Continuous production device for powder silicon resin

Abstract

The utility model belongs to the technical field of silicon resin, and particularly relates to a continuous production device for powder silicon resin. The utility model provides a continuous production device for powder silicon resin. The continuous production device comprises a hydrochloric acid storage tank, a hydrochloric acid dilution tank, a liquid sodium silicate storage tank, a liquid sodium silicate dilution tank, an alcohol storage tank, a screw machine, a solvent storage tank, a hydrolysis kettle, a water washing kettle, a vacuum stirrer and a screw conveyor, in the process of evaporating the solvent to form the powdery silicon resin, the powdery silicon resin can be continuously crushed by the shearing force formed in the continuous stirring process of the vacuum stirrer, so that the caking of the powdery silicon resin is reduced, the powdery silicon resin is not easy to block, and meanwhile, the yield and the production efficiency of the powdery silicon resin can also be improved; therefore, the technical problem that in the prior art, powder silicon resin is prone to being blocked during discharging is solved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of silicone resin, and particularly relates to a powder silicone resin continuous production device. BACKGROUND

[0002] Silicone resin is a thermosetting polyorganosiloxane with a highly cross-linked structure, has excellent heat resistance and electrical insulation, and can be used to prepare electrical insulating materials; the silicone resin also has excellent high and low temperature resistance and weather resistance, and can be used to prepare coatings; in addition, the silicone resin also has good bonding performance, and can be used to prepare adhesives; the various performances of the silicone resin enable it to be applied in multiple technical fields.

[0003] At present, the device for producing silicone resin mainly relies on a single reaction kettle for production, the whole production process has many procedures, and multiple procedure turnovers need to be performed, so that the production efficiency is low; time-consuming processes such as mixing, standing and separation in the reaction kettle for a long time are relied on; low boiling point removal in the kettle is adopted, product viscosity is uncontrollable, discharging is too slow, product materials are not easy to transfer, time is long, manual metering and feeding are adopted, and the quality of each batch of glue is not the same, so that the quality is unstable; therefore, the production efficiency of the device for producing silicone resin in batches is low.

[0004] The physical form of silicone resin can be divided into powder type solid silicone resin and fluid state liquid silicone resin; in the production process of the powder type solid silicone resin, the traditional process route is in-vessel vacuum low boiling point removal, and the powder silicone resin is easy to be agglomerated into blocks, which causes many problems such as that the discharging is easy to be blocked in the process of changing the liquid intermediate product into the powder type solid silicone resin, and the reaction kettle is stuck. CONTENT OF THE INVENTION

[0005] Therefore, the application provides a powder silicone resin continuous production device to solve the technical problem that the powder silicone resin is easy to be blocked during discharging in the prior art.

[0006] A powder silicone resin continuous production device, characterized in that the device comprises a hydrochloric acid storage tank, a hydrochloric acid dilution tank, a liquid sodium silicate storage tank, a liquid sodium silicate dilution tank, an alcohol storage tank, a screw machine, a solvent storage tank, a hydrolysis kettle, a water washing kettle, a vacuum stirrer and a screw conveyor.

[0007] The outlet of the hydrochloric acid storage tank is in communication with the inlet of the hydrochloric acid dilution tank.

[0008] The outlet of the liquid sodium silicate storage tank is in communication with the inlet of the liquid sodium silicate dilution tank.

[0009] The outlet of the hydrochloric acid dilution tank is in communication with the inlet of the screw machine, the outlet of the liquid sodium silicate dilution tank is in communication with the inlet of the screw machine, and the outlet of the alcohol storage tank is in communication with the inlet of the screw machine.

[0010] The outlet of the screw machine is communicated with the inlet of the hydrolysis kettle;

[0011] The outlet of the solvent storage tank is communicated with the inlet of the hydrolysis kettle;

[0012] The outlet of the water washing kettle is communicated with the inlet of the hydrolysis kettle;

[0013] The outlet of the water washing kettle is communicated with the inlet of the vacuum stirrer;

[0014] The outlet of the vacuum stirrer is communicated with the inlet of the screw conveyor.

[0015] According to the screw machine is a single screw or double screw machine with at least two inlets, the internal contact part is covered with a polytetrafluoroethylene coating.

[0016] According to the powder silicone resin continuous production device, the outlet of the water washing kettle is communicated with the inlet of the vacuum stirrer.

[0017] The outlet of the liquid-liquid centrifuge is communicated with the inlet of the vacuum stirrer.

[0018] According to the powder silicone resin continuous production device, the outlet of the liquid-liquid centrifuge is communicated with the inlet of the vacuum stirrer.

[0019] The outlet of the buffer tank is communicated with the inlet of the vacuum stirrer.

[0020] A powder silicone resin continuous production device is characterized in that the outlet of the hydrochloric acid storage tank is provided with a first liquid weighing scale.

[0021] The outlet of the liquid sodium silicate storage tank is provided with a second liquid weighing scale.

[0022] The outlet of the alcohol storage tank is provided with a third liquid weighing scale.

[0023] The outlet of the solvent storage tank is provided with a fourth liquid weighing scale.

[0024] According to the powder silicone resin continuous production device, the outlet of the hydrolysis kettle is provided with an online refractometer.

[0025] Compared with the prior art, the powder silicone resin continuous production device provided by the application at least has the following beneficial effects:

[0026] 1. The powder silicone resin continuous production device provided by the application can prevent the powder silicone resin formed by evaporating the solvent from being blocked during discharging by arranging a vacuum stirring kettle and other devices.

[0027] 2. The powder silicone resin continuous production device provided by the application can shorten the mixing and separation time of the intermediate product and improve the production efficiency of the powder silicone resin by arranging a screw mixer, a liquid-liquid centrifuge and other devices.

[0028] 3. The powder silicone resin continuous production device provided by the application can reduce the waste of the intermediate product and improve the yield of the powder silicone resin by arranging an online refractometer. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to more clearly illustrate the technical solutions in the specific embodiments or prior art of the present application, the drawings needed in the description of the specific embodiments or prior art will be briefly introduced below. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0030] Figure 1 The reference numerals are: 1-hydrochloric acid storage tank, 2-hydrochloric acid dilution tank, 3-liquid sodium silicate storage tank, 4-liquid sodium silicate dilution tank, 5-alcohol storage tank, 6-screw machine, 7-solvent storage tank, 8-hydrolysis kettle, 9-water washing kettle, 10-vacuum stirrer, 11-screw conveyor, 12-liquid-liquid centrifuge, 13-buffer tank, 14-first liquid weighing scale, 15-second liquid weighing scale, 16-third liquid weighing scale, 17-fourth liquid weighing scale, 18-online refractometer. DETAILED DESCRIPTION

[0031] The present application provides a powder silicone resin continuous production device to solve the technical problem that the powder silicone resin is easily blocked during discharging in the prior art.

[0032] The technical solutions of the present application will be described clearly and completely below in combination with the drawings. Obviously, the described embodiments are some embodiments of the present application, not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0033] In view of the traditional process route, in the process of producing powder silicone resin, the liquid is directly distilled in the kettle to become powder, the amount of distilled liquid part is too difficult to control, the powder silicone resin is easy to coalesce into a block, so that the powder silicone resin is easy to be blocked when discharging; The powder silicone resin continuous production device provided by the application, the structure comprises a hydrochloric acid storage tank, a hydrochloric acid dilution tank, a liquid sodium silicate storage tank, a liquid sodium silicate dilution tank, an alcohol storage tank, a screw machine, a solvent storage tank, a hydrolysis kettle, a water washing kettle, a vacuum stirrer and a screw conveyor, the connection relationship comprises that the hydrochloric acid storage tank and the hydrochloric acid dilution tank are communicated, the liquid sodium silicate storage tank and the liquid sodium silicate dilution tank, the outlets of the hydrochloric acid dilution tank, the liquid sodium silicate dilution tank and the alcohol storage tank are communicated with the inlet of the screw machine, and the screw machine, the hydrolysis kettle, the water washing kettle, the vacuum stirrer and the screw conveyor are communicated in sequence; In the powder silicone resin continuous production device provided by the application, the hydrochloric acid dilution tank and the liquid sodium silicate dilution tank can be used for diluting high-concentration hydrochloric acid and liquid sodium silicate respectively, the screw machine is used for conveying the mixture of hydrochloric acid and liquid sodium silicate to the hydrolysis kettle, and the mixture of hexamethyldisiloxane and the rest of aliphatic or aromatic hydrocarbons stored in the solvent storage tank is conveyed to the hydrolysis kettle for hydrolysis reaction, the hydrolysis cross-linking reaction liquid is separated by layering, the oil layer is washed in the water washing kettle, then the silicone solution enters the vacuum stirrer, the hexamethyldisiloxane and other solvents are evaporated by heating and vacuum evaporation in the process of continuous stirring of the vacuum stirrer to form powder silicone resin, and the shear force formed in the process of continuous stirring of the vacuum stirrer can continuously crush the powder silicone resin, so that the powder silicone resin formed by evaporating the solvent is difficult to coalesce into a block and is difficult to be blocked when discharging, thereby overcoming the defects that the amount of distilled liquid is too difficult to control, the powder silicone resin is easy to coalesce into a block, and the powder silicone resin is easy to be blocked when discharging.

[0034] Example 1

[0035] The example 1 of the application provides a powder silicone resin continuous production device, as shown in Figure 1 The structure comprises a hydrochloric acid storage tank, a hydrochloric acid dilution tank, a liquid sodium silicate storage tank, a liquid sodium silicate dilution tank, an alcohol storage tank, a screw machine, a solvent storage tank, a hydrolysis kettle, a water washing kettle and a vacuum stirrer; the connection relationship is that the outlet of the hydrochloric acid storage tank is communicated with the inlet of the hydrochloric acid dilution tank; the outlet of the liquid sodium silicate storage tank is communicated with the inlet of the liquid sodium silicate dilution tank; the outlet of the hydrochloric acid dilution tank is communicated with the inlet of the screw machine, and the outlet of the liquid sodium silicate dilution tank is communicated with the inlet of the screw machine; the outlet of the screw machine is communicated with the inlet of the hydrolysis kettle; the outlet of the hydrolysis kettle is communicated with the inlet of the water washing kettle; the outlet of the water washing kettle is communicated with the inlet of the vacuum stirrer; and the outlet of the vacuum stirrer is communicated with the inlet of the screw conveyor.

[0036] The powder silicone resin continuous production device provided by the example has the following steps in the preparation of powder silicone resin:

[0037] The raw material preparation step, the dilution water is added into the hydrochloric acid dilution tank, and then the concentrated hydrochloric acid is pumped from the hydrochloric acid storage tank, and the stirring is diluted into a certain concentration of dilute hydrochloric acid; at the same time, the dilution water is added into the liquid sodium silicate dilution tank, and then the concentrated liquid sodium silicate is pumped from the liquid sodium silicate storage tank, and the stirring is diluted into a certain concentration of dilute liquid sodium silicate;

[0038] The hydrolysis mixing step: the dilute hydrochloric acid and the dilute liquid sodium silicate, alcohol are pumped into the screw mixer in a certain flow rate in sequence, and the hydrolysis condensation reaction is generated in the screw machine, the experiment is mixed quickly, the material is transported to the hydrolysis kettle after the material is mixed, the solvent is added, and the reaction kettle is heated through the hydrolysis kettle jacket; after the reaction is completed, it is statically layered, and it is divided into upper and lower two layers, the lower layer is water layer, and the upper layer is oil layer, the water layer of the lower layer is sent to the waste storage tank, and the oil layer of the upper layer is transported to the water washing kettle;

[0039] The water washing step, the neutralized material is pumped into the water washing kettle, and an equal amount of water is added, and after the water washing is completed at room temperature, a water-oil mixed phase is obtained, the water phase and the oil phase are separated, and the oil phase is pumped into the distillation kettle for the next step.

[0040] The distillation powder making step, the oil phase after water washing is entered into the vacuum stirrer through self-flow or 0.2-0.3 MPa nitrogen pressure material, and the solvent such as hexamethyldisiloxane is evaporated in the process of continuous stirring in the vacuum stirrer at-0.09 MPa vacuum to form a powder silicon resin product, and the solvent evaporated in this step is condensed for recycling.

[0041] The conveying and packaging step, the powder silicon resin product is conveyed to the powder buffer tank through the screw conveyor device, then conveyed to the powder cooling tank through the split pump for cooling, and after the powder silicon resin product in the powder cooling tank is cooled to below 40 DEG C through the normal temperature cooling water in the jacket, the powder is conveyed to the packaging machine for automatic packaging and packaging into the final product through the powder conveying pump.

[0042] Example 2

[0043] The example 2 of the present application provides a powder silicon resin continuous production device, and the structure is as shown in Figure 1 The difference between the structure of the example 1 and the structure of the example 2 is that the centrifuge 12 and the buffer tank 13 are further included; the centrifuge is arranged between the outlet of the water washing kettle and the inlet of the distillation kettle, the buffer tank is arranged between the outlet of the centrifuge and the inlet of the distillation kettle, the inlet of the centrifuge is communicated with the outlet of the water washing kettle, the outlet of the centrifuge is communicated with the inlet of the buffer tank, and the outlet of the buffer tank is communicated with the inlet of the distillation kettle.

[0044] Since the neutralized material after water washing is a water-oil mixed phase, the speed of separating the water phase and the oil phase is slow, the centrifugal force generated by the centrifuge in this embodiment 3 can accelerate the separation of the water phase and the oil phase, which is beneficial to improve the production efficiency; at the same time, since the centrifuge can quickly separate the water phase and the oil phase, the oil phase can be generated quickly, and the buffer tank is arranged to store the oil phase and input into the distillation kettle for heating by the jacket steam.

[0045] Embodiment 3

[0046] The embodiment 3 of the present application provides a powder silicon resin continuous production device, and the structure is as shown in Figure 1 The difference between the structure of the embodiment 3 and the embodiment 1 is that the embodiment 3 further comprises a first liquid metering scale 14, a second liquid metering scale 15, a third liquid metering scale 16 and a fourth liquid metering scale 17, the first liquid metering scale is installed at the outlet of the hydrochloric acid storage tank, the second liquid metering scale is installed at the outlet of the liquid sodium silicate storage tank, the third liquid metering scale is installed at the outlet of the alcohol storage tank, and the fourth liquid metering scale is installed at the outlet of the solvent storage tank.

[0047] The first liquid metering scale, the second liquid metering scale, the third liquid metering scale and the fourth liquid metering scale provided in the embodiment 3 can accurately measure the liquid hydrochloric acid, the liquid sodium silicate, the alcohol and the hexamethyldisiloxane, so as to avoid manual measurement of the materials, which is easy to cause the quality of each batch of powder silicon resin products to be different and the quality to be unstable.

[0048] Embodiment 4

[0049] The embodiment 4 of the present application provides a powder silicon resin continuous production device, and the structure is as shown in Figure 1 The difference between the structure of the embodiment 4 and the embodiment 1 is that the embodiment 4 further comprises an online refractometer 18, and the online refractometer is installed at the outlet of the hydrolysis kettle.

[0050] The online refractometer provided in the embodiment 4 can be used to measure the refractive index of the liquid, and the refractive indexes of the oil phase and the water phase are obviously different. According to the detection result of the online refractometer, after hydrolysis, the lower acid water layer can be accurately sent to the waste storage tank, and the upper oil layer needed can be transported to the water washing kettle, so as to avoid the upper oil layer needed to be transported to the waste storage tank as far as possible, thereby improving the yield of the powder silicon resin.

[0051] The above embodiments are only used to illustrate the technical solutions of the present application, but not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A continuous powder silicone resin production apparatus characterized by comprising: 1) a powder silicone resin production device, The hydrochloric acid storage tank, the hydrochloric acid dilution tank, the liquid sodium silicate storage tank, the liquid sodium silicate dilution tank, the alcohol storage tank, the screw machine, the solvent storage tank, the hydrolysis kettle, the water washing kettle, the vacuum agitator and the screw conveyor are connected in series. The outlet of the hydrochloric acid storage tank is connected with the inlet of the hydrochloric acid dilution tank. The outlet of the liquid sodium silicate storage tank is connected with the inlet of the liquid sodium silicate dilution tank. The outlet of the hydrochloric acid dilution tank is connected with the inlet of the screw machine, the outlet of the liquid sodium silicate dilution tank is connected with the inlet of the screw machine, and the outlet of the alcohol storage tank is connected with the inlet of the screw machine. The outlet of the screw machine is connected with the inlet of the hydrolysis kettle. The outlet of the solvent storage tank is connected with the inlet of the hydrolysis kettle. The inlet of the water washing kettle is connected with the outlet of the hydrolysis kettle. The outlet of the water washing kettle is connected with the inlet of the vacuum agitator. The outlet of the vacuum agitator is connected with the inlet of the screw conveyor. The screw machine is a single screw or double screw machine with at least two inlets, and the internal and material contact part is covered with a polytetrafluoroethylene coating.

2. The apparatus for continuous production of powder silicone resin according to claim 1, wherein A liquid-liquid centrifuge is arranged between the outlet of the water washing kettle and the inlet of the vacuum agitator.

3. The apparatus for continuous production of powder silicone resin according to claim 1, wherein The inlet of the liquid-liquid centrifuge is connected with the outlet of the water washing kettle, and the outlet of the liquid-liquid centrifuge is connected with the inlet of the vacuum agitator. A buffer tank is arranged between the outlet of the liquid-liquid centrifuge and the inlet of the vacuum agitator.

4. The apparatus according to claim 3, wherein The inlet of the buffer tank is connected with the outlet of the centrifuge, and the outlet of the buffer tank is connected with the inlet of the vacuum agitator. A first liquid metering scale is installed at the outlet of the hydrochloric acid storage tank.

5. The apparatus for continuous production of powder silicone resin according to claim 1, wherein A second liquid metering scale is installed at the outlet of the liquid sodium silicate storage tank. A third liquid metering scale is installed at the outlet of the alcohol storage tank. A fourth liquid metering scale is installed at the outlet of the solvent storage tank. An online refractometer is installed at the outlet of the hydrolysis kettle.

6. The apparatus for continuous production of powder silicone resin according to claim 1, wherein ​

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