyst;

FIG. 2 is a schematic structural view of an automatic continuous catalyst addition apparatus;

the parts in the drawings are numbered as follows:

the device comprises a first tank 1, a catalyst feeding pipe 11, a nitrogen input pipe 12, a first valve 13, a second valve 14, a vacuumizing mechanism 15, a second tank 2, a frame 21, a first connecting pipe 22, a methyl chloride liquid inlet pipe 23, a stirring rod 24, a motor 25, a double-layer stirring blade 26, a third valve 27, a fourth valve 28, a pressure gauge 29, a conveying pump 3, a fluidized bed 4, a second connecting pipe 5, a flowmeter 6, a fifth valve 7, a sixth valve 8 and a seventh valve 9.

Detailed Description

To make the purpose, technical solution and advantages of the present invention clearer, the following will combine the embodiments of the present invention and the corresponding drawings to clearly and completely describe the technical solution of the present invention. It is to be understood that the embodiments described are only some embodiments of the invention, and not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

In the following description, numerous implementation details are set forth in order to provide a more thorough understanding of the present invention. It should be understood, however, that these implementation details should not be used to limit the invention. That is, in some embodiments of the invention, details of these implementations are not necessary. In addition, some conventional structures and components are shown in simplified schematic form in the drawings.

As shown in fig. 1, the present application provides a method for automatic continuous addition of a catalyst, comprising:

s01, mixing the catalyst with chloromethane liquid to prepare a mixed liquid with a solid content of 1-5%;

s02, continuously introducing the mixed solution into the fluidized bed, and carrying out methyl chlorosilane reaction in the fluidized bed.

In an embodiment of the present application, the step of continuously introducing the mixed solution into the fluidized bed in S02 to perform the methylchlorosilane reaction includes:

and introducing silicon powder and chloromethane gas into the fluidized bed, and reacting the silicon powder, the chloromethane liquid and the chloromethane gas under the action of a catalyst to generate methyl chlorosilane.

In one embodiment of the present application, the catalyst is primarily copper powder.

In one embodiment of the application, the content of the catalyst is controlled to be 1.3 +/-0.8% in the methyl chlorosilane reaction process. Preferably, the content of the catalyst is controlled to be 1.6-1.7%.

As shown in fig. 2, in one embodiment of the present application, there is provided an apparatus for an automatic continuous catalyst addition method, comprising: the device comprises a first tank body 1, a second tank body 2, a delivery pump 3 and a fluidized bed 4 which are connected in sequence; the first tank body 1 is used for containing and conveying catalyst; the second tank body 2 is used for mixing the catalyst and the chloromethane liquid to prepare a mixed liquid with the solid content of 1-5%; the delivery pump 3 is used for continuously introducing the mixed liquid into the fluidized bed 4; the fluidized bed 4 is used for carrying out the methylchlorosilane reaction. The continuous conveying of the mixed liquid with the solid content of 1-5% is realized through the conveying pump, and the stability of the reaction is improved.

In one embodiment of the present application, a catalyst feed line 11 and a nitrogen inlet line 12 are provided on the first tank 1, a first valve 13 is provided on the catalyst feed line 11, and a second valve 14 is provided on the nitrogen inlet line 12. The first tank 1 was pressurized with nitrogen gas, and the catalyst was flowed into the second tank 2.

In one embodiment of the present application, the automatic continuous catalyst adding apparatus further comprises: and the vacuumizing mechanism 15 is connected with the first tank body 1. So set up, be in vacuum state in order to guarantee first jar of body, avoided the oxidation of catalyst, it is that the catalyst preserves well, avoids extravagant.

In one embodiment of the application, a frame 21, a first connecting pipe 22 and a chloromethane liquid inlet pipe 23 are arranged at the upper part of the second tank body 2, and one end of the first connecting pipe 22 is connected to the bottom of the first tank body 1; a third valve 27 is arranged on the first connecting pipe 22, and a fourth valve 28 is arranged on the chloromethane liquid inlet pipe 23; a stirring rod 24 is arranged in the second tank body 2, the lower part of the rack 21 is connected with the stirring rod 24, the upper part of the rack 21 is connected with a motor 25, the motor 25 is connected with the stirring rod 24 through a speed reducer, and a double-layer stirring blade 26 is arranged on the stirring rod 24; the bottom of the second tank body 2 is connected with a delivery pump 3. The third valve 27 is used to control the amount of catalyst flowing into the second tank 2 and the fourth valve 28 is used to control the amount of methyl chloride liquid flowing into the second tank 2. The double-layer stirring enables the stirring to be more thorough, enables the catalyst and the chloromethane liquid to be mixed more uniformly, and has more scientific design.

In one embodiment of the application, a flow meter 6 is arranged on the second connecting pipe 5 between the transfer pump 3 and the fluidized bed 4; preferably, the flow is controlled within the range of 0.5-1 t/h through the flowmeter 6, so that the design is more scientific; a pressure gauge 29 is arranged at the upper part of the second tank body 3. Preferably, the pressure is controlled to be 0.5-0.6 MPa. And a fifth valve 7 and a sixth valve 8 are respectively arranged at two ends of the second connecting pipe 5, the fifth valve 7 is used for controlling the amount of the mixed liquid flowing into the second connecting pipe 5, and the sixth valve 8 is used for controlling the amount of the mixed liquid flowing into the fluidized bed 4.

In one embodiment of the present application, the automatic continuous catalyst adding apparatus further comprises: and the controller is connected with the flowmeter 6, the pressure gauge 29, the motor 25, the first valve 13, the second valve 14, the third valve 7 and the fourth valve 8. The controller is a PLC editable controller. The controller can adjust the opening and closing sizes of the first valve 13, the second valve 14, the third valve 27, the fourth valve 28, the fifth valve 7 and the sixth valve 8, and further adjust the amount of the input amount.

In an embodiment of the present application, the bottom of the fluidized bed is connected to the silicon powder input pipe and the chloromethane gas input pipe respectively, and the seventh valve 9 is disposed on the silicon powder input pipe and the chloromethane gas input pipe respectively, and the seventh valve 9 is connected to the controller for controlling the amount of the silicon powder and the chloromethane gas entering the fluidized bed 4. The controller can adjust the opening and closing size of the seventh valve 9, and further adjust the amount of the input amount.

The following is a detailed description of the present application with reference to specific experimental data:

a batch mode: the catalyst mainly adopts copper powder, the concentration range of the catalyst in the fluidized bed 4 is between 1.5 and 2 percent, and the hourly yield of the obtained methyl chlorosilane is 150 to 210 g/kg.

The continuous mode comprises the following steps: the catalyst mainly adopts copper powder, the concentration range of the catalyst in the fluidized bed 4 is 1.6-1.7%, and the hourly yield of the obtained methyl chlorosilane is 190-200 g/kg.

Therefore, the continuous mode and the intermittent mode are compared, the catalyst is obtained by adopting an automatic continuous adding mode, the fluctuation range of the content of the catalyst is reduced, and the stability of the methyl chlorosilane reaction is improved.

The above-mentioned embodiments of the present invention, which further illustrate the objects, technical solutions and advantages of the present invention, it should be understood that the above-mentioned embodiments are only specific examples of the present invention, and are not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An automatic continuous catalyst adding device is characterized by comprising: the first tank body, the second tank body, the delivery pump and the fluidized bed are connected in sequence;

the first tank body comprises a catalyst;

the second tank body comprises a mixed solution of a catalyst and chloromethane;

the delivery pump is respectively connected with the second tank body and the fluidized bed;

the fluidized bed comprises silicon powder, chloromethane gas and the mixed liquid.

2. The automatic continuous catalyst adding device according to claim 1, wherein a catalyst feeding pipe and a nitrogen input pipe are arranged on the first tank body, a first valve is arranged on the catalyst feeding pipe, and a second valve is arranged on the nitrogen input pipe; or/and

3. The automatic continuous catalyst addition device according to claim 2, comprising: the upper part of the second tank body is provided with a rack, a first connecting pipe and a chloromethane liquid inlet pipe, a stirring rod is arranged in the second tank body, the lower part of the rack is connected with the stirring rod, the upper part of the rack is connected with a motor, the motor is connected with the stirring rod through a speed reducer, and the stirring rod is provided with a double-layer stirring blade; the bottom of the second tank body is connected with the delivery pump.

4. The automatic continuous catalyst adding device according to claim 3, wherein a flow meter is provided on a second connecting pipe between the transfer pump and the fluidized bed; and a pressure gauge is arranged at the upper part of the second tank body.

5. The automatic continuous catalyst addition device according to claim 4, further comprising: and the controller is connected with the flowmeter, the pressure gauge, the motor, the first valve and the second valve.

6. The automatic continuous catalyst adding device according to claim 5, wherein a third valve is arranged on the first connecting pipe, a fourth valve is arranged on the methyl chloride liquid inlet pipe, and the third valve and the fourth valve are connected with the controller.

7. The automatic continuous catalyst adding device according to claim 5, wherein a fifth valve and a sixth valve are respectively disposed at two ends of the second connecting pipe, and the fifth valve and the sixth valve are connected to the controller.

8. The apparatus of claim 5, wherein the controller is a PLC programmable controller.