CN110698713A - High-dispersity silica gel foaming agent and preparation method thereof - Google Patents
High-dispersity silica gel foaming agent and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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Abstract
The invention relates to a preparation method of a foaming agent, in particular to a high-dispersity silica gel foaming agent and a preparation method thereof, and belongs to the technical field of rubber preparation. A high-dispersity silica gel foaming agent is prepared by mixing the following components: 100 parts of azodiisobutyronitrile, 1-20 parts of a separant and 5-20 parts of a liquid dispersant. According to the invention, the separant is added into the azobisisobutyronitrile before the jet milling, so that the agglomeration and caking problems of the foaming agent after the jet milling are greatly reduced, meanwhile, the separant and the azobisisobutyronitrile are mixed more uniformly after the co-crushing, the granularity of the separant is also greatly reduced, and the filling and reinforcing effects of the separant on the high-temperature vulcanized silicone rubber are improved; in addition, the addition of the separant reduces the concentration of the azobisisobutyronitrile, so that the safety of the azobisisobutyronitrile is improved to a certain extent.
Description
Technical Field
The invention relates to a preparation method of a foaming agent, in particular to a high-dispersity silica gel foaming agent and a preparation method thereof, and belongs to the technical field of rubber preparation.
Background
Silicone rubber is a linear organosiloxane polymer having a backbone composed of alternating siloxane bonds (Si-O) and pendant groups composed of organic groups (e.g., methyl, ethyl, vinyl, phenyl, trifluoropropyl, etc.). Due to the special structure, the silicone rubber has a plurality of excellent performances which can be simultaneously possessed by a plurality of other materials, such as excellent high temperature resistance and low temperature resistance, excellent oil resistance, solvent resistance, ultraviolet resistance and radiation resistance, good aging resistance, excellent electrical insulation, chemical stability, physiological inertia and the like.
The silicone porous elastomer prepared after foaming is a silicone rubber foam material, which is also called sponge silicone rubber and microporous silicone rubber. According to the cell structure, there are closed-cell, open-cell and mixed-cell silicone rubbers. Generally, open-cell foams have lower mechanical strength but better compressive stress relaxation properties, while closed-cell foams have better mechanical strength but poorer compressive stress relaxation properties. The properties of the hybrid cell foam are intermediate.
Silicone rubber foams can be divided into room temperature vulcanized silicone Rubber (RTV) foams and high temperature vulcanized silicone rubber (HTV) foams. The room temperature vulcanized silicone rubber foam is a spongy elastomer which is prepared by vulcanizing and foaming a condensed hydroxyl-terminated silicone rubber serving as a base material, a hydroxyl silicone oil serving as a foaming agent and a chloroplatinic acid complex serving as a catalyst at room temperature. The high-temperature vulcanized silicone rubber foam is suitable for in-situ foaming forming and has the functions of filling, sealing, shock absorption and the like. The high-temperature vulcanized foam silicone rubber is prepared by uniformly mixing silicone rubber with the molecular weight of 50-100 ten thousand, inorganic filler, foaming agent and vulcanizing agent, and then thermally vulcanizing and foaming the mixed rubber to obtain the silicone rubber foam. The high-temperature vulcanized foam silicon rubber can be molded into foam plates for use after cutting, or can be extruded and vulcanized by continuous hot air to form silicon rubber foam strips with various shapes and sections.
In the prior art, the foaming agent for free foaming of high-temperature vulcanized silicone rubber has the following problems:
(1) because the vulcanization speed is high, the high-temperature vulcanized silicone rubber requires that the foaming agent is quickly decomposed at about 100 ℃, and conventional chemical foaming agents such as azodicarbonamide (foaming agent ADC), sodium bicarbonate, 4 '-oxybisbenzenesulfonylhydrazide (foaming agent OBSH/OT), p-toluenesulfonylurea (foaming agent RA), N' -dinitrosopentamethylenetetramine (foaming agent DPT, which is also foaming agent H), urea (foaming agent BK), p-toluenesulfonylhydrazine (foaming agent TSH), benzenesulfonylhydrazide (foaming agent BSH) and the like can not simultaneously meet the requirements of uniform foaming and smooth and fine product surfaces when being used singly or compounded;
(2) azodiisobutyronitrile powder is high in danger, has the problems of self-accelerated decomposition and energy accumulation after being heated, and has extremely high potential explosion hazard after the temperature reaches 50-60 ℃;
(3) azodiisobutyronitrile powder has strong crystallinity, and ultrafine powder after being crushed has the problem of agglomeration and crystallization, so that the azodiisobutyronitrile powder has poor dispersibility in high-temperature vulcanized silicone rubber, the foam holes of the produced product are coarse and uneven, and the defects of fish eyes and pinholes and the like exist on the surface of the product;
(4) the fineness of azodiisobutyronitrile powder on the market is not enough, so that foam holes of a foaming product are directly large;
(5) the powdery azodiisobutyronitrile is dangerous and has serious dust problem, and the high toxicity of the powder greatly threatens the physical and psychological health of staff in a workplace;
(6) the powdery azodiisobutyronitrile powder is easy to deposit and agglomerate or form false agglomerates in the storage process, great inconvenience is brought to subsequent production and batching, and even explosion accidents are caused in the artificial crushing process;
(7) the powdery azodiisobutyronitrile is sensitive to collision and heat in the transportation process, and the azodiisobutyronitrile with high purity and high concentration has poor stability after being interfered by external energy, so that explosion accidents are easy to occur;
(8) the introduction of moisture in the process of crushing the azodiisobutyronitrile crystals can affect the quality of the product and accelerate agglomeration.
Disclosure of Invention
The invention aims to provide a high-dispersity silica gel foaming agent which is prepared by modifying azobisisobutyronitrile, and aims to overcome the technical defects of high danger, easy caking, poor dispersity and the like of azobisisobutyronitrile powder serving as the foaming agent.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high-dispersity silica gel foaming agent is prepared by mixing the following components: 100 parts of azodiisobutyronitrile, 1-20 parts of a separant and 5-20 parts of a liquid dispersant. During the production of the foaming agent, the separant needs to be mixed with the azobisisobutyronitrile in advance so as to avoid the risk that the powdery azobisisobutyronitrile is easy to explode in the air, and in the subsequent crushing process, the co-crushing efficiency is improved, so that the fineness of the azobisisobutyronitrile is higher during crushing; the liquid dispersant is used for improving the dispersibility of the azodiisobutyronitrile, effectively reducing dust pollution, improving the safety and the quality stability of the foaming agent and endowing a product with a more exquisite foam structure. The release agent and the liquid dispersant are used together, and have a synergistic effect on the performance of the foaming agent.
Preferably, the foaming agent is prepared by mixing the following components: 100 parts of azodiisobutyronitrile, 5-10 parts of a separant and 10-20 parts of a liquid dispersant.
Preferably, the azobisisobutyronitrile is commercial industrial grade crystal or powder, and the separant is one or a mixture of inorganic filler, fatty acid and derivatives thereof. Further, the inorganic filler is selected from one or a mixture of more of calcium carbonate, talcum powder, montmorillonite, silicon dioxide, magnesium carbonate, zinc oxide, bentonite, kaolin or ferric oxide; the fatty acid and its derivative is selected from one or more of stearic acid, zinc stearate, calcium stearate, magnesium stearate, aluminum stearate, barium stearate, glyceryl stearate, lauric acid, zinc laurate, calcium laurate, magnesium laurate, aluminum laurate, barium laurate, myristic acid, zinc myristate, calcium myristate, magnesium myristate, aluminum myristate, barium myristate, oleic acid, zinc oleate, calcium oleate, magnesium oleate, aluminum oleate, barium oleate or glyceryl oleate.
Preferably, the liquid dispersant is selected from one or more of methyl silicone oil, hydroxyl silicone oil, silane coupling agent, polyether modified silicone oil, titanate coupling agent, mineral oil, epoxidized soybean oil, dioctyl phthalate (DOP), dioctyl adipate (DOA), oleic acid, glyceryl oleate, polyethylene glycol or polyethylene glycol glyceride.
Preferably, the foaming agent also comprises silicon rubber, and the silicon rubber accounts for 20-100 parts by weight of the sum of the parts by weight of the azodiisobutyronitrile, the separant and the liquid dispersant being 100 parts. Further, the silicon rubber is high-temperature vulcanized silicon rubber with Shore hardness of 10-33.
Preferably, the foaming agent is prepared by mixing the following components: 100 parts of azodiisobutyronitrile, 5-10 parts of silicon dioxide, 1-2 parts of zinc stearate, 1-2 parts of ferric oxide, 8-10 parts of methyl silicone oil, 2-5 parts of polyethylene glycol glyceride, 2-7 parts of a silane coupling agent and 1-3 parts of glyceryl oleate.
A preparation method of the high-dispersity silica gel foaming agent comprises the following steps:
(1) firstly, uniformly mixing azodiisobutyronitrile and a separant by using a fluidized bed;
(2) deeply crushing the mixed powder in the step (1) by using a jet mill with nitrogen protection, and controlling the median particle size to be 5-20 microns;
(3) and (3) introducing the azobisisobutyronitrile superfine powder obtained in the step (2) into a fluidized bed from the bottom, and then atomizing and spraying the liquid dispersing agent from the top of the fluidized bed to obtain fully wetted and dispersed wet powder, namely the foaming agent product. The resulting azobisisobutyronitrile blowing agent is sold as a commercial product.
Preferably, the method further comprises a step (4), specifically: (4) and (4) uniformly mixing the wet powder obtained in the step (3) and silicon rubber by using an internal mixer, and cooling by adopting a cooling water introducing mode through an internal mixer jacket in the mixing process to obtain the pasty foaming agent.
Compared with the prior art, the invention has the beneficial effects that:
1. the isolating agent is added into the azobisisobutyronitrile before the jet milling, so that the agglomeration and caking problems of the foaming agent after the jet milling are greatly reduced, meanwhile, the isolating agent and the azobisisobutyronitrile are mixed more uniformly after the co-milling, the granularity of the isolating agent is greatly reduced, and the filling and reinforcing effects of the isolating agent on the high-temperature vulcanized silicone rubber are improved; in addition, the addition of the separant reduces the concentration of the azobisisobutyronitrile, so that the safety of the azobisisobutyronitrile is improved to a certain extent. The decomposition temperature of azodiisobutyronitrile is 100-103 ℃, the foaming agent in the prior art has explosion danger at 50-60 ℃ during co-crushing, and the explosion can be effectively avoided by adding the isolating agent.
2. The nitrogen protection is added in the air flow crushing process, so that the influence of a large amount of water absorption on the stability of a product in the material crushing process is prevented, the direct contact area of the isolating agent and the azodiisobutyronitrile is increased, the explosive mixture of the material and the air can be prevented, and the potential explosion hazard is reduced.
3. The invention adopts the fluidized bed to carry out the mixing operation of materials, thereby avoiding energy accumulation and explosion hidden trouble caused by frictional heat generation in the conventional mechanical stirring process.
4. According to the invention, the liquid dispersant is adopted to improve the dispersibility of the azodiisobutyronitrile, effectively reduce dust pollution, improve the safety and quality stability of the foaming agent and endow the product with a more delicate cell structure.
5. The low-hardness high-temperature vulcanized silicone rubber is used as a carrier, the azodiisobutyronitrile foaming agent is made into a paste, the dispersibility of the foaming agent is further improved through pre-dispersion, the heat insulation effect of the foaming agent is also improved through the isolation and coating effect of the silicone rubber on the azodiisobutyronitrile, and the safety of the foaming agent in the processes of storage, transportation and use is greatly improved.
Drawings
FIG. 1 is an appearance diagram of a foamed article prepared by using the highly dispersible silica gel foaming agents of examples and comparative examples, which are foamed sequentially from top to bottom by using the highly dispersible silica gels of comparative examples 1, 2 and 3 and examples 1, 2 and 3.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Examples 1 to 3
A high-dispersity silica gel foaming agent is prepared by mixing the components shown in Table 1:
TABLE 1 (unit: kg)
The preparation method of the high-dispersity silica gel foaming agent comprises the following specific steps:
(1) firstly, uniformly mixing azodiisobutyronitrile and a separant by using a fluidized bed;
(2) deeply crushing the mixed powder in the step (1) by using a jet mill with nitrogen protection, and controlling the median particle size to be 5-20 microns;
(3) introducing the azobisisobutyronitrile superfine powder obtained in the step (2) into a fluidized bed from the bottom, atomizing and spraying a liquid dispersant from the top of the fluidized bed to obtain fully wetted and dispersed wet powder,
(4) and (3) uniformly mixing the wet powder obtained in the step (3) and silicon rubber by using an internal mixer, wherein the silicon rubber is high-temperature vulcanized silicon rubber with the Shore hardness of 10-33, and a jacket of the internal mixer is cooled by introducing cooling water in the mixing process to obtain the pasty foaming agent.
Comparative examples 1 to 3
A silica gel foaming agent is prepared by mixing the components shown in Table 1.
The properties of the silicone foaming agents prepared in the above examples and comparative examples were compared and used for the production of foamed products, and the differences between the two foamed products were compared, as shown in table 2. The appearance of the foamed product obtained in each example is shown in FIG. 1.
TABLE 2 comparison of Properties
As can be seen from Table 2 and FIG. 1, the high-dispersibility silica gel foaming agent provided by the invention has the advantages of proper hardness and uniform dispersion compared with the conventional azodiisobutyronitrile powder foaming agent, and the prepared foamed product has a bright, smooth and defect-free surface, uniform and fine foam pores, and better tensile strength, tear strength and elongation than the azodiisobutyronitrile powder foaming agent of the comparative example.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The high-dispersity silica gel foaming agent is characterized by being prepared by mixing the following components in parts by weight:
100 parts of azobisisobutyronitrile,
1-20 parts of a release agent,
5-20 parts of a liquid dispersant.
2. The highly dispersible silicone blowing agent of claim 1, wherein: the foaming agent is prepared by mixing the following components:
100 parts of azobisisobutyronitrile,
5-10 parts of a release agent,
10-20 parts of a liquid dispersant.
3. The highly dispersible silicone blowing agent of claim 1, wherein: the azodiisobutyronitrile is a commercial industrial grade crystal or powder, and the separant is one or a mixture of more of inorganic filler, fatty acid and derivatives thereof.
4. The highly dispersible silicone blowing agent of claim 3, wherein: the inorganic filler is selected from one or a mixture of more of calcium carbonate, talcum powder, montmorillonite, silicon dioxide, magnesium carbonate, zinc oxide, bentonite, kaolin or ferric oxide; the fatty acid and its derivative is selected from one or more of stearic acid, zinc stearate, calcium stearate, magnesium stearate, aluminum stearate, barium stearate, glyceryl stearate, lauric acid, zinc laurate, calcium laurate, magnesium laurate, aluminum laurate, barium laurate, myristic acid, zinc myristate, calcium myristate, magnesium myristate, aluminum myristate, barium myristate, oleic acid, zinc oleate, calcium oleate, magnesium oleate, aluminum oleate, barium oleate or glyceryl oleate.
5. The highly dispersible silicone blowing agent of claim 1, wherein: the liquid dispersant is selected from one or more of methyl silicone oil, hydroxyl silicone oil, silane coupling agent, polyether modified silicone oil, titanate coupling agent, mineral oil, epoxidized soybean oil, dioctyl phthalate (DOP), dioctyl adipate (DOA), oleic acid, glyceryl oleate, polyethylene glycol or polyethylene glycol glyceride.
6. The highly dispersible silicone blowing agent of claim 1, wherein: the foaming agent also comprises silicon rubber, and the silicon rubber accounts for 20-100 parts by weight of the total 100 parts by weight of the azodiisobutyronitrile, the separant and the liquid dispersant.
7. The highly dispersible silicone blowing agent of claim 6, wherein: the silicone rubber is high-temperature vulcanized silicone rubber with Shore hardness of 10-33.
8. The highly dispersible silicone blowing agent of claim 1, wherein: the foaming agent is prepared by mixing the following components: 100 parts of azodiisobutyronitrile, 5-10 parts of silicon dioxide, 1-2 parts of zinc stearate, 1-2 parts of ferric oxide, 8-10 parts of methyl silicone oil, 2-5 parts of polyethylene glycol glyceride, 2-7 parts of a silane coupling agent and 1-3 parts of glyceryl oleate.
9. A method for preparing the highly dispersible silicone blowing agent of claim 1, comprising the steps of:
(1) firstly, uniformly mixing azodiisobutyronitrile and a separant by using a fluidized bed;
(2) deeply crushing the mixed powder in the step (1) by using a jet mill with nitrogen protection, and controlling the median particle size to be 5-20 microns;
(3) and (3) introducing the azobisisobutyronitrile superfine powder obtained in the step (2) into a fluidized bed from the bottom, and then atomizing and spraying the liquid dispersing agent from the top of the fluidized bed to obtain fully wetted and dispersed wet powder, namely the foaming agent product.
10. The method of claim 9, wherein: the method also comprises a step (4), which is specifically as follows:
(4) and (4) uniformly mixing the wet powder obtained in the step (3) and silicon rubber by using an internal mixer, and cooling by adopting a cooling water introducing mode through an internal mixer jacket in the mixing process to obtain the pasty foaming agent.
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Cited By (1)
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| CN112592504A (en) * | 2021-03-04 | 2021-04-02 | 山东万圣博化工有限公司 | Paste-like separant and preparation and use methods thereof |
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