CN112659520A - Semi-continuous production process and production device of addition type liquid silicone rubber-based adhesive - Google Patents

Semi-continuous production process and production device of addition type liquid silicone rubber-based adhesive Download PDF

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Publication number
CN112659520A
CN112659520A CN202011425724.2A CN202011425724A CN112659520A CN 112659520 A CN112659520 A CN 112659520A CN 202011425724 A CN202011425724 A CN 202011425724A CN 112659520 A CN112659520 A CN 112659520A
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silicone oil
section
kneader
screw extruder
storage device
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黎哲辉
雷丽娟
郭鹏
吴超波
涂广水
李水保
刘建军
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Abstract

In order to solve the technical problems of low production efficiency and high difficulty in uniformly mixing powder rubber mixtures in the prior art, the invention provides a semi-continuous production process and a production device of addition type liquid silicone rubber base rubber. Compared with the traditional process for producing the base rubber by using the kneader in the whole process, the process of the invention shortens the batch production time of the base rubber by more than 50%; only the powder adhesive is produced in the kneading machine with the screw extrusion function, the powder adhesive cannot be adhered in the kneading machine, and the screw on the kneading machine is adopted for discharging, so that a large amount of time for manual discharging and cleaning of the kneading machine can be saved, and the safety is greatly improved; the double-screw extruder has good sealing effect, so that the stripping rate is greatly superior to that of a kneader, the VOC (volatile organic compounds) of the base rubber is greatly reduced, and the double-screw extruder can be used for producing two-section-free liquid silicone rubber.

Description

Semi-continuous production process and production device of addition type liquid silicone rubber-based adhesive
Technical Field
The invention belongs to the field of liquid silicone rubber production, and particularly relates to a semi-continuous production process and a production device of addition type liquid silicone rubber base rubber.
Background
The addition type liquid silicon rubber has the advantages of high processing efficiency, transparent and tasteless products and the like, so that the use proportion in the field of silicon rubber products is increased year by year, and the demand is increased more and more.
The addition type liquid silicone rubber is generally prepared by uniformly mixing the A/B components in a static mixer according to the ratio of 1:1 and injecting the mixture into a mold to prepare a required silicone rubber product, wherein liquid silicone rubber base rubber is required to be used in the production process of the A/B components. Through the development of many years, the production process of the liquid silicone rubber-based adhesive is basically shaped, generally, silicone oil, a treating agent and white carbon black are put into a kneader, uniformly mixed, heated to about 150 ℃ for vacuum reduction, and then diluted silicone oil is added and uniformly stirred. Taking a common kneader with the volume of 2000L as an example, the method usually takes 10-16 hours to produce a batch of base rubber, and the production efficiency is low, so that the production efficiency of the liquid silicone rubber base rubber is severely restricted. In addition, due to the low efficiency of the kneader, the VOC of the liquid silicone rubber-based adhesive produced by the method is often high, about 1.5%, and the requirement that the VOC of the product specified in national standard GB4806.2-2015 of the infant and toddler industry is less than or equal to 0.5% cannot be directly met. For this reason, silicone rubber products are commonly post-vulcanized (200 ℃/4h) in the industry to ensure VOC compliance. The post-vulcanization process can reduce VOC but the process is troublesome, so that the post-vulcanization-free product has become a current trend. In addition, after the liquid silicone rubber base rubber is produced, the viscous base rubber is often manually pulled out of the kneader, which not only consumes manpower but also has great potential safety hazard.
Chinese patent CN102615801B discloses an injection type bi-component liquid silicone rubber continuous production line, which is characterized in that silicone oil, white carbon black and a treating agent are premixed in a first side feeding machine and a second side feeding machine, and then are fed into a first-stage screw extruder to be subjected to heating, lowering, diluting and other treatments, and finally, the continuous production of liquid silicone rubber base rubber is realized, so that the production efficiency is improved. However, it is very difficult to premix the mixture of silicone oil and white carbon black with the content of white carbon black up to about 40% by using a feeder, and if the powder-rubber mixture formed in the mixing stage is not well treated, the anti-structuring capability, the rubber material operable time and the mechanical property of the liquid silicone rubber-based rubber can be directly influenced, and the influence on the quality of the final product is very large.
Chinese patent CN205343730U discloses a complete set of continuous production apparatus for organic silica gel base material, which comprises a stirring device (such as a kneader or a disperser), a screw machine (such as a twin-screw machine) and a first interface of a three-way valve, which are connected in sequence, wherein the second interface of the three-way valve is connected with the inlet of the stirring device, and the third interface of the three-way valve is connected with a high-viscosity material cooler. However, this method can only be used for producing paste silicone sealant base material with certain fluidity, and cannot produce liquid silicone rubber powder with the fumed silica content as high as about 40%, and since the liquid silicone rubber powder is basically solid in appearance, it cannot be pumped out from a dispersion machine or a kneader by a booster pump.
Disclosure of Invention
The invention provides a semi-continuous production process and a production device for addition type liquid silicone rubber-based rubber, aiming at solving the technical problems that the production efficiency of addition type liquid silicone rubber-based rubber is not high and the difficulty in uniformly mixing powder rubber mixtures is high in the prior art.
A semi-continuous production device for addition type liquid silicone rubber base rubber comprises a kneading machine and a double-screw extruder which are connected in sequence and have a screw extrusion function.
According to the invention, the discharge port of the kneading machine with the screw extrusion function is directly connected with the feed port of the double-screw extruder or is connected with the feed port of the double-screw extruder through a conveying device. In one embodiment of the invention, the conveying means is a conveyor belt.
According to the invention, the production device further comprises a first silicone oil storage device, a treating agent storage device and a white carbon black storage device, which are respectively connected with the kneading machine with the screw extrusion function through pipelines, and the silicone oil, the treating agent and the white carbon black in the silicone oil storage device, the treating agent storage device and the white carbon black storage device are respectively fed into the kneading machine with the screw extrusion function to be mixed to prepare the powder adhesive.
According to the invention, preferably, the production device further comprises an intermediate mixing device, the intermediate mixing device is positioned on a connecting pipeline of the first silicone oil storage device and the treating agent storage device and the kneader with the screw extrusion function, and the silicone oil and the treating agent in the corresponding silicone oil storage device and the treating agent storage device are fed into the intermediate mixing device to be mixed and then fed into the kneader with the screw extrusion function.
According to the invention, the production device preferably also comprises a silicone oil metering pump which is located on the output line of the silicone oil storage device, before entering the intermediate mixing device (when an intermediate mixing device is present) or the kneader with screw extrusion function (when an intermediate mixing device is not present).
According to the invention, the production device preferably also comprises a treatment agent metering pump which is located on the outlet line of the treatment agent storage device, before entering the intermediate mixing device (when an intermediate mixing device is present) or the kneader with screw extrusion function (when an intermediate mixing device is not present).
According to the present invention, preferably, the production apparatus further comprises a white carbon black pump, and the white carbon black pump is located on an output pipeline of the white carbon black storage device and before entering the kneader with the screw extrusion function. The pump can add white carbon black into the kneader with the screw extrusion function in a plurality of times. In one embodiment of the present invention, the white carbon black pump is an air operated diaphragm pump.
According to the invention, the kneader with screw extrusion function has a vacuum extraction opening.
According to the invention, the twin-screw extruder comprises a feed opening section, a heat treatment section, a dilution section and a cooling section which are arranged in sequence.
According to the invention, the feed opening section of the twin-screw extruder is provided with a vacuum suction opening. The feed inlet section has a heating function.
According to the invention, the heat treatment section of the twin-screw extruder is provided with a vacuum extraction opening. The heat treatment section has a heating function.
According to the invention, the dilution section of the twin-screw extruder is provided with a vacuum extraction opening.
According to the invention, the diameter of the cylinder of the double-screw extruder is 110-160mm, and the length-diameter ratio is 60-75. In one embodiment of the invention, the twin screw extruder has a barrel diameter of 135mm and a length to diameter ratio of 68.
According to the invention, the production device also comprises a second silicone oil storage device which is connected with the dilution section of the twin-screw extruder.
According to the present invention, when the silicone oil for the preparation of the jelly and the silicone oil for dilution are the same silicone oil, the first silicone oil storage means and the second silicone oil storage means may be unified into one device or may be two separate devices.
According to the invention, each vacuum pumping hole is connected with a vacuum pumping device.
The invention also provides a process method for carrying out addition type liquid silicone rubber-based semi-continuous production by using the production device, which comprises the following steps:
(1) preparing powder rubber: adding silicone oil, a treating agent and white carbon black into a kneading machine with a screw extrusion function, and mixing to prepare powder rubber;
(2) and (3) performing low temperature removal treatment and dilution treatment: extruding the powder adhesive prepared in the step (1) through a kneading machine with a screw, conveying the powder adhesive to a feed inlet section of a double-screw extruder, heating the powder adhesive to 150-180 ℃ in a heat treatment section under a vacuum condition, keeping the temperature in the heat treatment section at 150-180 ℃ for 20-40 minutes in vacuum, then feeding the powder adhesive into a dilution section, uniformly mixing the powder adhesive with the added silicon oil for dilution, and finally feeding the powder adhesive into a cooling section for cooling and discharging.
According to the invention, in the step (1), the silicone oil and the treating agent are mixed to form a mixture before being added into a kneader with a screw extrusion function.
According to the invention, in the step (1), the white carbon black is added into the kneader in portions.
According to the invention, in the step (1), after the silicone oil, the treating agent and the white carbon black are uniformly mixed, the ammonia gas generated in the mixing process is removed by vacuumizing.
According to the invention, in the step (2), vacuumizing operation is carried out in the feed inlet section, the heat treatment section and the dilution section so as to discharge low-boiling substances and/or bubbles generated in the processes of dehydration, heat treatment and dilution.
According to the invention, in the step (2), the speed of the powder adhesive entering the feeding port section of the double-screw extruder is 900-1300 kg/h. In one embodiment of the invention, the speed is 1150 kg/h.
According to the invention, in the step (2), the speed of adding the silicone oil for dilution into the dilution section of the twin-screw extruder is 200-500 kg/h. In one embodiment of the invention, the speed is 380 kg/h.
According to the invention, in step (2), cooling is carried out to below 80 ℃, for example to room temperature.
According to the invention, the production process further comprises a detection step of the addition type liquid silicone rubber-based adhesive to resist the structurization and/or VOC of the addition type liquid silicone rubber-based adhesive.
According to the invention, the structured detection method of the addition type liquid silicone rubber-based adhesive comprises the following steps: taking the prepared base adhesive, keeping the temperature of the prepared base adhesive at 23 ℃ for 1h, and testing the viscosity of the base adhesive by using a TA rheometer under the condition of 10/s; and then, placing the residual base adhesive in a 90 ℃ oven for 16h, taking out, keeping the temperature for 1h at 23 ℃, testing the viscosity of 10/s under the same condition, and judging the structural resistance of the base adhesive according to the viscosity and the viscosity increase ratio.
In one embodiment of the present invention, the method for detecting the structurization of the addition type liquid silicone rubber-based adhesive comprises the following steps: 100g of prepared base rubber is kept at the constant temperature of 23 ℃ for 1h, then the viscosity of the base rubber is tested under the condition of 10/s by using a TA rheometer, the rest base rubber is placed in a 90 ℃ oven after the completion of the viscosity testing, the rest base rubber is taken out after the constant temperature of 23 ℃ for 1h, the viscosity of 10/s is tested under the same condition, and the anti-structural capacity of the base rubber is judged according to the viscosity and the viscosity rising ratio.
According to the invention, the detection method of the VOC of the addition type liquid silicone rubber-based rubber comprises the following steps: and uniformly coating the prepared liquid silicone rubber base rubber on a glass slide at room temperature, putting the glass slide on a 200 ℃ blast oven, baking for 4 hours, taking out the glass slide, putting the glass slide in a drier, cooling for 1 hour, and weighing, wherein the weight loss ratio of the liquid silicone rubber base rubber is the base rubber VOC.
In one embodiment of the invention, the detection method of the addition type liquid silicone rubber-based VOC comprises the following steps: and uniformly coating 5.00 +/-0.2 g of the prepared liquid silicone rubber base adhesive on a glass slide with a groove of 50 multiplied by 2mm at room temperature, putting the glass slide in a blast oven at 200 ℃ for baking for 4 hours, taking out the glass slide, putting the glass slide in a drier for cooling for 1 hour, and weighing, wherein the weight loss ratio of the liquid silicone rubber base adhesive is the base adhesive VOC.
In the present invention, the treating agent is a treating agent for white carbon known in the art, including but not limited to: hexamethyldisilazane, tetramethyldivinylsilazane, heptamethyldisilazane, vinyl-bis-head, hydroxysilane, etc.
The production device and the production process are suitable for producing various addition type liquid silicone rubber base adhesives, the silicone oil can be various silicone oils or mixtures thereof which are known in the field and used for producing corresponding base adhesives, and the viscosity range can be 100-1000000 cs.
Compared with the prior art, the invention has the following beneficial effects:
although the production process of the invention is semi-continuous (the production of the powder adhesive by the kneader with the screw extrusion function is carried out intermittently according to batches, and the low temperature removal treatment and dilution by the double-screw extruder are carried out continuously), compared with the traditional process for producing the base adhesive by the kneader in the whole process, the process of the invention still shortens the batch production time of the base adhesive by more than 50 percent, greatly improves the production efficiency of the base adhesive and reduces the production cost.
In addition, the method only produces the powder adhesive in the kneader with the screw extrusion function, the powder adhesive cannot be adhered in the kneader, and the screw on the kneader is adopted for discharging, so that the safety is greatly improved while a large amount of time of the traditional manual discharging and kneader cleaning methods is saved.
Thirdly, compared with other continuous production processes reported in the prior art, the invention improves the powder rubber production equipment and method, further combines the post-treatment process of a double-screw extruder, and improves the anti-structuring capacity, the rubber material operable time and the mechanical property of the addition type liquid silicone rubber-based rubber. And the double-screw extruder has good sealing effect, the stripping rate is greatly superior to that of a kneader, the VOC (volatile organic compounds) of the base rubber is greatly reduced, and the double-screw extruder can be used for producing two-section addition-free liquid silicone rubber.
Drawings
FIG. 1 is a schematic diagram of a semi-continuous production apparatus and process for addition type liquid silicone rubber-based adhesive. In the figure: 1: a first silicone oil storage tank; 2: a treating agent storage tank; 3: a white carbon black storage tank; 4: intermediate mixing device-mixing tank; 5: a kneading machine with a screw extrusion function; 6: a feed inlet of the double-screw extruder; 7: a heat treatment section of the double-screw extruder; 8: a second silicone oil storage tank; 9: a dilution section of a double-screw extruder; 10: a cooling section of the double-screw extruder; 11. 12, 13, 14: and a vacuum pumping hole.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
In the following examples, the semi-continuous production of addition type liquid silicone rubber-based rubber was carried out according to the apparatus and flow diagram shown in FIG. 1. The semi-continuous production device for the addition type liquid silicone rubber base rubber provided by the embodiment of the invention comprises a first silicone oil storage tank 1, a treating agent storage tank 2, a white carbon black storage tank 3, a mixing tank 4 (an intermediate mixing device), a kneader 5 with a screw extrusion function and a double-screw extruder, wherein the double-screw extruder comprises a feeding port section 6, a heat treatment section 7, a dilution section 9 and a cooling section 10. Silicone oil and a treating agent are respectively fed into a mixing tank 4 from a first silicone oil storage tank 1 and a treating agent storage tank 2 through a metering pump for mixing, and the mixture is fed into a kneader 5 with a screw extrusion function; the white carbon black is added into the kneading machine 5 with the screw extrusion function by a pump in several times, and the white carbon black and the kneading machine 5 with the screw extrusion function are mixed to prepare the powder adhesive. And extruding the powder adhesive by a screw of the kneader, feeding the powder adhesive into a feed inlet 6 of a double-screw extruder through a conveying device, carrying out heat treatment in a heat treatment section 7 of the double-screw extruder, feeding the powder adhesive into a dilution section 9 of the double-screw extruder, mixing and diluting the powder adhesive with the silicon oil from the second silicon oil storage tank 2, and feeding the powder adhesive into a cooling section 10 of the double-screw extruder for cooling and then discharging. The device comprises a kneader 5 with a screw extrusion function, a double-screw extruder feed inlet 6, a double-screw extruder heat treatment section 7 and a double-screw extruder dilution section 9, wherein the double-screw extruder dilution section is provided with vacuum extraction ports (11, 12, 13 and 14 respectively), the extraction ports are connected with vacuum-pumping equipment, and the vacuum-pumping equipment is used for vacuumizing in production so as to remove ammonia gas, low-boiling-point substances, bubbles and the like generated in the production.
Example 1:
(1) preparing powder rubber: respectively pumping 650kg of vinyl-terminated silicone oil with the viscosity of 60000cs and 130kg of hexamethylsilazane from a first silicone oil storage tank 1 and a treating agent storage tank 2 into a mixing tank 4 by using a metering pump, mixing for 20 minutes, completely adding into a kneader 5 with a screw extrusion function, and pumping 420kg of white carbon black with the specific surface area of 400m from a white carbon black storage tank 3 by times through a pneumatic diaphragm pump2Adding the silica white in per gram into a kneader 5 with a screw extrusion function, and pumping out ammonia gas generated in the kneader 5 through a vacuum pumping hole 11 after uniformly stirring.
(2) And (3) performing low temperature removal heat treatment dilution: extruding the prepared powder adhesive in the step (1) through a kneader and a screw, uniformly conveying the powder adhesive to a feed inlet 6 of a double-screw extruder with a barrel diameter of 135mm and a length-diameter ratio of 68 through a conveying belt at a constant speed according to a conveying speed of 1150kg/h, heating the material to 150 ℃ (for 1 minute), and pumping out low-boiling-point substances generated in the heating process through a vacuum pumping hole 12. The material enters a heat treatment section 7 of the double-screw extruder and is sheared for more than 30min at the temperature of 150 ℃, and low-boiling-point substances in the material are continuously removed through a vacuum pumping hole 13. And (3) extracting vinyl-terminated silicone oil with the viscosity of 60000cs from the second silicone oil storage tank 8 at a constant speed of 380kg/h by using a metering pump, adding the vinyl-terminated silicone oil into the dilution section 9 of the double-screw extruder, uniformly mixing the vinyl-terminated silicone oil and the dilution section, and removing bubbles generated by mixing the materials through a vacuum extraction opening 14. The material enters a cooling section 10 to be cooled to below 80 ℃, and the liquid silicone rubber-based rubber is obtained after continuous discharging.
(3) And (3) liquid silicone rubber-based anti-structural detection: 100g of the base adhesive is kept at the constant temperature of 23 ℃ for 1h, then the viscosity of the base adhesive is tested under the condition of 10/s by using a TA rheometer, the rest of the base adhesive is placed in a 90 ℃ oven after the completion of the test for 16h, the viscosity of the base adhesive is tested under the same condition after the constant temperature of 23 ℃ for 1h, and the anti-structural capacity of the base adhesive is judged according to the viscosity and the viscosity rising ratio.
(4) Testing of base rubber VOC: and (3) uniformly coating 5.00 +/-0.2 g of the base adhesive on a glass slide with a groove of 50 multiplied by 2mm at room temperature, putting the glass slide in a blast oven at 200 ℃ for baking for 4 hours, taking out the glass slide, putting the glass slide in a drier for cooling for 1 hour, and weighing, wherein the weight loss ratio of the liquid silicone rubber base adhesive is the base adhesive VOC.
Comparative example 1:
the operation mode and the time for preparing the powder rubber before the heat treatment are the same as those of the example 1 by adopting a kneader without a screw extrusion function to produce the base rubber, and the concrete steps are as follows:
(1) preparing base rubber: respectively pumping 650kg of vinyl-terminated silicone oil with the viscosity of 60000cs and 130kg of hexamethylsilazane from a first silicone oil storage tank 1 and a treating agent storage tank 2 into a mixing tank 4 by using a metering pump, mixing for 20 minutes, completely adding into a kneader without a screw extrusion function, and pumping 420kg of white carbon black with the specific surface area of 420kg from a white carbon black storage tank 3 by times through a pneumatic diaphragm pump400m2Adding the white carbon black in a kneader per gram. After the stirring was uniform, vacuum was applied through the vacuum extraction port 11 of the kneader. Heating to 150 ℃ (for 2-3 hours), stirring for 2 hours at 150 ℃ under vacuum condition, adding 380kg/h of vinyl-terminated silicone oil with viscosity of 60000cs at uniform speed by a metering pump, stirring uniformly, cooling to 80 ℃, and discharging to obtain the liquid silicone rubber-based adhesive.
(2) And (3) liquid silicone rubber-based anti-structural detection: 100g of the base adhesive is kept at the constant temperature of 23 ℃ for 1h, then the viscosity of the base adhesive is tested under the condition of 10/s by using a TA rheometer, the rest of the base adhesive is placed in a 90 ℃ oven after the completion of the test for 16h, the viscosity of the base adhesive is tested under the same condition after the constant temperature of 23 ℃ for 1h, and the anti-structural capacity of the base adhesive is judged according to the viscosity and the viscosity rising ratio.
(3) Testing of base rubber VOC: and (3) uniformly coating 5.00 +/-0.2 g of the base adhesive on a glass slide with a groove of 50 multiplied by 2mm at room temperature, putting the glass slide in a blast oven at 200 ℃ for baking for 4 hours, taking out the glass slide, putting the glass slide in a drier for cooling for 1 hour, and weighing, wherein the weight loss ratio of the liquid silicone rubber base adhesive is the base adhesive VOC.
Comparative example 2
(1) Preparing base rubber: the vinyl-terminated silicone oil with the viscosity of 60000cs and the specific surface area of 400m are respectively added at a feeding rate of 650kg/h and the feeding rate of 130kg/h to hexamethyl silazane2And mixing and agglomerating the fumed silica/g in a feeder at a feeding speed of 420kg/h, feeding the mixture into a primary screw extruder for dispersing, kneading, grinding, heating to 150-170 ℃, vacuumizing for removing low, adding vinyl-terminated silicone oil with the viscosity of 60000cs at a feeding speed of 380kg/h for diluting, and cooling to obtain the continuous-method liquid silicone rubber base rubber.
(2) And (3) liquid silicone rubber-based anti-structural detection: 100g of the base adhesive is kept at the constant temperature of 23 ℃ for 1h, then the viscosity of the base adhesive is tested under the condition of 10/s by using a TA rheometer, the rest of the base adhesive is placed in a 90 ℃ oven after the completion of the test for 16h, the viscosity of the base adhesive is tested under the same condition after the constant temperature of 23 ℃ for 1h, and the anti-structural capacity of the base adhesive is judged according to the viscosity and the viscosity rising ratio.
(3) Testing of base rubber VOC: and (3) uniformly coating 5.00 +/-0.2 g of the base adhesive on a glass slide with a groove of 50 multiplied by 2mm at room temperature, putting the glass slide in a blast oven at 200 ℃ for baking for 4 hours, taking out the glass slide, putting the glass slide in a drier for cooling for 1 hour, and weighing, wherein the weight loss ratio of the liquid silicone rubber base adhesive is the base adhesive VOC.
Figure BDA0002824751880000091
As can be seen from the comparison of the above examples, by adopting the production method of the invention, the batch production time of the product is reduced from 12.5 hours to 6 hours; the initial viscosity and the viscosity after aging of the product are not different from those of the product produced by the traditional kneader process or even slightly lower; manual discharging is not needed in the production process of the base rubber, so that the safety is greatly improved; the VOC of the base rubber is greatly reduced from 1.50 percent to 0.35 percent, and the base rubber can be used for the production of two-section-free silicon rubber; the yield of the base rubber is improved to 100 percent from the original 99.0 percent.
The inventor of the present invention also studied a feeder or a disperser as a powder rubber preparation device, which is matched with a first-stage screw extruder, and found that: the initial viscosity (10/s) of the obtained base gum is more than 930Pa.s, the viscosity (10/s) after 90 ℃/16h rises to more than 1399Pa.s, and the viscosity rise ratio reaches 50.4 percent, which indicates that the anti-structural capability of the base gum is poor, and presumably the reason is improper treatment in the preparation of the powder gum.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A semi-continuous production method of addition type liquid silicone rubber-based rubber is characterized by comprising the following steps:
(1) preparing powder rubber: adding silicone oil, a treating agent and white carbon black into a kneading machine with a screw extrusion function, and mixing to prepare powder rubber;
(2) and (3) performing low temperature removal treatment and dilution treatment: extruding the powder adhesive prepared in the step (1) through a kneading machine with a screw, and feeding the powder adhesive to a double-screw extruder, wherein the double-screw extruder comprises a feeding port section, a heat treatment section, a dilution section and a cooling section which are sequentially arranged, the powder adhesive enters the double-screw extruder through the feeding port section, is heated to 150-180 ℃ in the feeding port section and the heat treatment section under the vacuum condition, is kept for 20-40 minutes in the heat treatment section under the vacuum of 150-180 ℃, then enters the dilution section, is uniformly mixed with the added dilution silica oil, and finally enters the cooling section for cooling and discharging;
preferably, the diameter of the cylinder of the double-screw extruder is 110-160mm, and the length-diameter ratio is 60-75;
preferably, in the step (2), the speed of the powder adhesive entering the feeding port section of the double-screw extruder is 900-1300 kg/h;
preferably, in the step (2), the speed of adding the silicone oil for dilution into the dilution section of the twin-screw extruder is 200-500 kg/h.
2. The production method according to claim 1, wherein in the step (1), the silicone oil and the treating agent are mixed to form a mixture before being fed into a kneader having a screw extrusion function.
3. The production method according to claim 1 or 2, wherein in the step (1), the white carbon black is added to the kneader in divided portions.
4. The production method according to any one of claims 1 to 3, wherein in the step (1), after the silicone oil, the treating agent and the white carbon black are uniformly mixed, ammonia gas generated in the mixing process is removed by vacuumizing; in the step (2), vacuumizing operation is carried out in the feeding port section, the heat treatment section and the diluting section so as to discharge low-boiling-point substances and/or bubbles generated in the processes of removing low boiling-point substances, heat treatment and diluting.
5. The production method according to any one of claims 1 to 4, further comprising a step of detecting the resistance of the addition liquid silicone rubber-based adhesive to structuring and/or VOC's in the addition liquid silicone rubber-based adhesive.
6. A production apparatus for use in the semi-continuous production method of the addition type liquid silicone rubber-based gum described in any one of claims 1 to 5, comprising a kneader with screw extrusion function and a twin-screw extruder which are connected in sequence, the discharge port of the kneader with screw extrusion function and the feed port of the twin-screw extruder being connected directly or through a conveying device, the twin-screw extruder comprising a feed port section, a heat treatment section, a dilution section and a cooling section which are arranged in sequence; the kneader with the screw extrusion function is provided with a vacuum pumping hole; the feeding port section of the double-screw extruder is provided with a vacuum pumping port, and the feeding port section has a heating function; the heat treatment section of the double-screw extruder is provided with a vacuum pumping hole and has a heating function; the diluting section of the double-screw extruder is provided with a vacuum pumping hole; each vacuum pumping hole is connected with a vacuum pumping device.
7. The production apparatus according to claim 6, wherein the production apparatus further comprises a first silicone oil storage device, a treating agent storage device, and a white carbon black storage device, which are respectively connected to the kneader with screw extrusion function through pipes, and the silicone oil, the treating agent, and the white carbon black in the silicone oil storage device, the treating agent storage device, and the white carbon black storage device are respectively fed into the kneader with screw extrusion function to be mixed to prepare the powder adhesive;
preferably, the production device further comprises an intermediate mixing device, the intermediate mixing device is located on a connecting pipeline between the first silicone oil storage device and the processing agent storage device and the kneader with the screw extrusion function, and the silicone oil and the processing agent in the corresponding silicone oil storage device and the processing agent storage device are sent to the intermediate mixing device to be mixed and then sent to the kneader with the screw extrusion function.
8. The production apparatus as claimed in claim 6 or 7, wherein the production apparatus further comprises a silicone oil metering pump which is located at a position before the outlet line of the silicone oil storage device enters the intermediate mixing device when the intermediate mixing device is present, and which is located at a position before the outlet line of the silicone oil storage device enters the kneader with screw extrusion function when the intermediate mixing device is not present;
preferably, the production apparatus further comprises a treating agent metering pump which is located at a position before the outlet line of the treating agent storage device enters the intermediate mixing device when the intermediate mixing device is present, and at a position before the outlet line of the treating agent storage device enters the kneader with screw extrusion function when the intermediate mixing device is not present;
preferably, the production device further comprises a white carbon black pump, wherein the white carbon black pump is positioned on an output pipeline of the white carbon black storage device and before entering the kneader with the screw extrusion function; preferably, the white carbon black pump is a pneumatic diaphragm pump.
9. The production apparatus according to any one of claims 6 to 8, wherein the production apparatus further comprises a second silicone oil storage device connected to the dilution section of the twin-screw extruder; preferably, when the silicone oil used for the preparation of the jelly and the silicone oil used for the dilution are the same silicone oil, the first silicone oil storage means and the second silicone oil storage means are the same device or two separate devices.
CN202011425724.2A 2020-12-08 2020-12-08 Semi-continuous production process and production device of addition type liquid silicone rubber-based adhesive Pending CN112659520A (en)

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