Polysulfide rubber modification synthesis device

Abstract

The utility model belongs to the technical field of polymer modification devices, and relates to a polysulfide rubber modification synthesis device which comprises an ultraviolet lamp, a modification synthesis reaction kettle, an absorption bottle, a vacuum pump and a cooling reflux device, the ultraviolet lamp is arranged outside the modified synthesis reaction kettle, and ultraviolet light generated by the ultraviolet lamp is radiated to the modified synthesis reaction kettle; the modified synthesis reaction kettle is also externally connected with a nitrogen inlet pipe; the absorption bottle is respectively communicated with the cooling reflux device, the modified synthesis reaction kettle and the vacuum pump. According to the utility model, the ultraviolet lamp, the modification synthesis reaction kettle, the absorption bottle, the vacuum pump and the cooling reflux device are integrated, so that modification and synthesis of polysulfide rubber are realized, and the device is suitable for modification synthesis of liquid polysulfide rubber raw rubber.

Description

Technical Field

[0001] The utility model belongs to the technical field of polymer modification devices and relates to a polysulfide rubber modification synthesis device. Background Art

[0002] Polysulfide sealant is a key sealing material used in aircraft engines because of its excellent oil resistance, low air permeability and good weather resistance. The main component of polysulfide sealant, polysulfide sealant, is an elastic sealing material with good bonding strength formed by chemical crosslinking (vulcanization) of liquid polysulfide rubber with low molecular weight. The structure of liquid polysulfide rubber is [-CH 2 -CH 2 -S x -]n, its molecular chain contains thermosensitive disulfide bonds (—SS—) and acetal bonds (—OCO—); therefore, the long-term use temperature should be maintained between -55°C and 120°C. This is because when the long-term use temperature is higher than 120°C, the polysulfide sealant will experience problems such as degradation and aging, which seriously affects the application of this medium-resistant polysulfide sealant in high-temperature fields and is difficult to meet the high-temperature use requirements of modern high-performance aircraft. Therefore, it is necessary to modify and synthesize the liquid polysulfide rubber to broaden the application range of the medium-resistant polysulfide sealant.

[0003] There are many existing rubber modification device structures. A Chinese patent document with reference application number CN201310621293.0 discloses a rubber surface fluorination modification test device, including: a xenon difluoride gas generating device, a gas flow meter, a pressure gauge, a rubber surface fluorination device, an exhaust gas recovery device, a vacuum pump, a motor, a xenon difluoride gas recovery device, a throttle valve, a stainless steel pipe, a temperature control panel, a heating plate, a sealing ring, a rubber sample placement rack and other components. The device can perform surface fluorination modification tests on rubber under different temperature and pressure conditions.

[0004] Although the existing devices can achieve fluorine modification of rubber, the functions of the devices are single and cannot achieve the synthesis after modification; in addition, the existing devices are mainly used for fluorine modification of rubber. This modification method is limited by the chemical structure and is difficult to break through the barriers, so it is not suitable for the modified synthesis of liquid polysulfide rubber. Utility Model Content

[0005] Aiming at the technical problems that the existing rubber modification device has a single function, cannot realize the synthesis after modification and is not suitable for the modification synthesis of liquid polysulfide rubber, the utility model provides a polysulfide rubber modification synthesis device.

[0006] The utility model integrates an ultraviolet lamp, a modified synthesis reaction kettle, an absorption bottle, a vacuum pump and a cooling reflux device to realize the modification and synthesis of polysulfide rubber and is suitable for the modification and synthesis of liquid polysulfide rubber raw rubber.

[0007] In order to achieve the above purpose, the technical solution adopted by the utility model is:

[0008] A polysulfide rubber modification synthesis device comprises an ultraviolet lamp, a modification synthesis reactor, an absorption bottle, a vacuum pump and a cooling reflux device; the ultraviolet lamp is arranged outside the modification synthesis reactor, and the ultraviolet light generated by the ultraviolet lamp radiates onto the modification synthesis reactor; the modification synthesis reactor is also externally connected with a nitrogen inlet pipe; the absorption bottle is respectively connected with the cooling reflux device, the modification synthesis reactor and the vacuum pump.

[0009] It is further defined that the polysulfide rubber modified synthesis device also includes a cooling reflux device, and the cooling reflux device is connected to the interior of the absorption bottle.

[0010] It is further defined that the absorption bottle is connected with a reflux pipe; the reflux pipe is respectively connected with a cooling reflux device, a vacuum pump and a modified synthesis reactor.

[0011] It is further defined that the polysulfide rubber modification synthesis device also includes a nitrogen bottle connected to the nitrogen inlet pipe.

[0012] It is further defined that the polysulfide rubber modification synthesis device also includes a chain-breaking reducing agent storage tank, a polysulfide rubber storage tank, a diene terminal compound storage tank and a photoinitiator storage tank, which are respectively connected to the modification synthesis reactor.

[0013] It is further defined that the polysulfide rubber modification synthesis device also includes a heating and cooling water jacket arranged on the outer wall of the modification synthesis reactor.

[0014] It is further defined that the polysulfide rubber modification synthesis device also includes a temperature sensor arranged on the modification synthesis reactor.

[0015] It is further defined that the polysulfide rubber modification synthesis device also includes a power source connected to the ultraviolet lamp.

[0016] It is further defined that a control switch is provided between the ultraviolet lamp and the power supply.

[0017] It is further defined that the polysulfide rubber modification synthesis device also includes a stirrer and a stirring motor; the stirring motor is placed on the modification synthesis reactor, one end of the stirrer extends into the modification synthesis reactor, and the other end of the stirrer is placed outside the modification synthesis reactor and connected to the stirring motor.

[0018] The beneficial effects of the utility model are:

[0019] 1. The utility model integrates an ultraviolet lamp, a modified synthesis reactor, an absorption bottle, a vacuum pump and a cooling reflux device to achieve the modification and synthesis of liquid polysulfide rubber, and completes the modified synthesis of polysulfide rubber by a photochemical method using ultraviolet lamp irradiation, which can be applied to the modified synthesis of liquid polysulfide rubber (i.e., original rubber).

[0020] 2. In the utility model, a reflux pipe is connected to the absorption bottle, and the cooling reflux device and the absorption bottle are connected through the reflux pipe, so that the cooled low-molecular volatiles can be refluxed into the absorption bottle for absorption, thereby achieving the treatment of the low-molecular volatiles.

[0021] 3. In the utility model, the ultraviolet lamp is connected to a power supply, and a control switch is arranged between the ultraviolet lamp and the power supply. The ultraviolet lamp is turned on by the control switch, so that an intermittent irradiation mode is adopted in the synthesis. While irradiating light, the generation of light and heat can be controlled to prevent the temperature from being too high during the synthesis and promote the synthesis reaction.

[0022] 4. The synthesis device provided by the utility model has a simple structure and is easy to operate, and is suitable for realizing batch modification synthesis of liquid polysulfide rubber. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 A structural diagram of the device provided by the utility model;

[0024] in:

[0025] 1-nitrogen inlet pipe; 2-ultraviolet lamp; 3-modification synthesis reactor; 4-heating and cooling water jacket; 5-absorption bottle; 6-vacuum pump; 7-cooling reflux device; 8-temperature sensor; 9-agitator. DETAILED DESCRIPTION

[0026] The technical solution protected by the utility model is now described in detail in conjunction with the accompanying drawings and embodiments. However, it is obvious that the described embodiments are part of the embodiments of the present application, rather than all of the embodiments. Based on the described embodiments of the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present application.

[0027] Unless otherwise defined, the technical terms or scientific terms used in this application should be understood by people with ordinary skills in the field to which this application belongs. The "first", "second" and similar words used in this application do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and other similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0028] Example 1

[0029] See also Figure 1 The present embodiment provides a polysulfide rubber modification synthesis device, comprising an ultraviolet lamp 2, a modification synthesis reactor 3, an absorption bottle 5, a vacuum pump 6 and a cooling reflux device 7; the ultraviolet lamp 2 is placed outside the modification synthesis reactor 3, and the ultraviolet light generated by the ultraviolet lamp 2 radiates onto the modification synthesis reactor 3; the modification synthesis reactor 3 is also externally connected to a nitrogen inlet pipe 1; the absorption bottle 5 is respectively connected to the cooling reflux device 7, the modification synthesis reactor 3 and the vacuum pump 6.

[0030] In this embodiment, the modified synthesis reactor 3 includes a shell and a feed port, a nitrogen port, a discharge port and a volatiles outlet respectively arranged on the shell, the discharge port is located on the bottom of the shell, and the feed port, the nitrogen port and the discharge port are all located on the top of the shell. The nitrogen inlet pipe 1 is connected to the nitrogen port, and the volatiles outlet is respectively connected to the absorption bottle 5, the vacuum pump 6 and the cooling reflux device 7. When in use, the reaction materials all enter from the feed port, the nitrogen enters from the nitrogen port, the low analysis volatiles generated in the modified synthesis are discharged through the volatiles outlet, and the product of the modified synthesis reaction is discharged from the discharge port.

[0031] Preferably, the shell is a cylindrical structure and is made of stainless steel.

[0032] In this embodiment, the polysulfide rubber modification synthesis device also includes a chain scission reducing agent storage tank, a polysulfide rubber storage tank, a diene terminal compound storage tank and a photoinitiator storage tank respectively connected to the modification synthesis reactor 3. The polysulfide rubber storage tank is used to store the raw material to be modified, that is, liquid polysulfide rubber, also called liquid polysulfide rubber.

[0033] During implementation, there is one feed inlet, and the chain-breaking reducing agent storage tank, the polysulfide rubber storage tank, the diene terminal compound storage tank and the photoinitiator storage tank are all connected to the feed inlet.

[0034] During implementation, there may be four feed ports, and the chain-breaking reducing agent storage tank, the polysulfide rubber storage tank, the diene terminal compound storage tank, and the photoinitiator storage tank are connected to the four feed ports in a one-to-one correspondence. Preferably, a discharge valve is provided on each of the four storage tanks, the chain-breaking reducing agent storage tank, the polysulfide rubber storage tank, the diene terminal compound storage tank, and the photoinitiator storage tank, and the order in which the four materials are added is controlled by controlling the discharge valve according to the progress requirements in the modified synthesis reaction.

[0035] During implementation, the absorption bottle 5 is connected with a reflux pipe; the reflux pipe is connected with the cooling reflux device 7, the vacuum pump 6 and the modified synthesis reaction kettle 3 respectively.

[0036] During implementation, the structure of the absorption bottle 5 is preferably a spherical structure, and the absorption bottle 5 is filled with an absorbent to absorb the small molecular sulfide generated in the modification synthesis, and the absorption bottle 5, the vacuum pump 6 and the cooling reflux device 7 are combined to realize the reflux of the small molecules. During implementation, the absorbent filled in the absorption bottle is a strong alkaline solution, and the small molecular sulfide (high temperature) generated in the modification synthesis enters the cooling reflux device 7 to cool down under the vacuum environment of the vacuum pump 6, and then refluxes into the absorption bottle 5 to be absorbed and processed by the absorbent.

[0037] In this embodiment, the polysulfide rubber modification synthesis device also includes a nitrogen bottle connected to the nitrogen inlet pipe 1, and a regulating valve is also provided between the nitrogen bottle and the nitrogen inlet pipe 1 to control and adjust the flow rate of nitrogen entering the modification synthesis reactor 3.

[0038] In this embodiment, the polysulfide rubber modification synthesis device further includes a power supply connected to the ultraviolet lamp 2. A control switch is provided between the ultraviolet lamp 2 and the power supply. The control switch is used to turn on or off the power supply to the ultraviolet lamp 2, thereby adjusting the turning on and off of the ultraviolet light, so that the ultraviolet lamp can intermittently irradiate the modification synthesis reactor 3.

[0039] Example 2

[0040] See also Figure 1 On the basis of Example 1, the polysulfide rubber modification synthesis device provided in this embodiment further includes a heating and cooling water jacket 4 arranged on the outer wall of the modification synthesis reactor 3; the temperature in the modification synthesis reactor 3 during the reaction is controlled by the heating and cooling water jacket 4. For example, when a high temperature is required during the reaction, the heating and cooling water jacket 4 is filled with circulating hot water to heat the modification synthesis reactor 3; when a low temperature is required during the reaction, the heating and cooling water jacket 4 is filled with circulating cooling water to cool the modification synthesis reactor 3, thereby meeting the temperature requirement during the modification synthesis reaction.

[0041] In this embodiment, the polysulfide rubber modification synthesis device further includes a temperature sensor 8 disposed on the modification synthesis reactor 3. The temperature sensor 8 extends from the top of the modification synthesis reactor 3 into the modification synthesis reactor 3. When in use, the temperature measuring end of the temperature sensor 8 is placed in the reactants in the modification synthesis reactor 3 to detect the temperature during the modification synthesis reaction, so as to facilitate the heating and cooling water jacket 4 to be heated or cooled according to the measured temperature.

[0042] Example 3

[0043] See also Figure 1 On the basis of Example 1, the polysulfide rubber modification synthesis device provided in this embodiment further includes a stirrer 9 and a stirring motor; the stirring motor is placed on the modification synthesis reactor 3, one end of the stirrer 9 extends into the modification synthesis reactor 3, and the other end of the stirrer 9 is placed outside the modification synthesis reactor 3 and connected to the stirring motor.

[0044] In this embodiment, the agitator 9 includes a stirring rod, a stirring blade is provided on one end of the stirring rod, and the other end of the stirring rod is connected to a stirring motor. The stirring motor is placed on the top of the modified synthesis reactor 3, and the stirring blade is placed in the modified synthesis reactor 3 for stirring the materials in the modified synthesis reactor 3.

[0045] The polysulfide rubber modification synthesis device provided by the utility model has the following modification synthesis reaction process:

[0046] 1) Open the discharge valve at the bottom of the chain-breaking reducing agent storage tank and the discharge valve at the bottom of the polysulfide rubber storage tank, add the chain-breaking reducing agent and liquid polysulfide rubber (liquid polysulfide rubber) into the modified synthesis reactor 3 through the feed port at a mass ratio of 1:100, fill nitrogen into the modified synthesis reactor 3 through the nitrogen inlet pipe 1, and drive the stirrer 9 to work by the stirring motor. Under stirring and nitrogen atmosphere, adjust the temperature in the modified synthesis reactor 3 to 90° C. by heating and cooling the water jacket 4 to start the chain-breaking reaction; at the same time, when the chain-breaking reaction starts, the vacuum pump 6 Start to evacuate to reflux the low molecular volatiles (i.e., small molecular sulfides) generated during the chain scission process; after 4 hours of chain scission reaction, the chain scission reducing agent and the liquid polysulfide rubber form a low molecular raw rubber mixture in the modified synthesis reactor 3, and the agitator 9 is turned off; and the generated low molecular volatiles flow from the volatile outlet on the modified synthesis reactor 3 to the cooling reflux device 7. In the vacuum environment formed by the vacuum pump 6, the low molecular volatiles enter the cooling reflux device 7, cool down, and then flow to the absorption bottle 5 in the form of liquid through the reflux pipe, and are absorbed by the absorbent in the absorption bottle 5;

[0047] 2) At this time, the discharge valve at the bottom of the diene terminal compound storage tank is opened, and the diene terminal compound is added to the low molecular weight rubber mixture, and then the discharge valve at the bottom of the photoinitiator storage tank is opened to add the photoinitiator;

[0048] 3) The temperature in the modified synthesis reactor 3 is adjusted to 60°C by heating and cooling the water jacket 4, and the ultraviolet lamp 2 is turned on in a nitrogen atmosphere. The ultraviolet radiation generated by the ultraviolet lamp 2 is irradiated on the reactants in the modified synthesis reactor 3. Under ultraviolet light, the low molecular rubber mixture, the diene terminal compound and the photoinitiator undergo a synthesis reaction. In this process, since ultraviolet light generates heat, the synthesis reaction temperature is prevented from being too high. The ultraviolet light is adjusted by the control switch to be carried out at an intermittent time, that is, after each irradiation of the ultraviolet lamp 2 for 5 minutes, the ultraviolet lamp 2 is turned off for 5 minutes, and this cycle is repeated many times until the reaction is completely completed. The obtained synthetic product is discharged from the modified synthesis reactor 3 from the discharge port, and then washed and dried to obtain the modified polysulfide rubber. In the utility model, washing and drying are respectively achieved by conventional existing washing devices (such as washing kettles) and drying devices (such as drying ovens) in the industry.

[0049] The polysulfide rubber modification synthesis device of the utility model has a simple structure and is easy to operate. The modification synthesis of liquid polysulfide rubber is completed by a two-step method, the reaction steps are few, and the raw material cost is low, so the device is suitable for batch and large-scale production.

[0050] The specific implementation methods described above further illustrate the purpose, technical solutions and beneficial effects of the utility model in detail. It should be understood that the above description is only the specific implementation method of the utility model and is not used to limit the protection scope of the utility model. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the utility model should be included in the protection scope of the utility model.

Claims

1. A polysulfide rubber modification synthesis device, characterized in that: The invention comprises an ultraviolet lamp (2), a modified synthesis reactor (3), an absorption bottle (5), a vacuum pump (6) and a cooling reflux device (7); the ultraviolet lamp (2) is arranged outside the modified synthesis reactor (3), and the ultraviolet light generated by the ultraviolet lamp (2) is radiated onto the modified synthesis reactor (3); the modified synthesis reactor (3) is also externally connected to a nitrogen inlet pipe (1); the absorption bottle (5) is respectively connected to the cooling reflux device (7), the modified synthesis reactor (3) and the vacuum pump (6).

2. The polysulfide rubber modified synthesis device according to claim 1, characterized in that: The absorption bottle (5) is connected to a reflux pipe, which is respectively connected to a cooling reflux device (7), a vacuum pump (6) and a modified synthesis reaction kettle (3).

3. The polysulfide rubber modified synthesis device according to claim 1, characterized in that: The polysulfide rubber modified synthesis device also includes a nitrogen bottle connected to the nitrogen inlet pipe (1).

4. The polysulfide rubber modified synthesis device according to claim 1, characterized in that: The polysulfide rubber modification synthesis device also includes a chain-breaking reducing agent storage tank, a polysulfide rubber storage tank, a diene terminal compound storage tank and a photoinitiator storage tank, which are respectively connected to the modification synthesis reaction kettle (3).

5. The polysulfide rubber modification synthesis device according to claim 1, characterized in that: The polysulfide rubber modification synthesis device also includes a heating and cooling water jacket (4) arranged on the outer wall of the modification synthesis reaction kettle (3).

6. The polysulfide rubber modification synthesis device according to claim 5, characterized in that: The polysulfide rubber modification synthesis device further comprises a temperature sensor (8) arranged on the modification synthesis reaction kettle (3).

7. The polysulfide rubber modification synthesis device according to claim 1, characterized in that: The polysulfide rubber modified synthesis device also includes a power source connected to the ultraviolet lamp (2).

8. The polysulfide rubber modification synthesis device according to claim 7, characterized in that: A control switch is provided between the ultraviolet lamp (2) and the power supply.

9. The polysulfide rubber modification synthesis device according to any one of claims 1 to 8, characterized in that: The polysulfide rubber modified synthesis device also includes a stirrer (9) and a stirring motor; the stirring motor is placed on the modified synthesis reactor (3), one end of the stirrer (9) extends into the modified synthesis reactor (3), and the other end of the stirrer (9) is placed outside the modified synthesis reactor (3) and connected to the stirring motor.

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