CN115505366A - Alpha, omega-dihydroxy polysiloxane, method for producing same and use thereof as sealing material - Google Patents
Alpha, omega-dihydroxy polysiloxane, method for producing same and use thereof as sealing material Download PDFInfo
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- CN115505366A CN115505366A CN202211065909.6A CN202211065909A CN115505366A CN 115505366 A CN115505366 A CN 115505366A CN 202211065909 A CN202211065909 A CN 202211065909A CN 115505366 A CN115505366 A CN 115505366A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention belongs to the technical field of sealing materials, and relates to alpha, omega-dihydroxy polysiloxane, a preparation method thereof and application of the alpha, omega-dihydroxy polysiloxane as a sealing material. The structure of the alpha, omega-dihydroxy polysiloxane is shown as a formula (I), wherein n is a natural number of 800-1500. The alpha, omega-dihydroxy polysiloxane and the preparation method thereof can ensure that the prepared alpha, omega-dihydroxy polysiloxane has good fire resistance, shock resistance, air tightness, water tightness and scrubbing resistance when being used as a sealing material of gaps or holes.
Description
Technical Field
The invention belongs to the technical field of sealing materials, and relates to alpha, omega-dihydroxy polysiloxane, a preparation method thereof and application of the alpha, omega-dihydroxy polysiloxane as a sealing material.
Background
Nuclear power plants and nuclear fuel aftertreatment plants are mostly radioactive plants, and the situations that deformation joints are arranged in the plants, pipelines penetrate through wallboards and the like are common due to the complex process flow, various processes and large quantities of the plants, so that the indexes of the caulking materials, such as radiation resistance, fire resistance, earthquake deformation resistance, airtight and watertight performance, decontamination performance and the like, are high in requirement, the deformation requirement of buildings under external factors is met, meanwhile, the leakage of radiation objects is prevented, the requirements of fire prevention, sealing and radiation resistance are met, and the safety of the surrounding personnel environment is ensured.
In the design of the prior radioactive factory building, the deformation joint caulking and hole plugging materials are usually universal caulking materials in the building market, and the indexes of fire resistance, deformation performance, sealing performance, scrubbing resistance, seismic resistance and the like after irradiation can not meet the radiation safety design requirement of the radioactive factory building, and only can be replaced periodically to meet the use requirement of the factory building.
Therefore, under the condition that the existing caulking sealing material cannot meet the radiation safety of a radioactive factory building, a novel caulking material needs to be researched and developed, so that the caulking method of a deformation joint part and a hole part of the radioactive factory building meets the requirement of a barrier on a boundary, and the integrity of the protection boundary is ensured.
Disclosure of Invention
The invention provides alpha, omega-dihydroxy polysiloxane which has good fire resistance, shock resistance, air tightness, water tightness and scrubbing resistance when used as a sealing material for gaps or holes.
To achieve this object, in a basic embodiment, the present invention provides an α, ω -dihydroxypolysiloxane characterized in that the α, ω -dihydroxypolysiloxane has the formula HO (C) 2 H 6 OSi) n H, the structure is shown as the following formula (I):
wherein n is a natural number of 800-1500.
The second object of the present invention is to provide a method for preparing the above-mentioned α, ω -dihydroxypolysiloxane, so as to better prepare the above-mentioned α, ω -dihydroxypolysiloxane, and the obtained α, ω -dihydroxypolysiloxane can have good fire-resistant, shock-resistant, airtight, watertight and scrub-resistant properties when used as a sealant for gaps or holes.
To achieve the object, in a basic embodiment, the present invention provides a method for preparing the above-mentioned α, ω -dihydroxy polysiloxane, comprising mixing the component A and the component B, polymerizing, curing and molding to obtain the α, ω -dihydroxy polysiloxane,
the component A comprises 10000-50000cps hydroxyl-terminated polydimethylsilane 50 parts, phenyl silicone oil 5-10 parts, fumed silica 5-10 parts, novel silicate flame-retardant composite powder 50-60 parts, and 2-hydroxy-4-methoxybenzophenone 2-5 parts; the preparation method comprises the steps of adding 50 parts of alpha, omega-dihydroxy polydimethylsiloxane into a planetary stirrer, sequentially adding 5 parts of fumed silica, 60 parts of novel silicate flame-retardant composite powder and 5 parts of 2-hydroxy-4-methoxybenzophenone at normal temperature, dispersing for 1 hour at high speed at normal temperature, continuously adding 10 parts of phenyl silicone oil and 2 parts of deionized water, stirring for 15 minutes at high speed, vacuumizing for the next step, and stirring and defoaming for 10 minutes. And discharging and subpackaging after finishing.
The component B comprises, by weight, 10000-50000cps hydroxyl-terminated polydimethylsilane 50 parts, nano calcium carbonate 20-40 parts, nano silicon dioxide powder subjected to surface hydrophobic treatment 20-40 parts, composite flame-retardant graphite 10 parts, graphene oxide 5-10 parts, carbon nano tubes 5-10 parts, carbon black 1-2 parts, KH550 coupling agent 2-5 parts, phenyltrimethoxysilane 2-5 parts, diphenyl dimethoxysilicon 2-5 parts, and an organotin catalyst 0.2-0.5 part.
In a preferred embodiment, the present invention provides a method of preparing an α, ω -dihydroxy polysiloxane as described above, wherein the combined weight ratio of said a-component to said B-component is from 1.
In a preferred embodiment, the present invention provides a process for the preparation of an α, ω -dihydroxy polysiloxane as described above, wherein said polymerization reaction is carried out at a temperature of 15 to 35 ℃ for a time of 20 to 30 minutes.
In a preferred embodiment, the present invention provides a process for preparing an α, ω -dihydroxypolysiloxane as described above, wherein said curing is carried out at a temperature of from 15 to 35 ℃ for a time of from 2 to 7 hours.
It is a third object of the present invention to provide the use of an α, ω -dihydroxypolysiloxane as described above as a sealant for crevices or holes, to enable good fire, shock, air, water, and scrub resistance.
To achieve this object, the present invention provides, in a basic embodiment, the use of an α, ω -dihydroxypolysiloxane as described above as a sealant for gaps or holes.
In a preferred embodiment, the present invention provides the use of an α, ω -dihydroxypolysiloxane as described above as a sealing material for gaps or pores, wherein said gaps or pores are gaps or pores of a radioactive region.
In a preferred embodiment, the present invention provides the use of an α, ω -dihydroxypolysiloxane as described above as a sealing material for gaps or holes, wherein said use is the use of said α, ω -dihydroxypolysiloxane as a sealing material for the caulking of radioactive area deformation joints, or for the blocking of reserved holes.
The alpha, omega-dihydroxy polysiloxane and the preparation method thereof have the beneficial effects that the prepared alpha, omega-dihydroxy polysiloxane has good fire-resistant, shock-resistant, airtight, watertight and scrubbing-resistant performances when being used as a sealing material for gaps or holes.
The alpha, omega-dihydroxy polysiloxane can ensure that caulking plugging of deformation joint parts, fireproof boundaries, radiation partition boundaries and other parts of a radioactive factory building meets various barrier requirements of the boundaries on the premise of meeting deformation requirements of external factors, and ensures the normal operation of the factory building and the integrity of a protection barrier under the working conditions of accidents in the life period.
The alpha, omega-dihydroxy polysiloxane is an organosilicon sealant with medium and high viscosity, excellent fireproof and irradiation-resistant performance, can still keep good performance under long-term gamma irradiation, and is suitable for workshops under long-term irradiation conditions. Meanwhile, the fireproof and flame-retardant composite material has good fireproof and flame-retardant capabilities and airtight and water-tight properties, and is suitable for positions such as structural gaps, holes and the like with fireproof and sealing requirements. In addition, the composite material has excellent tensile property and bonding capability, and is suitable for deformation gaps with displacement resistance and vibration resistance requirements. It still possesses good decontamination ability simultaneously, makes things convenient for the clearance and the maintenance in later stage.
When the alpha, omega-dihydroxy polysiloxane is used as a sealing material for caulking radioactive region deformation joints or blocking reserved holes:
1) The fire resistance limit is 3h;
2) Receive 1X 10 6 A deformation ratio of at least 50% can be maintained after irradiation of a cumulative dose of Gy;
3) Receive 1X 10 6 After irradiation of Gy accumulated dose, the artificial wetland remains intact and is not damaged under the condition of earthquake-resistant class I earthquake force;
4) Receive 1X 10 6 After irradiation with the Gy accumulated dose, the decontamination performance meets the decontamination requirement of a radioactive factory building;
5) Receive 1X 10 6 After irradiation with the Gy accumulated dose, the airtight and watertight performance meets the sealing requirement of the radioactive factory building.
Detailed Description
The following examples further illustrate embodiments of the present invention.
Example 1: preparation of alpha, omega-dihydroxy polysiloxane and basic performance detection
The preparation of alpha, omega-dihydroxy polysiloxane and the basic property test items and results are shown in the following table 1, wherein the property data before curing are measured at the room temperature of 25 ℃ and the relative humidity of 55%.
TABLE 1 preparation of alpha, omega-dihydroxypolysiloxanes and basic Property test items, results
Wherein the component A comprises 10000-50000cps hydroxyl-terminated polydimethylsiloxane (sold on the market) 50 parts, phenyl silicone oil (monophenyl substituted low molecular weight silane sold on the market) 10 parts, fumed silica (nano white powder generated by high-temperature hydrolysis of silicon halide in oxyhydrogen flame, sold on the market) 5 parts, novel silicate flame-retardant composite powder (superfine powder is prepared by calcining and grinding various silicates at high temperature, and the main components are calcium silicate, magnesium silicate and aluminum silicate) 60 parts, and 2-hydroxy-4-methoxybenzophenone (sold on the market, in powder form) 5 parts according to the weight ratio; the preparation method comprises the following steps: adding 50 parts of alpha, omega-dihydroxy polydimethylsiloxane into a planetary stirrer, sequentially adding 5 parts of fumed silica, 60 parts of novel silicate flame-retardant composite powder and 5 parts of 2-hydroxy-4-methoxybenzophenone at normal temperature, dispersing at high speed for 1 hour at normal temperature, continuously adding 10 parts of phenyl silicone oil and 2 parts of deionized water, stirring at high speed for 15 minutes, vacuumizing at the next step, and stirring and defoaming for 10 minutes.
The component B comprises 10000-50000cps hydroxyl-terminated polydimethylsiloxane (sold on the market) 50 parts, nano calcium carbonate (sold on the market) 20 parts, nano silica powder (obtained by performing hydrophobic treatment on the surface of ultrafine microspherical silica powder) subjected to surface hydrophobic treatment, 30 parts of composite flame-retardant graphite (sold on the market) 10 parts, graphene oxide (sheet graphene oxide prepared by a Hummers method, prepared by using materials such as graphite, concentrated sulfuric acid, potassium permanganate, hydrogen peroxide and hydrochloric acid) 5 parts, carbon nanotubes (multi-walled carbon nanotubes) 5 parts, carbon black (sold on the market) 1 part, KH550 coupling agent (silane coupling agent sold on the market) 5 parts, phenyltrimethoxysilane (sold on the market) 5 parts, diphenyldimethoxysilane (sold on the market) 5 parts, organotin catalyst (KRH-4 type organotin catalyst, sold on the market) 0.5 part. The preparation method comprises the following steps: adding 50 parts of alpha, omega-dihydroxy polydimethylsiloxane into a planetary mixer, adding 20 parts of nano calcium carbonate and 30 parts of nano silicon dioxide powder subjected to surface hydrophobic treatment, heating to 120 ℃, and vacuumizing for high-speed dispersion for 30 minutes. Continuously adding 10 parts of composite flame-retardant graphite, 5 parts of graphene oxide, 5 parts of carbon nano tubes and 1 part of carbon black, and continuously stirring at a high temperature of 120 ℃ for 240 minutes. And next, keeping the vacuum and stirring of the equipment, stopping heating, adding 5 parts of KH550 coupling agent, 5 parts of phenyltrimethoxysilane, 5 parts of diphenyldimethoxysilane and 0.5 part of organic tin catalyst when the temperature of the system is reduced to below 50 ℃, stirring at high speed for 30 minutes in vacuum at normal temperature, and keeping the vacuum degree of the system above 0.090Mpa in the whole feeding and stirring process. And discharging and subpackaging after finishing.
Example 2: specific application of alpha, omega-dihydroxy polysiloxane and performance detection after application
Method of use of the α, ω -dihydroxy polysiloxane prepared in example 1 as a sealing material:
1) And uniformly stirring and mixing the components A and B according to the mass ratio of 1.
2) And pouring the uniformly mixed glue stock to a gap position needing construction, and suggesting that the construction is finished within 15 minutes after the mixing, wherein the construction is influenced because the fluidity is gradually reduced along with the solidification of the glue stock after the mixing for 30 minutes.
3) After the completion of the caulking of the sizing material, the primary molding needs 3 to 5 hours, the primary molding is basically cured within 24 to 48 hours, and no external force is applied to the caulking glue within 72 hours.
1) Plugging of wall holes of various radioactive plants or parts
The continuity and the integrity of the civil construction structure are ensured by plugging the through holes of the mechanical pipelines and the cables. According to different requirements of civil structures, each plugging structure has one or more functions as follows:
air tight (no air leakage at 50mm head pressure difference);
watertight (2 m head differential pressure does not leak);
refractory (guarantee 3h refractory limit);
biological shielding (gamma ray shielding effect is equivalent to that of concrete with the same thickness);
personnel safety (if necessary);
the hole blocking structure is not changed under the earthquake-resistant I-type condition (the hole blocking structure is not damaged under the SL-2 earthquake condition).
Stable under irradiation conditions (cumulative dose of gamma radiation over a 50 year lifetime (1X 10) 6 Gy), maintenance of stability)
-contamination of radioactive material is removed (contamination of radioactive material should be removed from the outer surface)
2) Caulking treatment of deformation joint parts of various radioactive factory buildings
In a building structural member, a gap (e.g., a deformation joint, a prefabricated joint, a construction joint, etc.) reserved or assembled between two or more adjacent surfaces is sealed. Each caulking configuration should have one or more of the following functions:
physical, chemical and mechanical Properties (Specification of modified Silicone sealants (MS) GB/T14683-II-F-25 LM type sealants)
Air tightness (50 mm head pressure difference, no gas leakage)
Watertight performance (2 m head pressure difference no leakage)
Refractory performance (guarantee 3h fire endurance)
Radiation resistance (cumulative dose 1X 10 upon gamma irradiation) 6 After Gy, the mechanical properties before and after irradiation do not decrease)
Detergency (percentage radioactive decontamination of the sealing surface should not be lower than 85%, contamination sensitivity should not be greater than 20%)
Seismic performance (integrity of caulking structure under seismic I type conditions)
The α, ω -dihydroxypolysiloxane used as the sealing material was subjected to the performance test, and the test items and test results are shown in table 2 below.
TABLE 2 results of measuring properties of alpha, omega-dihydroxypolysiloxanes used as sealing materials
The above-described embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (8)
1. Alpha, omega-dihydroxy polysiloxane, characterized in that the molecular formula of the alpha, omega-dihydroxy polysiloxane is HO (C) 2 H 6 OSi) n H, the structure is shown as the following formula (I):
wherein n is a natural number of 800-1500.
2. The method of preparing an α, ω -dihydroxy polysiloxane according to claim 1, characterized in that: the preparation method comprises the steps of mixing the component A and the component B, carrying out polymerization reaction, curing and forming to obtain the alpha, omega-dihydroxy polysiloxane,
the component A comprises 10000-50000cps hydroxyl-terminated polydimethylsilane 50 parts, phenyl silicone oil 5-10 parts, fumed silica 5-10 parts, novel silicate flame-retardant composite powder 50-60 parts, and 2-hydroxy-4-methoxybenzophenone 2-5 parts;
the component B comprises, by weight, 10000-50000cps hydroxyl-terminated polydimethylsilane 50 parts, nano calcium carbonate 20-40 parts, nano silicon dioxide powder subjected to surface hydrophobic treatment 20-40 parts, composite flame-retardant graphite 10 parts, graphene oxide 5-10 parts, carbon nano tubes 5-10 parts, carbon black 1-2 parts, KH550 coupling agent 2-5 parts, phenyltrimethoxysilane 2-5 parts, diphenyl dimethoxysilicon 2-5 parts, and an organotin catalyst 0.2-0.5 part.
3. The method of claim 2, wherein: the mixing weight ratio of the component A to the component B is 1.
4. The method of claim 2, wherein: the temperature of the polymerization reaction is 15-35 ℃, and the time is 20-30 minutes.
5. The production method according to claim 2, characterized in that: the temperature of the solidification molding is 15-35 ℃, and the time is 2-7 hours.
6. Use of an α, ω -dihydroxypolysiloxane according to claim 1 as a sealant for gaps or holes.
7. Use according to claim 6, characterized in that: the gap or hole is a gap or hole of the radioactive region.
8. Use according to claim 6, characterized in that: the application is that the alpha, omega-dihydroxy polysiloxane is used as a sealing material for caulking deformation joints of radioactive regions or blocking reserved holes.
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| CN104945909A (en) * | 2015-06-30 | 2015-09-30 | 烟台金润消防工程有限公司 | Medium-density silicone rubber for nuclear power |
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2022
- 2022-09-01 CN CN202211065909.6A patent/CN115505366A/en active Pending
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| CN103122146A (en) * | 2011-11-18 | 2013-05-29 | 镇江亿致能源科技有限公司 | Fireproof and irradiation-resisting room temperature vulcanization two-component silicone foam sealant used in nuclear power station and preparation process thereof |
| CN104945909A (en) * | 2015-06-30 | 2015-09-30 | 烟台金润消防工程有限公司 | Medium-density silicone rubber for nuclear power |
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