CN105385401B - A kind of organic silicon modified polyurethane rubber polymer and preparation method thereof - Google Patents

A kind of organic silicon modified polyurethane rubber polymer and preparation method thereof Download PDF

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CN105385401B
CN105385401B CN201510986816.0A CN201510986816A CN105385401B CN 105385401 B CN105385401 B CN 105385401B CN 201510986816 A CN201510986816 A CN 201510986816A CN 105385401 B CN105385401 B CN 105385401B
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CN105385401A (en
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丁达亚
陆平
王友余
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Jiangsu West Ole Medical Technology Co Ltd
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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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/61—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
    • C08G18/78—Nitrogen
    • C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
    • C08G18/797—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing carbodiimide and/or uretone-imine groups
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
    • 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
    • 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
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2265—Oxides; Hydroxides of metals of iron
    • C08K2003/2272—Ferric oxide (Fe2O3)

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to a kind of organic silicon modified polyurethane rubber polymers and preparation method thereof.Conventional bandages wrapping be easy to cause fracture site displacement, aggravates the pain of patient.The present invention is based on mass percentage, including following components：35%~37% Carbodiimide-Modified MDI, 17%~19% polyether polyol GE 210,2%~4% polyether polyol GE 303,26%~28% hydroxyl-terminated injecting two methyl siloxane, 1%~2% methyl tributanoximo silane, 0.2%~0.4% lauryl sodium sulfate, 0.1%~0.2% organo-tin compound, 1%~3% triethyl phosphate, 7%~9% aluminium hydroxide and 2%~4% di-iron trioxide.The present invention also provides the preparation methods of organic silicon modified polyurethane rubber polymer.Binder of the present invention as consolidation band, and it is in non-condensable state that finished product consolidation band, which is encapsulated in aluminium plastic bag, meets air consolidation band and is hardened, the Postural immobilization that can be used for after people's bone folding.

Description

A kind of organic silicon modified polyurethane rubber polymer and preparation method thereof
Technical field
The present invention relates to a kind of organic silicon modified polyurethane rubber polymers and preparation method thereof, further relate to the rubber polymer as fast The winding that speed repairs damaged object consolidates the application with bonding agent, belongs to technical field of polymer materials.
Background technology
Known field of medicaments often utilizes reaction kettle to synthesize target product.Reaction kettle interlayer can lead to different Cooling and Heat Sources（It is cold Freeze liquid, hot water or deep fat）Do circulating-heating or cooling reaction.Its operation principle is：By reaction kettle interlayer, a constant temperature is injected The thermosol media of degree or cooling media, are heated or are freezed to the material in reaction kettle.
Usually in terms of medical device, people carry out Postural immobilization using the methods of bandaging to fracture site, avoid Damaged part shifts and aggravates fracture and injury.Preferable fixed or hemostasis is just can ensure that since bandaging will reach certain thickness Effect, otherwise fracture site once displacement, can aggravate the pain of patient, serious to even result in patient's Massive Bleeding and generate not Gram phenomenon.In today that per capita health care is becoming tight resource day, realize that the fixed patient's fracture site of quickly wrapping is particularly important. In addition, in terms of household items, such as chair leg, fishing rod, metal tube, plastic tube fracture or crack, because lacking professional tool, often It can not fix or repair within a short period of time, the common processing mode of people is to give it up, therefore cause huge waste. In terms of engineering construction, such as steam line break gently then influences the production and living of people, serious also to cause accident.These are all Winding to quickly repairing damaged object consolidates the research and development with bonding agent and industrialization proposes requirement.Quickly repair damaged object Not only it can also extend object service life with accident prevention risk, it is cost-effective.
Invention content
The purpose of the present invention is to provide a kind of organic silicon modified polyurethane rubber polymers.The rubber polymer takes for consolidating Bonding agent.
Another object of the present invention provides a kind of preparation method of organic silicon modified polyurethane rubber polymer.
The purpose of the present invention is achieved through the following technical solutions：
A kind of organic silicon modified polyurethane rubber polymer, based on mass percentage, including following components：35%~37% carbon Change diimine and is modified MDI, 17%~19% polyether polyol GE-210,2%~4% polyether polyol GE-303,26%~28% end hydroxyl Base dimethyl silicone polymer, 0.1%~0.2% dibutyl hydroxy toluene, 1%~2% methyl tributanoximo silane, 0.2%~0.5% It is aerosil A380,0.2%~0.4% lauryl sodium sulfate, 0.05%~0.07% pyrovinic acid, 0.1%~0.2% organic Tin compound, 1%~3% triethyl phosphate, 7%~9% aluminium hydroxide and 2%~4% di-iron trioxide.The sum of each component content is 100%。
The preparation method of above-mentioned organic silicon modified polyurethane rubber polymer, includes the following steps according to sequencing：
（1）Reaction kettle is opened, 72~74 DEG C of setting interlayer hot oil temperature, reaction kettle is heated to 72~74 DEG C；
（2）35~37 parts by weight Carbodiimide-Modified MDI, reaction kettle rotating speed 60r/min, 14~16min of time are added, Heating temperature is to 67~69 DEG C；
（3）Be added 17~19 parts by weight polyether polyol GE-210,120 r/min of reaction kettle rotating speed, the time 19~ 21min, 67~69 DEG C of temperature；
（4）0.2~0.5 parts by weight aerosil of addition, reaction kettle rotating speed 180 r/min, 29~31min of time, 67~69 DEG C of temperature；
（5）0.2~0.4 parts by weight lauryl sodium sulfate, 0.1~0.2 parts by weight dibutyl hydroxy toluene, reaction is added Kettle rotating speed 180 r/min, 14~16min of time, 67~69 DEG C of temperature；
（6）It is added 2~4 parts by weight polyether polyol GE-303,120 r/min of reaction kettle rotating speed, temperature is heated to 81~ 83 DEG C, 29~31min of time；
（7）0.05~0.07 parts by weight pyrovinic acid, 120 r/min of reaction kettle rotating speed is added, temperature is down to 67~69 DEG C, 9~11min of time；
（8）26~28 parts by weight hydroxyl-terminated injecting two methyl siloxanes of addition, 1~2 parts by weight methyl tributanoximo silane, 120 r/min of reaction kettle rotating speed, temperature are down to 64~66 DEG C, 29~31min of time；
（9）0.1~0.2 parts by weight organo-tin compound, 60 r/min of reaction kettle rotating speed is added, temperature is down to 59~61 DEG C, 9~11min of time；
（10）1~3 parts by weight of phosphoric acid triethyl of addition, 60 r/min of reaction kettle rotating speed, 59~61 DEG C of temperature, the time 9~ 11min；
（11）7~9 parts by weight aluminium hydroxides, 2~4 parts by weight di-iron trioxides, 60 r/min of reaction kettle rotating speed, temperature is added 59~61 DEG C of degree, 14~16min of time is to get the organic silicon modified polyurethane rubber polymer.
The present invention chooses polyether polyol and increases fluid viscosity in reaction kettle.Utilize the water-wet side of lauryl sodium sulfate And hydrophobic side, increase surface-active.Organo-tin compound is added as catalyst, carries out catalysis reaction.In preparation process, according to Secondary selection hydroxyl-terminated injecting two methyl siloxane, triethyl phosphate, aluminium hydroxide increase heat-resisting quantity and the resistance of polyurethane rubber polymer Combustion property.
Raw material according to the present invention can be bought by market and be obtained.
Beneficial effects of the present invention：
Binder of the present invention as consolidation band, and it is in non-condensable state that finished product consolidation band, which is encapsulated in aluminium plastic bag,.It uses When, it cuts off aluminium plastic bag and takes out use, after a period of time, meet air consolidation band and be hardened.The Postural immobilization that can be used for after people's bone folding, It can be used for fixation or repairing after chair leg, fishing rod, metal tube, plastic tube etc. fracture or crack, can also be used to repairing and steam Feed channel.The present invention has the advantages that tensile strength is high, condensation is firm, anti-aging, also has heat safe characteristic.
Specific implementation mode
In terms of below by the sum of each component content for 100kg, the specific implementation mode of the present invention is described in detail.
Table 1 prepares the first, second, and third embodiment raw material composition of organic silicon modified polyurethane rubber polymer
Embodiment 4
The preparation method of organic silicon modified polyurethane rubber polymer, includes the following steps according to sequencing：
（1）Reaction kettle is opened, 73 DEG C of setting interlayer hot oil temperature, reaction kettle is heated to 73 DEG C；
（2）36.5kg Carbodiimide-Modified MDI are added, reaction kettle rotating speed 60r/min, time 15min, heating temperature is extremely 68℃；
（3）18.2kg polyether polyol GE-210, reaction kettle rotating speed 120 r/min, time 20min, 68 DEG C of temperature is added；
（4）0.36kg aerosils, reaction kettle rotating speed 180 r/min, time 30min, 68 DEG C of temperature is added；
（5）Addition 0.29kg lauryl sodium sulfate, 0.15kg dibutyl hydroxy toluenes, 180 r/min of reaction kettle rotating speed, Time 15min, 68 DEG C of temperature；
（6）2.6kg polyether polyol GE-303,120 r/min of reaction kettle rotating speed is added, temperature is heated to 82 DEG C, the time 30min；
（7）0.06kg pyrovinic acids, 120 r/min of reaction kettle rotating speed is added, temperature is down to 68 DEG C, time 10min；
（8）27.2kg hydroxyl-terminated injecting two methyl siloxanes, 1.5kg methyl tributanoximo silanes, reaction kettle rotating speed is added 120 r/min, temperature are down to 65 DEG C, time 30min；
（9）0.14kg organo-tin compounds, 60 r/min of reaction kettle rotating speed is added, temperature is down to 60 DEG C, time 10min；
（10）2kg triethyl phosphates, 60 r/min of reaction kettle rotating speed, temperature 60 C, time 10min is added；
（11）8kg aluminium hydroxides, 3kg di-iron trioxides, 60 r/min of reaction kettle rotating speed, temperature 60 C, time is added 15min is to get the organic silicon modified polyurethane rubber polymer.
Beneficial effects of the present invention：
Binder of the present invention as consolidation band, and it is in non-condensable state that finished product consolidation band, which is encapsulated in aluminium plastic bag,.It uses When, it cuts off aluminium plastic bag and takes out use, after a period of time, meet air consolidation band and be hardened.The Postural immobilization that can be used for after people's bone folding, It can be used for fixation or repairing after chair leg, fishing rod, metal tube, plastic tube etc. fracture or crack.The present invention has tension The advantage that intensity is high, condensation is firm, anti-aging.In addition, invention can be with resistance to 350 DEG C or so of high temperature, therefore can be used to repair Steam pipeline.

Claims (2)

1. a kind of organic silicon modified polyurethane rubber polymer, it is characterised in that：Based on mass percentage, including following components：35% ~37% Carbodiimide-Modified MDI, 17%~19% polyether polyol GE-210,2%~4% polyether polyol GE-303,26%~ 28% hydroxyl-terminated injecting two methyl siloxane, 0.1%~0.2% dibutyl hydroxy toluene, 1%~2% methyl tributanoximo silane, 0.2%~0.5% aerosil A380,0.2%~0.4% lauryl sodium sulfate, 0.05%~0.07% pyrovinic acid, 0.1% ~0.2% organo-tin compound, 1%~3% triethyl phosphate, 7%~9% aluminium hydroxide and 2%~4% di-iron trioxide.
2. the preparation method of the organic silicon modified polyurethane rubber polymer described in claim 1, it is characterised in that according to sequencing Include the following steps：
（1）Reaction kettle is opened, 72~74 DEG C of setting interlayer hot oil temperature, reaction kettle is heated to 72~74 DEG C；
（2）35~37 parts by weight Carbodiimide-Modified MDI, reaction kettle rotating speed 60r/min, 14~16min of time, heating is added Temperature is to 67~69 DEG C；
（3）17~19 parts by weight polyether polyol GE-210, reaction kettle rotating speed 120 r/min, 19~21min of time, temperature is added 67~69 DEG C of degree；
（4）0.2~0.5 parts by weight aerosil, reaction kettle rotating speed 180 r/min, 29~31min of time, temperature is added 67~69 DEG C；
（5）0.2~0.4 parts by weight lauryl sodium sulfate, 0.1~0.2 parts by weight dibutyl hydroxy toluene is added, reaction kettle turns Speed 180 r/min, 14~16min of time, 67~69 DEG C of temperature；
（6）2~4 parts by weight polyether polyol GE-303,120 r/min of reaction kettle rotating speed are added, temperature is heated to 81~83 DEG C, 29~31min of time；
（7）0.05~0.07 parts by weight pyrovinic acid, 120 r/min of reaction kettle rotating speed is added, temperature is down to 67~69 DEG C, the time 9~11min；
（8）26~28 parts by weight hydroxyl-terminated injecting two methyl siloxanes, 1~2 parts by weight methyl tributanoximo silane, reaction is added 120 r/min of kettle rotating speed, temperature are down to 64~66 DEG C, 29~31min of time；
（9）0.1~0.2 parts by weight organo-tin compound, 60 r/min of reaction kettle rotating speed is added, temperature is down to 59~61 DEG C, when Between 9~11min；
（10）1~3 parts by weight of phosphoric acid triethyl of addition, 60 r/min of reaction kettle rotating speed, 59~61 DEG C of temperature, the time 9~ 11min；
（11）7~9 parts by weight aluminium hydroxides, 2~4 parts by weight di-iron trioxides, 60 r/min of reaction kettle rotating speed, temperature 59 is added ~61 DEG C, 14~16min of time is to get the organic silicon modified polyurethane rubber polymer.
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CN107082862A (en) * 2017-05-18 2017-08-22 中国科学院深圳先进技术研究院 Selfreparing organic silicon modified polyurethane elastomer and preparation method thereof
DE102018114549A1 (en) 2018-06-18 2019-12-19 CHT Germany GmbH Polyurethane organopolysiloxanes with carbodiimide groups
CN112646118A (en) * 2020-12-24 2021-04-13 江苏东邦科技有限公司 Preparation method of fluorine-free water splashing agent for polyurethane

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