CN114950294B - Device for preparing polythioether rubber by continuous light synthesis - Google Patents

Device for preparing polythioether rubber by continuous light synthesis Download PDF

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CN114950294B
CN114950294B CN202111505890.8A CN202111505890A CN114950294B CN 114950294 B CN114950294 B CN 114950294B CN 202111505890 A CN202111505890 A CN 202111505890A CN 114950294 B CN114950294 B CN 114950294B
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kettle
rubber
nitrogen
liquid
polythioether
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CN114950294A (en
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李智辉
靳耿栓
郭庆远
毛思鳗
景星凯
贺欢
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Xi'an Xifei Chenguang Aviation Technology Co.,Ltd.
Xian Jiaotong University
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Xi'an Aircraft Industry Group Chenguang Industry And Trade Co ltd
Xian Jiaotong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/123Ultra-violet light
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G75/00Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
    • C08G75/02Polythioethers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00004Scale aspects
    • B01J2219/00006Large-scale industrial plants
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock

Abstract

The device comprises a material mixing kettle, a liquid material tank, a nitrogen bottle, a solid material injection reaction kettle, a flow meter, a synthesis reaction kettle, a water washing kettle, a water drier, a dewatering drier, a water washing kettle, a dewatering drier and a nitrogen bottle.

Description

Device for preparing polythioether rubber by continuous light synthesis
Technical Field
The invention relates to the technical field of aviation material polythioether rubber preparation, in particular to a device for preparing polythioether rubber by continuous photosynthesis.
Background
The polysulfide sealant is an elastic sealing material with good cohesive force formed by chemically crosslinking (vulcanizing) liquid polysulfide rubber with small molecular weight, and the polysulfide sealant is a key sealing material used for aircraft engines all the time, because the polysulfide sealant has the characteristics of excellent oil resistance, low air permeability, good weather resistance and the like, the virgin rubber-liquid polysulfide rubber for preparing the polysulfide sealant is prepared from dihalogenSynthetic rubber obtained by polycondensation of alkyl substituted and polysulfide of alkali metal or alkaline earth metal, the structure is [ -CH 2 -CH 2 -S x -] n Because of more sulfur bonds in the structure, the rubber has good endurance capacity to air, fuel, water vapor, non-polar liquid and atmospheric environment, always maintains reliable adhesive force to the surfaces of various materials, has a relatively wide temperature range, and is particularly suitable for sealing parts such as airplane fuel tanks, cockpit, watertight compartments and the like. Polysulphide rubber was reported by Switzerland scientists in 1838, and in 1928 Thiokol Corp, inc. first produced a liquid tetrasulphethylene polymer useful as a sealing material
Figure BDA0003404359100000011
A. The vigorous application of the product promotes the rapid development of polysulfide rubber. China carries out intermediate tests by the chemical research institute of the Jinxi in 1955, and the yield can meet the domestic requirements. Polysulfide rubbers have been produced in soviet union, germany, france, italy, belgian, japan, etc. At present, only Germany, japan, russia and China have production. At present, polysulfide rubber is still an important material for application in the aviation industry of China, although polysulfide rubber has many advantages, liquid polysulfide rubber still has defects along with the continuous improvement of application environment requirements, liquid polysulfide rubber raw rubber contains a large number of disulfide bonds, and the liquid polysulfide rubber can be firstly broken under the heating condition, so that the heat resistance of a sealant is reduced, and then polysulfide rubber is derived. Like polysulfide rubber, polysulfide has the advantages of polysulfide rubber because it contains sulfur atoms in the main molecular chain. And the main chain of the polythioether molecule only contains a monothio bond, namely a thioether bond (the C-S bond energy is 289 kJ/mol), and the polysulfide rubber is a disulfide bond (-the S-S bond energy is 246 kJ/mol), so that the heat resistance of the polythioether polymer is 50 ℃ higher than that of liquid polysulfide rubber, the curing process of raw polythioether rubber is not influenced by the environmental humidity, a sealant which can resist hot air and fuel oil with the temperature of 180 ℃ can be prepared, and the service life of the sealant is 3-10 times that of the polysulfide sealant. PRC company and Dow Corning company in the United states successfully develop dozens of series aviation polythioethers with different functions, such as PR-2001, PR-2201, CS5306 and the likeAnd (3) a sealant. The research of China on the polythioether rubber is mainly performed by Beijing aviation material institute and Jinxi chemical research institute, only a small amount of domestic polythioether products exist at present, and the liquid polythioether and the production equipment thereof become the key point for solving the current problems.
The above information disclosed in this background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not form the prior art that is well known to those of ordinary skill in the art.
Disclosure of Invention
The invention aims to provide a device for preparing polythioether rubber by continuous photosynthesis, and in order to realize the aim, the invention provides the following technical scheme:
the device for preparing the polythioether rubber by continuous photosynthesis comprises,
a nitrogen gas bottle for storing nitrogen gas,
a liquid raw material tank for storing the liquid raw material for preparing the polythioether rubber, the liquid raw material tank is communicated with the nitrogen cylinder,
a mixing kettle for storing solid raw materials for preparing the polythioether rubber, wherein the mixing kettle is communicated with a liquid raw material tank and a nitrogen cylinder to mix the solid raw materials and the liquid raw materials to form a mixture, the mixture is injected into the light synthesis reaction kettle under the pressure of nitrogen,
a flow meter provided between the liquid raw material tank and the mixing kettle to measure a flow rate of the liquid raw material injected into the mixing kettle under nitrogen pressure,
a photosynthetic reaction kettle which is a transparent structure and is communicated with the mixing kettle and the nitrogen bottle,
the photosynthetic reaction kettle comprises an ultraviolet light source arranged in the photosynthetic reaction kettle to provide ultraviolet light, the mixture is subjected to a photosynthetic reaction under the irradiation of the ultraviolet light to generate liquid virgin rubber, the liquid virgin rubber is pushed to the water washing kettle under the pressure of nitrogen,
a water washing kettle which is communicated with the photosynthesis reaction kettle and the nitrogen bottle to wash the liquid virgin rubber, the liquid virgin rubber is conveyed to a dewatering dryer under the pressure of nitrogen,
a dewatering dryer connected with the washing kettle and the nitrogen bottle, wherein the dewatering dryer dries the liquid virgin rubber to form finished virgin rubber,
and the gas washing tank is communicated with the mixing kettle, the photosynthesis reaction kettle, the water washing kettle and the dewatering dryer to clean waste gas.
The device for preparing the polythioether rubber by continuous photosynthesis further comprises a fan facing the reaction kettle, and the surface of the reaction kettle is provided with cooling fins.
In the device for preparing the polythioether rubber by continuous photosynthesis, a communicating pipeline of the nitrogen cylinder is provided with a pressure reducing valve and an electromagnetic valve.
In the device for preparing the polythioether rubber by continuous photosynthesis, the top end of the mixing kettle is provided with a solid feeding hole.
In the device for preparing the polythioether rubber by continuous photosynthesis, the photosynthesis reaction kettle is provided with a pressure gauge for measuring pressure.
In the device for preparing the polythioether rubber by continuous photosynthesis, the bottom end of the washing kettle is provided with a wastewater outlet for discharging wastewater.
In the technical scheme, the device for preparing the polythioether rubber by continuous photosynthesis has the following beneficial effects: the device for preparing the polythioether rubber by continuous photosynthesis adopts an electrical control system, an integrated raw material tank body, a mixing kettle, a photosynthetic reaction kettle, an ultraviolet light source, inert gas protection, a circulating cooling system, a washing system, a tail gas collection and discharge bin and the like, and can automatically execute the synthesis of a program only by weighing raw materials and adjusting parameters through equipment, so that the efficiency of the test can be greatly improved, meanwhile, the whole process of the equipment is in a sealed state, the release of gas in the synthesis process can be reduced, the emission of odor to pollute the environment can be reduced, the device has the advantages of rapidness, accuracy, controllable products and the like, can be used for continuously modifying the polythioether and synthesizing the polythioether, has the characteristics of good sealing property, adjustable proportion, controllable pollution, controllable odor and good safety, and simultaneously, the efficiency and the times of synthesizing the polythioether are greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is a schematic diagram showing the structure of one embodiment of an apparatus for continuous photosynthetic production of polythioether rubber.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations or positional relationships based on those shown in the drawings, merely for convenience of description and simplicity of description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described in detail with reference to the accompanying drawings.
As shown in FIG. 1, an apparatus for continuous photosynthetic preparation of polythioether rubber comprises:
a nitrogen gas cylinder 1 which stores nitrogen gas,
a liquid raw material tank 4 for storing a liquid raw material for preparing the polythioether rubber, the liquid raw material tank 4 being communicated with the nitrogen gas cylinder 1,
a mixing kettle 5 for storing solid raw materials for preparing the polythioether rubber, wherein the mixing kettle 5 is communicated with a liquid raw material tank 4 and a nitrogen gas bottle 1 to mix the solid raw materials and the liquid raw materials to form a mixture, the mixture is injected into a light synthesis reaction kettle 7 under the pressure of nitrogen gas,
a flow meter 18 provided between the liquid raw material tank 4 and the mixing kettle 5 to measure a flow rate of the liquid raw material injected into the mixing kettle 5 under a nitrogen pressure,
a photosynthetic reaction kettle 7 which is a transparent structure and is communicated with the mixing kettle 5 and the nitrogen bottle 1,
the photosynthetic reaction kettle 7 comprises an ultraviolet light source 8 arranged in the photosynthetic reaction kettle to provide ultraviolet light, the mixture is subjected to a photosynthetic reaction under the irradiation of the ultraviolet light to generate liquid virgin rubber, the liquid virgin rubber is pushed to a water washing kettle 12 under the pressure of nitrogen,
a water washing kettle 12 which is communicated with the photosynthesis reaction kettle 7 and the nitrogen gas bottle 1 to wash the liquid virgin rubber with water, the liquid virgin rubber is conveyed to a dewatering dryer 14 under the pressure of nitrogen gas,
a dewatering dryer 14 connected with the water washing kettle 12 and the nitrogen gas bottle 1, wherein the dewatering dryer 14 dries the liquid virgin rubber to form finished virgin rubber,
and the gas washing tank 17 is in gas communication with the mixing kettle 5, the photosynthesis reaction kettle 7, the water washing kettle 12 and the dewatering dryer 14 to wash the waste gas.
In the preferred embodiment of the device for preparing the polythioether rubber by continuous photosynthesis, the device further comprises a fan 9 facing the reaction kettle, and the surface of the reaction kettle is provided with a radiating fin 10.
In the preferred embodiment of the device for preparing the polythioether rubber by continuous photosynthesis, a communication pipeline of the nitrogen cylinder 1 is provided with a pressure reducing valve 2 and an electromagnetic valve 3.
In the preferred embodiment of the device for preparing the polythioether rubber by continuous photosynthesis, the top end of the mixing kettle 5 is provided with a solid feeding hole 6.
In the preferred embodiment of the device for preparing the polythioether rubber by continuous photosynthesis, the photosynthesis reaction kettle 7 is provided with a pressure gauge 11 for measuring pressure.
In the preferred embodiment of the continuous photosynthesis apparatus for preparing polythioether rubber, the bottom end of the water washing kettle 12 is provided with a waste water outlet 13 for discharging waste water.
In one embodiment, the dewatering dryer 14 comprises a heating resistor 15 for heating.
In one embodiment, the liquid feed tank 4 is replaced by replacing the feed tank or by filling, and the required initiator and other solid materials are added through the solid feed inlet 6. The system can be opened after the raw materials are injected, the raw materials in the liquid raw material tank 4 are injected into the mixing kettle 5 through the flow meter under the existence of positive pressure nitrogen to be stirred and mixed with solid raw materials, after the mixing time is reached, the liquid is continuously injected into the photosynthetic reaction kettle 7 through the pushing of the nitrogen, the photosynthetic reaction kettle is made of transparent quartz, the ultraviolet light source 8 starts the photosynthetic reaction after being opened, the reaction kettle performs heat dissipation and cooling through a cooling fan 9 and a radiating fin 10 in the reaction process, the synthesized liquid crude rubber is then pushed into a washing kettle 12 through nitrogen, after multiple times of washing, the waste water is discharged through an outlet 13, the liquid crude rubber is further conveyed into a dewatering dryer to remove the moisture in the rubber, and the finished product crude rubber after dewatering is sent out through an outlet 16. In the whole gas loop, the positive pressure gas comes from the gas steel cylinder 1, and is controlled to be opened through a pressure reducing valve and an electromagnetic valve, and the waste gas in the mixing kettle 5, the photosynthesis reaction kettle 7, the washing kettle 12 and the dewatering dryer is finally and uniformly discharged into the washing tank 17 through an exhaust pipeline in the conveying process.
In this test machine, whole experimental flow is carried through gas, liquid fluid coupling to all there is agitating unit in mixing and the reation kettle, at first made things convenient for the washing of system, reation kettle 7 adopts the mode of upper and lower gland simultaneously, and central authorities are transparent quartz, make things convenient for in the observation of reaction, also convenient for simultaneously dismantle and the inside washing of reation kettle.
In one embodiment, the device also comprises a PLC control system for controlling the experimental process in the device, and the polysulfide and polythioether rubber and raw materials have strong odor, so that the invention adopts a closed pipeline nitrogen positive pressure conveying mode to reduce the emission of the odor, and simultaneously, exhaust gas is collected intensively. The ultraviolet light initiated synthesis reaction of the device can continuously have the advantages of rapidness, accuracy, controllable products and the like, and the development of the polythioether sealant for aviation in China is promoted.
Finally, it should be noted that: the embodiments described are only a part of the embodiments of the present application, and not all embodiments, and all other embodiments obtained by those skilled in the art without making creative efforts based on the embodiments in the present application belong to the protection scope of the present application.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.

Claims (6)

1. An apparatus for continuous photosynthesizing a polythioether rubber, comprising:
a nitrogen gas bottle for storing nitrogen gas,
a liquid raw material tank for storing the liquid raw material for preparing the polythioether rubber, the liquid raw material tank is communicated with the nitrogen cylinder,
a mixing kettle for storing solid raw materials for preparing the polythioether rubber, wherein the mixing kettle is communicated with a liquid raw material tank and a nitrogen cylinder to mix the solid raw materials and the liquid raw materials to form a mixture, the mixture is injected into the light synthesis reaction kettle under the pressure of nitrogen,
a flow meter provided between the liquid raw material tank and the mixing kettle to measure a flow rate of the liquid raw material injected into the mixing kettle under nitrogen pressure,
a photosynthetic reaction kettle which is a transparent structure and is communicated with the mixing kettle and the nitrogen bottle,
the photosynthetic reaction kettle comprises an ultraviolet light source arranged in the photosynthetic reaction kettle to provide ultraviolet light, the mixture is subjected to a photosynthetic reaction under the irradiation of the ultraviolet light to generate liquid virgin rubber, the liquid virgin rubber is pushed to the water washing kettle under the pressure of nitrogen,
a water washing kettle which is communicated with the photosynthesis reaction kettle and the nitrogen bottle to wash the liquid virgin rubber, the liquid virgin rubber is conveyed to a dewatering dryer under the pressure of nitrogen,
a dewatering dryer connected with the washing kettle and the nitrogen bottle, wherein the dewatering dryer dries the liquid virgin rubber to form finished virgin rubber,
and the gas washing tank is communicated with the mixing kettle, the photosynthesis reaction kettle, the water washing kettle and the dewatering dryer to clean waste gas.
2. The apparatus of claim 1, further comprising a fan facing the reaction vessel, wherein the surface of the reaction vessel is provided with heat dissipation fins.
3. The apparatus for continuous photosynthetically preparing polythioether rubber according to claim 1, wherein the communication line of the nitrogen gas cylinder is provided with a pressure reducing valve and an electromagnetic valve.
4. The apparatus for continuous photosynthetically preparing polythioether rubber of claim 1, wherein the top of said mixing kettle is provided with a solid feed inlet.
5. The apparatus for continuous photosynthesizing polyether rubber as defined in claim 1, wherein said photosynthesizing reaction kettle is provided with a pressure gauge for measuring pressure.
6. The apparatus for continuous photosynthesizing polyether rubber as defined in claim 1, wherein a waste water outlet for discharging waste water is arranged at the bottom end of the washing kettle.
CN202111505890.8A 2021-12-10 2021-12-10 Device for preparing polythioether rubber by continuous light synthesis Active CN114950294B (en)

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US3992274A (en) * 1974-12-23 1976-11-16 Hooker Chemicals & Plastics Corporation Sensitized production of sulfhydryl compounds using ultra violet radiation
BR9812092A (en) * 1997-02-19 2000-11-21 Courtaulds Aerospace Inc Polyetherether, method for the production of polyester and polymerizable composition
US20160130400A1 (en) * 2014-11-06 2016-05-12 Solvay Sa Continuous process for producing poly(arylene sulfide)
CN105032323B (en) * 2015-07-30 2018-01-12 中国科学院化学研究所 Polymerizing reactor
CN111434705B (en) * 2019-01-14 2022-03-15 中国石油化工股份有限公司 Modified liquid rubber and preparation method and application thereof
CN214183030U (en) * 2020-12-11 2021-09-14 成都晨光博达橡塑有限公司 Photochemical reaction kettle

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