CN116082872A - Active rubber isolating agent and preparation method thereof - Google Patents
Active rubber isolating agent and preparation method thereof Download PDFInfo
- Publication number
- CN116082872A CN116082872A CN202310231066.0A CN202310231066A CN116082872A CN 116082872 A CN116082872 A CN 116082872A CN 202310231066 A CN202310231066 A CN 202310231066A CN 116082872 A CN116082872 A CN 116082872A
- Authority
- CN
- China
- Prior art keywords
- parts
- weight
- porous ceramic
- active rubber
- nano porous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920001971 elastomer Polymers 0.000 title claims abstract description 72
- 239000005060 rubber Substances 0.000 title claims abstract description 72
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000919 ceramic Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 229910052909 inorganic silicate Inorganic materials 0.000 claims abstract description 22
- 239000004094 surface-active agent Substances 0.000 claims abstract description 18
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 18
- 239000008158 vegetable oil Substances 0.000 claims abstract description 18
- 239000002861 polymer material Substances 0.000 claims abstract description 16
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims abstract description 15
- 229940063655 aluminum stearate Drugs 0.000 claims abstract description 15
- 238000004945 emulsification Methods 0.000 claims abstract description 15
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 15
- UCPYLLCMEDAXFR-UHFFFAOYSA-N triphosgene Chemical compound ClC(Cl)(Cl)OC(=O)OC(Cl)(Cl)Cl UCPYLLCMEDAXFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 14
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 8
- 239000004952 Polyamide Substances 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002647 polyamide Polymers 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical group [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 7
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 6
- 235000019483 Peanut oil Nutrition 0.000 claims abstract description 5
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 5
- 239000000312 peanut oil Substances 0.000 claims abstract description 5
- 235000019484 Rapeseed oil Nutrition 0.000 claims abstract description 4
- 235000019438 castor oil Nutrition 0.000 claims abstract description 4
- 239000004359 castor oil Substances 0.000 claims abstract description 4
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229920005862 polyol Polymers 0.000 claims description 13
- 150000003077 polyols Chemical class 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229960004050 aminobenzoic acid Drugs 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 125000006850 spacer group Chemical group 0.000 claims 4
- 238000003860 storage Methods 0.000 abstract description 13
- -1 emulsification aid Substances 0.000 abstract description 9
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 21
- 235000017550 sodium carbonate Nutrition 0.000 description 11
- 238000002955 isolation Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 3
- 238000005576 amination reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000012754 barrier agent Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 150000002513 isocyanates Chemical class 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229940024546 aluminum hydroxide gel Drugs 0.000 description 1
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an active rubber isolating agent and a preparation method thereof, and relates to the technical field of rubber additives. The active rubber isolating agent prepared by the invention comprises inorganic silicate, aluminum stearate, water-soluble high polymer material, surfactant, emulsifier, emulsification aid, vegetable oil, polyalcohol, sodium carbonate, deionized water and triphosgene; the inorganic silicate is amino nano porous ceramic; the water-soluble polymer material is amino-terminated hyperbranched polyamide; the surfactant is sodium oleate; the emulsifier is sodium dodecyl benzene sulfonate; the emulsifying aid is melamine; the vegetable oil is any one of peanut oil, castor oil and rapeseed oil; the polyalcohol is polyethylene glycol; the active rubber isolating agent prepared by the invention has strong high temperature resistance and storage stability.
Description
Technical Field
The invention relates to the technical field of rubber additives, in particular to an active rubber isolating agent and a preparation method thereof.
Background
In the production and processing process of rubber products, the rubber material is subjected to open mill or banburying and then laminated and placed. Because the film has high self-adhesion, and under the action of layer pressure, the film is easy to be adhered layer by layer, and the subsequent processing and use are seriously affected. Therefore, before rubber is carried and stacked for storage, polyethylene plastic films or a layer of release agent on the rubber sheets are used for realizing isolation, so that the rubber sheets are prevented from being adhered to each other. The physical properties of vulcanized rubber products are reduced due to the incorporation of polyethylene films, and rubber products such as tires, which have high performance requirements, must be removed but are difficult to remove. Therefore, the isolation method of the rubber sheet basically adopts spraying or coating of the isolating agent.
Isolation principle of rubber isolating agent: under the premise of not affecting the processability of rubber and the performance of products, the mechanical isolation effect of inorganic particles is utilized to prevent plasticating or mixing films from being mutually stuck; or liquid with large solubility parameter and rubber phase difference is adopted as a separating agent, and after the surface of the rubber sheet is coated, a thin separating layer is formed between the rubber sheets to block or slow down the mutual adhesion between the rubber sheets, thereby achieving the separating effect. Therefore, it is necessary to satisfy the following as a rubber film release agent: (1) The rubber is incompatible with rubber, and an isolation layer is formed on the surface of the rubber sheet safely and efficiently; (2) The negative effect on the processability of rubber sheets and the mechanical properties of products is small; (3) The process is convenient to operate, low in cost, harmless to human health, nontoxic, pollution-free to the environment and the like.
However, in the process of storing and using the rubber film release agent, the problems of poor storage stability, poor high temperature resistance and the like often occur, so that the rubber is adhered, and the invention solves the problem by preparing the active rubber release agent.
Disclosure of Invention
The invention aims to provide an active rubber isolating agent and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the active rubber isolating agent comprises, by weight, 3-15 parts of inorganic silicate, 30-38 parts of aluminum stearate, 2-4 parts of water-soluble polymer material, 1-5 parts of surfactant, 2-4 parts of emulsifier, 1-3 parts of emulsification aid, 2-4 parts of vegetable oil, 2-4 parts of polyol, 1-5 parts of sodium carbonate, 60-100 parts of deionized water and 1-3 parts of triphosgene.
Further, the inorganic silicate is an aminated nanoporous ceramic.
Further, the water-soluble polymer material is amino-terminated hyperbranched polyamide.
Further, the surfactant is sodium oleate.
Further, the emulsifier is sodium dodecyl benzene sulfonate; the emulsifying aid is melamine.
Further, the vegetable oil is any one of peanut oil, castor oil and rapeseed oil; the polyalcohol is polyethylene glycol.
Further, the preparation method of the active rubber release agent comprises the following preparation steps:
step 1): under the protection of nitrogen, 1 to 3 parts by weight of triphosgene, 2 to 4 parts by weight of water-soluble polymer material, 1 to 3 parts by weight of emulsification auxiliary agent, 3 to 15 parts by weight of inorganic silicate and 0.1 to 0.3 part by weight of triethylamine are put into a reaction kettle, stirred for 20 to 40 minutes at 120 to 140r/min, heated to 130 ℃, continuously stirred for 1 to 3 hours, then added with 0.04 to 0.06 part by weight of catalyst P838 and 2 to 4 parts by weight of polyol, and stirred for 3 to 5 hours at 40 to 60r/min to obtain a primary mixed material;
step 2): adding 30-38 parts by weight of aluminum stearate, 1-5 parts by weight of surfactant, 2-4 parts by weight of emulsifier, 2-4 parts by weight of vegetable oil and 60-100 parts by weight of deionized water into the primary mixed material obtained in the step 1) under the protection of nitrogen, stirring for 4 hours at the rotating speed of 55r/min, then adding 1-5 parts of sodium carbonate, heating to 35-60 ℃ and continuously stirring for 8 hours to obtain a middle mixed material;
step 3): naturally cooling for 24h to room temperature, and vacuum defoaming to obtain the active rubber release agent.
Further, the inorganic silicate in the step 1) is an aminated nano porous ceramic, and the preparation method of the aminated nano porous ceramic comprises the following steps: the nano porous ceramic with the grain diameter of 200nm and the porosity of 70 percent and concentrated sulfuric acid are mixed according to the mass ratio of 1: 50-1: 90, ultrasonic treatment for 20-40 min at 30kHz, adding concentrated nitric acid with the mass fraction of 68% and the mass fraction of 50-54 times of the nano porous ceramic, stirring for 9-11 min at 1200-1400 r/min, heating to 58-62 ℃, continuously stirring for 1.5-2.5 h, adding deionized water with the mass of 100 times of the nano porous ceramic for dilution, standing for 3.5-4.5 h, vacuum filtering, washing with deionized water until the pH value of the filtrate is 7, washing with absolute ethyl alcohol for 2-4 times, baking in a baking oven at 55-65 ℃ for 40-60 min, adding into diethyl ether with the mass of 20-40 times of the nano porous ceramic, ultrasonic treatment for 20-40 min at 30kHz, adding p-aminobenzoic acid with the mass of 0.8-1 time of the nano porous ceramic, dripping concentrated sulfuric acid with the mass of 0.6-0.8 times of the nano porous ceramic at 40-60 drops/min, heating to 60-80 ℃, continuously stirring for 1-3 h, filtering, washing with absolute ethyl alcohol and deionized water for 2-4 times, respectively, and baking in an baking oven at 55-65 ℃ for 40-60 min to obtain the nano porous ceramic.
Compared with the prior art, the invention has the following beneficial effects:
the active rubber isolating agent prepared by the invention comprises inorganic silicate, aluminum stearate, water-soluble high polymer material, surfactant, emulsifier, emulsification aid, vegetable oil, polyalcohol, sodium carbonate, deionized water and triphosgene; the inorganic silicate is amino nano porous ceramic; the water-soluble polymer material is amino-terminated hyperbranched polyamide; the surfactant is sodium oleate; the emulsifier is sodium dodecyl benzene sulfonate; the emulsifying aid is melamine; the vegetable oil is any one of peanut oil, castor oil and rapeseed oil; the polyalcohol is polyethylene glycol.
The triphosgene is heated and decomposed to form phosgene, part of the phosgene reacts with amino groups on the water-based high polymer material, inorganic silicate and an emulsifying aid to form isocyanate, the isocyanate reacts with polyol to form polyurethane, and the inorganic silicate is firmly fixed in the active rubber isolating agent, so that the inorganic silicate is prevented from settling, and the storage stability and the high temperature resistance of the active rubber isolating agent are further enhanced; and part of phosgene is hydrolyzed to form hydrogen chloride, the hydrogen chloride and aluminum stearate are adsorbed into pore channels of inorganic silicate to react to form aluminum chloride, and aluminum trichloride is hydrolyzed to form aluminum hydroxide gel under the action of sodium carbonate, so that the viscosity of the active rubber isolating agent is increased, and the storage stability of the active rubber isolating agent is further improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used to describe the method for testing each index of the active rubber release agent prepared in the following examples as follows:
high temperature resistance, storage stability: the film used for testing the barrier properties was a masticated natural film. Wherein, the plasticating process for plasticating the natural rubber sheet is that the standard rubber No. 5 is thinned and passed for 12 times under the roll spacing of 0.5 mm; discharging the plasticated rubber in a tablet press, cutting the plasticated rubber into 50mm multiplied by 100mm films with the thickness of 3-5 mm, dip-coating the active rubber isolating agent, air-drying, laminating the two by two, clamping the two, uniformly applying 5Kg pressure between iron plates with the thickness of 80 multiplied by 120 multiplied by 10mm, and standing for 24 hours and 144 hours at the temperature of 25 ℃; and standing at 60 ℃ for 24 hours, and respectively performing film peeling test detection.
Example 1
The preparation method of the active rubber release agent is characterized by comprising the following preparation steps:
step 1): the nano porous ceramic with the grain diameter of 200nm and the porosity of 70 percent and concentrated sulfuric acid are mixed according to the mass ratio of 1:50, mixing, performing ultrasonic treatment at 30kHz for 20min, then adding concentrated nitric acid with the mass fraction of 68% and 50 times of the mass of the nano porous ceramic, stirring for 9min at 120r/min, heating to 58 ℃, continuously stirring for 1.5h, adding deionized water with the mass of 100 times of the nano porous ceramic for dilution, standing for 3.5h, performing vacuum suction filtration, washing with the deionized water until the pH value of the filtrate is 7, then washing with absolute ethyl alcohol for 2 times, placing into a 55 ℃ oven for baking for 40min, then adding into diethyl ether with the mass of 20 times of the nano porous ceramic, performing ultrasonic treatment at 30kHz for 20min, adding concentrated sulfuric acid with the mass of 0.6 times of the nano porous ceramic into the nano porous ceramic, heating to 60 ℃, continuously stirring for 1h, filtering, washing with absolute ethyl alcohol and deionized water for 2 times, and placing into a 55 ℃ oven for baking for 40min, thus obtaining the aminated nano porous ceramic;
step 2): under the protection of nitrogen, 1 part by weight of triphosgene, 2 parts by weight of water-soluble polymer material amino-terminated hyperbranched polyamide, 1 part by weight of emulsification auxiliary agent melamine, 3 parts of inorganic silicate amination nano porous ceramic and 0.1 part by weight of triethylamine are put into a reaction kettle, stirred for 20min at 120r/min, heated to 130 ℃, continuously stirred for 1h, then added with 0.04 part by weight of catalyst P838 and 2 parts by weight of polyol polyethylene glycol, and stirred for 3h at 40r/min to obtain a primary mixed material;
step 3): adding 30 parts by weight of aluminum stearate, 1 part by weight of surfactant sodium oleate, 2 parts by weight of sodium dodecyl benzene sulfonate, 2 parts by weight of vegetable oil peanut oil and 6 parts of deionized water into the primary mixed material obtained in the step 1) under the protection of nitrogen, stirring for 4 hours at the rotating speed of 55r/min, then adding 1 part of sodium carbonate, heating to 35 ℃ and continuously stirring for 8 hours to prepare a middle mixed material;
step 4): naturally cooling for 24h to room temperature, and vacuum defoaming to obtain the active rubber release agent.
The preparation method of the active rubber release agent is characterized by comprising the following preparation steps:
step 1): the nano porous ceramic with the grain diameter of 200nm and the porosity of 70 percent and concentrated sulfuric acid are mixed according to the mass ratio of 1:70, mixing, performing ultrasonic treatment at 30kHz for 30min, then adding concentrated nitric acid with the mass fraction of 68% and the mass fraction of the nano porous ceramic, stirring for 10min at 1300r/min, heating to 60 ℃, continuing stirring for 2h, adding deionized water with the mass of 100 times of the nano porous ceramic, diluting, standing for 4h, performing vacuum filtration, washing with deionized water until the pH value of filtrate is 7, then washing with absolute ethyl alcohol for 3 times, placing into a 60 ℃ oven for baking for 50min, then adding into diethyl ether with the mass of 30 times of the nano porous ceramic, performing ultrasonic treatment at 30kHz for 30min, adding p-aminobenzoic acid with the mass of 0.9 times of the nano porous ceramic, dropwise adding concentrated sulfuric acid with the mass of 0.7 times of the nano porous ceramic at 50 drops/min, heating to 70 ℃, continuing stirring for 2h, filtering, washing with absolute ethyl alcohol and deionized water for 3 times, and placing into a 60 ℃ oven for baking for 50min, thus obtaining the amino nano porous ceramic;
step 2): under the protection of nitrogen, 2 parts by weight of triphosgene, 3 parts by weight of water-soluble polymer material polyamide, 2 parts by weight of emulsification auxiliary agent melamine, 9-part inorganic silicate amination nano porous ceramic and 0.2 part by weight of triethylamine are put into a reaction kettle, stirred for 30min at 130r/min, heated to 130 ℃, continuously stirred for 2h, then added with 0.05 part by weight of catalyst P838 and 3 parts by weight of polyol polyethylene glycol, and stirred for 4h at 50r/min to obtain a primary mixed material;
step 3): under the protection of nitrogen, 34 parts by weight of aluminum stearate, 3 parts by weight of surfactant sodium oleate, 3 parts by weight of sodium dodecyl benzene sulfonate, 3 parts by weight of vegetable oil and 80 parts of deionized water are added into the primary mixed material obtained in the step 1), stirring is carried out for 4 hours under the condition of the rotating speed of 55r/min, then 3 parts of calcined soda is added, and the temperature is raised to 45 ℃ and stirring is continued for 8 hours, so that a middle mixed material is obtained;
step 4): naturally cooling for 24h to room temperature, and vacuum defoaming to obtain the active rubber release agent.
Example 3
The preparation method of the active rubber release agent is characterized by comprising the following preparation steps:
step 1): the nano porous ceramic with the grain diameter of 200nm and the porosity of 70 percent and concentrated sulfuric acid are mixed according to the mass ratio of 1:90, mixing, performing ultrasonic treatment at 30kHz for 40min, then adding concentrated nitric acid with the mass fraction of 68% and 54 times of the mass of the nano porous ceramic, stirring for 11min at 1400r/min, heating to 62 ℃, continuously stirring for 2.5h, adding deionized water with the mass of 100 times of the nano porous ceramic for dilution, standing for 4.5h, performing vacuum suction filtration, washing with the deionized water until the pH value of the filtrate is 7, then washing with absolute ethyl alcohol for 4 times, placing into a 65 ℃ oven for baking for 60min, then adding into diethyl ether with the mass of 40 times of the nano porous ceramic, performing ultrasonic treatment at 30kHz for 40min, adding p-aminobenzoic acid with the mass of 1 time of the nano porous ceramic, dropwise adding concentrated sulfuric acid with the mass of 0.8 times of the nano porous ceramic at 60 drops/min, heating to 80 ℃, continuously stirring for 3h, filtering, washing with absolute ethyl alcohol and deionized water for 4 times, and placing into a 65 ℃ oven for baking for 60min, so as to obtain amino nano porous ceramic;
step 2): under the protection of nitrogen, 3 parts by weight of triphosgene, 4 parts by weight of water-soluble polymer material polyamide, 3 parts by weight of emulsification auxiliary agent melamine, 15 parts of inorganic silicate amination nano porous ceramic and 0.3 part by weight of triethylamine are put into a reaction kettle, stirred for 40min at 140r/min, heated to 130 ℃, continuously stirred for 3h, then added with 0.06 parts by weight of catalyst P838 and 4 parts by weight of polyol polyethylene glycol, and stirred for 5h at 60r/min to obtain a primary mixed material;
step 3): under the protection of nitrogen, adding 38 parts by weight of aluminum stearate, 5 parts by weight of surfactant sodium oleate, 4 parts by weight of sodium dodecyl benzene sulfonate, 4 parts by weight of vegetable oil and 100 parts of deionized water into the primary mixed material obtained in the step 1), stirring for 4 hours at the rotating speed of 55r/min, then adding 5 parts of sodium carbonate, heating to 60 ℃ and continuously stirring for 8 hours to obtain a middle mixed material;
step 4): naturally cooling for 24h to room temperature, and vacuum defoaming to obtain the active rubber release agent.
Comparative example 1
Comparative example 1 differs from example 2 in that only inorganic silicate nanoceramics, aluminum stearate, water-soluble high molecular materials, surfactants, emulsifiers, emulsification aids, vegetable oils, polyols, soda ash, deionized water, triphosgene were used to prepare the active rubber release agent. The remaining preparation steps were the same as in example 2.
Comparative example 2
Comparative example 2 differs from example 2 in that only the inorganic silicate aminated nanoporous ceramic, sodium stearate water-soluble polymer material, surfactant, emulsifier, emulsification aid, vegetable oil, polyol, soda ash, deionized water, triphosgene were used to prepare the active rubber release agent. The remaining preparation steps were the same as in example 2.
Comparative example 3
Comparative example 3 differs from example 2 in that only the inorganic silicate-aminated nanoporous ceramic, aluminum stearate, surfactant, emulsifier, emulsification aid, vegetable oil, polyol, soda ash, deionized water, triphosgene were used to prepare the active rubber release agent. The remaining preparation steps were the same as in example 2.
Comparative example 4
Comparative example 4 differs from example 2 in that only the inorganic silicate-aminated nanoporous ceramic, aluminum stearate, water-soluble high molecular material, surfactant, emulsifier, emulsification aid, vegetable oil, polyol, soda ash, deionized water were used to prepare the active rubber release agent. The remaining preparation steps were the same as in example 2.
Comparative example 5
Comparative example 5 differs from example 2 in that only the inorganic silicate-aminated nanoporous ceramic, aluminum stearate, water-soluble polymer material, surfactant, emulsifier, emulsification aid, vegetable oil, polyol, soda ash, deionized water, and triphosgene were used to prepare the active rubber release agent. The remaining preparation steps were the same as in example 2.
Effect example
The following table 1 shows the results of analysis of the high temperature resistance and storage stability of the active rubber separators prepared in examples 1 to 3 and comparative examples 1 to 4 according to the present invention.
TABLE 1
| 60℃24h | 25℃24h | 25℃144h | |
| Example 1 | Non-adhesion | Non-adhesion | Non-adhesion |
| Example 2 | Non-adhesion | Non-adhesion | Non-adhesion |
| Example 3 | Non-adhesion | Non-adhesion | Non-adhesion |
| Comparative example 1 | Non-adhesion | Non-adhesion | Edge part adhesion |
| Comparative example 2 | Non-adhesion | Non-adhesion | Edge part adhesion |
| Comparative example 3 | Non-adhesion | Non-adhesion | Edge part adhesion |
| Comparative example 4 | Non-adhesion | Non-adhesion | Edge part adhesion |
| Comparative example 5 | Edge part adhesion | Non-adhesion | Edge part adhesion |
From Table 1, it can be found that the active rubber separators prepared in examples 1, 2 and 3 are strong in high temperature resistance and storage stability; from comparison of experimental data of examples 1, 2, 3 and comparative example 1, it was found that the active rubber release agent prepared by using the inorganic silicate aminated nanoporous ceramic was strong in storage stability; from the experimental data of examples 1, 2, 3 and comparative example 2, it was found that the use of aluminum stearate as an active rubber release agent produced with a high storage stability; from the experimental data of examples 1, 2, 3 and comparative example 3, it can be found that the active rubber isolating agent prepared by using the amino-terminated hyperbranched polyamide of the water-soluble high polymer material has stronger storage stability; from the experimental data of examples 1, 2, 3 and comparative example 4, it was found that the use of triphosgene to prepare the active rubber barrier agent resulted in the active rubber barrier agent having a higher storage stability; from the experimental data of examples 1, 2, 3 and comparative example 5, it can be found that the active rubber release agent is prepared by using the emulsification aid melamine, and the prepared active rubber release agent has strong high temperature resistance and storage stability.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. The active rubber isolating agent is characterized by comprising, by weight, 3-15 parts of inorganic silicate, 30-38 parts of aluminum stearate, 2-4 parts of water-soluble polymer material, 1-5 parts of surfactant, 2-4 parts of emulsifier, 1-3 parts of emulsification aid, 2-4 parts of vegetable oil, 2-4 parts of polyol, 1-5 parts of sodium carbonate, 60-100 parts of deionized water and 1-3 parts of triphosgene.
2. An active rubber spacer according to claim 1, wherein the inorganic silicate is an aminated nanoporous ceramic.
3. An active rubber spacer according to claim 1, wherein the water-soluble polymeric material is an amino-terminated hyperbranched polyamide.
4. An active rubber spacer according to claim 1, wherein the surfactant is sodium oleate.
5. An active rubber release agent according to claim 1, wherein the emulsifier is sodium dodecylbenzenesulfonate; the emulsifying aid is melamine.
6. The active rubber spacer of claim 1, wherein the vegetable oil is any one of peanut oil, castor oil and rapeseed oil; the polyalcohol is polyethylene glycol.
7. The preparation method of the active rubber release agent is characterized by comprising the following preparation steps:
step 1): under the protection of nitrogen, 1 to 3 parts by weight of triphosgene, 2 to 4 parts by weight of water-soluble polymer material, 1 to 3 parts by weight of emulsification auxiliary agent, 3 to 15 parts by weight of inorganic silicate and 0.1 to 0.3 part by weight of triethylamine are put into a reaction kettle, stirred for 20 to 40 minutes at 120 to 140r/min, heated to 130 ℃, continuously stirred for 1 to 3 hours, then added with 0.04 to 0.06 part by weight of catalyst P838 and 2 to 4 parts by weight of polyol, and stirred for 3 to 5 hours at 40 to 60r/min to obtain a primary mixed material;
step 2): adding 30-38 parts by weight of aluminum stearate, 1-5 parts by weight of surfactant, 2-4 parts by weight of emulsifier, 2-4 parts by weight of vegetable oil and 60-100 parts by weight of deionized water into the primary mixed material obtained in the step 1) under the protection of nitrogen, stirring for 4 hours at the rotating speed of 55r/min, then adding 1-5 parts of sodium carbonate, heating to 35-60 ℃ and continuously stirring for 8 hours to obtain a middle mixed material;
step 3): naturally cooling for 24h to room temperature, and vacuum defoaming to obtain the active rubber release agent.
8. The method for preparing an active rubber isolating agent according to claim 7, wherein the inorganic silicate in step 1) is an aminated nano porous ceramic, and the method for preparing the aminated nano porous ceramic comprises the following steps: the nano porous ceramic with the grain diameter of 200nm and the porosity of 70 percent and concentrated sulfuric acid are mixed according to the mass ratio of 1: 50-1: 90, ultrasonic treatment for 20-40 min at 30kHz, adding concentrated nitric acid with the mass fraction of 68% and the mass fraction of 50-54 times of the nano porous ceramic, stirring for 9-11 min at 1200-1400 r/min, heating to 58-62 ℃, continuously stirring for 1.5-2.5 h, adding deionized water with the mass of 100 times of the nano porous ceramic for dilution, standing for 3.5-4.5 h, vacuum filtering, washing with deionized water until the pH value of the filtrate is 7, washing with absolute ethyl alcohol for 2-4 times, baking in a baking oven at 55-65 ℃ for 40-60 min, adding into diethyl ether with the mass of 20-40 times of the nano porous ceramic, ultrasonic treatment for 20-40 min at 30kHz, adding p-aminobenzoic acid with the mass of 0.8-1 time of the nano porous ceramic, dripping concentrated sulfuric acid with the mass of 0.6-0.8 times of the nano porous ceramic at 40-60 drops/min, heating to 60-80 ℃, continuously stirring for 1-3 h, filtering, washing with absolute ethyl alcohol and deionized water for 2-4 times, respectively, and baking in an baking oven at 55-65 ℃ for 40-60 min to obtain the nano porous ceramic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310231066.0A CN116082872A (en) | 2023-03-13 | 2023-03-13 | Active rubber isolating agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310231066.0A CN116082872A (en) | 2023-03-13 | 2023-03-13 | Active rubber isolating agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116082872A true CN116082872A (en) | 2023-05-09 |
Family
ID=86202742
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310231066.0A Pending CN116082872A (en) | 2023-03-13 | 2023-03-13 | Active rubber isolating agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116082872A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116891714A (en) * | 2023-07-13 | 2023-10-17 | 韦尔通科技股份有限公司 | Heat conduction underfill adhesive and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709428A (en) * | 2013-11-29 | 2014-04-09 | 山东永泰化工有限公司 | Water soluble rubber separant |
| CN114621482A (en) * | 2022-03-07 | 2022-06-14 | 江苏源通新材料有限公司 | Dust-free paste film separant |
-
2023
- 2023-03-13 CN CN202310231066.0A patent/CN116082872A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709428A (en) * | 2013-11-29 | 2014-04-09 | 山东永泰化工有限公司 | Water soluble rubber separant |
| CN114621482A (en) * | 2022-03-07 | 2022-06-14 | 江苏源通新材料有限公司 | Dust-free paste film separant |
Non-Patent Citations (1)
| Title |
|---|
| 陈兆麟: "光气安全评价管理", 华东理工大学出版社, pages: 6 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116891714A (en) * | 2023-07-13 | 2023-10-17 | 韦尔通科技股份有限公司 | Heat conduction underfill adhesive and preparation method thereof |
| CN116891714B (en) * | 2023-07-13 | 2024-02-02 | 韦尔通科技股份有限公司 | Heat conduction underfill adhesive and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN116082872A (en) | Active rubber isolating agent and preparation method thereof | |
| US4076656A (en) | Method of producing porous plastic materials | |
| JP6680206B2 (en) | Polyolefin microporous membrane, battery separator and battery | |
| EP2723479B1 (en) | Process for manufacturing porous membranes | |
| TWI621680B (en) | Dual-coating, fast curing and solvent-free polyurethane adhesive with wide substrate adaptability, composite film material and manufacturing method thereof | |
| CN111231455A (en) | Solvent-resistant inert resin coated fluororubber sealing rubber plug and manufacturing method thereof | |
| CN111331932B (en) | High-strength composite corrugated board and production process thereof | |
| CN115819912B (en) | Breathable polytetrafluoroethylene stretched film and preparation method thereof | |
| CN115584012A (en) | Polyurethane composite material for foaming sealing rubber strip and preparation method thereof | |
| CN110437686B (en) | Electrolyte-resistant BOPA film and preparation method thereof | |
| CN114181481A (en) | Screening method and application for preparing multilayer PTFE composite expanded sheet material, expanded sheet and preparation method thereof | |
| CN108394139A (en) | A kind of lithium battery flexible packaging composite membrane, preparation method, lithium battery pack pack, lithium battery and its application of the composite membrane | |
| CN112937006A (en) | Multilayer composite impact-resistant plate based on high-strength polyethylene microporous membrane and preparation method thereof | |
| CN111082061A (en) | Preparation method of adhesive for lithium battery | |
| JPH11106532A (en) | Porous polyethylene resin film and its production | |
| CN113150583B (en) | Water-based graphite film isolating agent and preparation method thereof | |
| CN214522534U (en) | Transparent high-barrier composite packaging film | |
| CN111703162B (en) | Scratch-resistant high-barrier primer-free multilayer co-extrusion BOPP pre-coated base film and preparation method thereof | |
| CN115651369A (en) | Novel polyester film, preparation method thereof and high-resistance Gao Chong deep aluminum-plastic composite film | |
| CN116422064A (en) | Polymer filter plate and manufacturing method thereof | |
| CN113415007A (en) | Processing method of environment-friendly noise-reduction type car door waterproof film | |
| CN115172986A (en) | Multilayer composite lithium ion battery diaphragm and preparation method thereof | |
| CN116396546A (en) | High-elasticity foam material and manufacturing process thereof | |
| CN1142207C (en) | Irradiation crosslinking technological process of preparing linear low-density foamed polyethylene plastics | |
| JP2000178044A (en) | Intermediate film for laminated glass and laminated glass |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |