CN103992653B - Take ester type waxes as the preparation method of the extrusion type flame-proof silicon rubber of releasing agent - Google Patents
Take ester type waxes as the preparation method of the extrusion type flame-proof silicon rubber of releasing agent Download PDFInfo
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Abstract
Take ester type waxes as the preparation method of the extrusion type flame-proof silicon rubber of releasing agent, relate to the preparing technical field of extrusion type flame-proof silicon rubber.Methyl vinyl silicone rubber 100 parts, gas-phase silica 50 parts, 40 parts, aluminium hydroxide, magnesium hydroxide 50 parts, zinc borate 10 parts, ester type waxes 2 ~ 4 parts, antistructurizing agent 15 parts and silane coupling agent 2 ~ 4 parts are refined through banburying and opening.Extrusion type flame-proof silicon rubber of the present invention adopts ester type waxes to be releasing agent, can the stripping of reinforced insulation layer and conductor, improve the processing characteristics of finished product cable, effectively improve traditional flame-proof silicon rubber stearic acid or silicone oil is releasing agent, easily make silicone rubber products tell white, to tell oil, demolding performace difference shortcoming.
Description
Technical field
The present invention relates to the preparing technical field of extrusion type flame-proof silicon rubber.
Background technology
Ester type waxes is by containing the ester formed with the higher fatty acid of even-numbered carbon atom and high fatty alcohol, is spermaceti main body of oil, is widely used in the industry such as chemical industry, weaving, medicine, daily use chemicals and food.Wherein, liquid unsaturated ester type waxes is biodegradable, good at high temperature, high pressure and high-speed lubrication, can as the base-material of quality lubricant and advanced skin cream.In most of object, wax ester content is few, is difficult to collect, and usually needs to carry out under high temperature, high pressure and strong acid condition with the wax ester of chemical method synthesis, low conversion rate, by product is many, and production cost is high, and along with the lengthening of lipid acid and fatty alcohol carbochain, reaction difficulty strengthens.
Silicon rubber refers to the class elastomerics that molecular backbone chain contains Si-O structure, side chain contains organic group.Silicon rubber has the performances such as excellent thermotolerance, winter hardiness, dielectricity, resistance to ozone and resistance to atmospheric aging, and the outstanding performance of silicon rubber is that use temperature is broad, can life-time service at low or elevated temperatures.Flame-proof silicon rubber adds fire retardant in silicon rubber, produces the product with flame retardancy and self-extinguishing.In prior art, flame-proof silicon rubber makes the amount of being fuming large at material combustion, and gas of its release is poisonous and be corrosive, not environmentally.
Publication number is: CN1364755A application discloses that a kind of ester type waxes preparation method: the straight chain saturated mono carboxylic acid of carbonatoms in 14 ~ 30 scopes and carbonatoms in 14 ~ 30 scopes straight_chain single fatty alcohols or carbonatoms obtained under varsol or alcoholic solvent exist at 2 ~ 6 yuan of multi-alcohols of 2 ~ 30.This ester type waxes is mainly used in the imaging of duplicating machine, laser printer, and this preparation method is owing to using hydro carbons or alcoholic solvent, can produce pollution, and the rate of recovery is lower when removing.
Publication number is: the preparation method that application discloses that a kind of flame-proof silicon rubber of CN102532913A: adopt primer and masterbatch through banburying, open refining, secondary banburying, secondary open refining, the operation of sulfuration is obtained, wherein primer comprises methyl vinyl silicone rubber 175 parts, white carbon black 100 parts, hydroxy silicon oil 7.8 parts, containing hydrogen silicone oil 0.6 part, releasing agent 0.6 part, and masterbatch comprises methyl vinyl silicone rubber 75 parts, 160 parts, aluminium hydroxide, containing hydrogen silicone oil 2 parts, methyl-silicone oil 5 parts, halogen-free flame retardants 20 parts.The releasing agent of such traditional extrusion type flame-proof silicon rubber is generally stearic acid or silicone oil, easily make silicone rubber products tell white, tell wet goods, and demolding performace is poor.
Summary of the invention
The object of the invention is for the original releasing agent of silicon rubber easily make silicone rubber products tell white, tell wet goods, and the deficiencies in the prior art of demolding performace difference, a kind of preparation method of extrusion type flame-proof silicon rubber is provided.
Methyl vinyl silicone rubber 100 parts, gas-phase silica 50 parts, 40 parts, aluminium hydroxide, magnesium hydroxide 50 parts, zinc borate 10 parts, ester type waxes 2 ~ 4 parts, antistructurizing agent 15 parts and silane coupling agent 2 ~ 4 parts are refined through banburying and opening.
Extrusion type flame-proof silicon rubber of the present invention adopts ester type waxes to be releasing agent, can the stripping of reinforced insulation layer and conductor, improve the processing characteristics of finished product cable, effectively improve traditional flame-proof silicon rubber stearic acid or silicone oil is releasing agent, easily make silicone rubber products tell white, to tell oil, demolding performace difference shortcoming.
Methyl vinyl silicone rubber, gas-phase silica, aluminium hydroxide, magnesium hydroxide, zinc borate, ester type waxes, antistructurizing agent and silane coupling agent are added in kneader, after shaping, 130 DEG C are warming up to through mixing, stop vacuum after vacuumizing 20 minutes, discharging obtains thick product; Again thick product is put into mill to carry out opening refining at least three times and obtain extrusion type flame-proof silicon rubber.
The extrusion type flame-proof silicon rubber that the inventive method is obtained, adopt unique three kinds of fire retardants (aluminium hydroxide, magnesium hydroxide, zinc borate) used in combination on the one hand, drastically reduce the area the addition of fire retardant, enhance the tensile strength of product, and flame retardant effect can reach FV0 level, the use of the defrosting compound in traditional extrusion type flame-proof silicon rubber can be reduced on the other hand, enhance the glossiness on finished cable surface.
The preferred hydroxy silicon oil of described antistructurizing agent.
Embodiment
Embodiment 1:
1, ester type waxes: prepare and 1000mol citric acid and 100L water are added in reactor simultaneously, open and stir, open the reflux backflow of reactor, reactor is warmed up to temperature in the kettle to 70 ~ 80 DEG C and dissolves citric acid, after citric acid dissolves completely, add the fatty alcohol of 3000molC12 ~ 14 again, be warming up to temperature in the kettle 110 ~ 120 DEG C and fatty alcohol is dissolved completely.Then in still, 50mol catalyzer is added---sulfuric acid, after keeping temperature 100 DEG C reaction 10h, closing volume device, slowly opens vacuum hydro-extraction, and keep temperature in the kettle to be 100 DEG C, vacuum tightness-0.09 ~-0.1MPa carries out dehydration reaction 8h.After reaction terminates, after adding neutralizing agent liquid caustic soda adjust pH to 7, vacuumizing dehydration is 0.2% to water ratio, and discharging obtains 735kg ester type waxes, and transformation efficiency is 99.59%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 1 ester type waxes 2kg, antistructurizing agent (hydroxy silicon oil) 15kg and silane coupling agent 4kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
Embodiment 2:
1, the preparation of ester type waxes: 1000mol citric acid and 100L water are simultaneously added in reactor, opens and stirs, and opens reflux backflow, be warmed up to 70 ~ 80 DEG C of dissolvings, after material dissolves completely, then add the fatty alcohol of 3500molC18 ~ 20, be warming up to temperature 110 ~ 120 DEG C dissolving.Until completely dissolved, adding 40mol catalyzer---tosic acid, after keeping temperature 130 DEG C reaction 15h, closing volume, slowly opens vacuum hydro-extraction, and keep temperature 130 DEG C, vacuum tightness-0.09 ~-0.1MPa reacts 10h.After reaction terminates, add neutralizing agent sodium carbonate and adjust pH value to 7, vacuumizing dehydration is 0.1% to water ratio, and discharging obtains 1128kg ester type waxes, and transformation efficiency is 99.65%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 2 ester type waxes 3kg, antistructurizing agent (hydroxy silicon oil) 15kg, silane coupling agent 3kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
Embodiment 3:
1, the preparation of ester type waxes: 1000mol citric acid and 100L water are simultaneously added in reactor, opens and stirs, and opens reflux backflow, be warmed up to 70 ~ 80 DEG C of dissolvings, after material dissolves completely, then add the fatty alcohol of 3200molC14-16, be warming up to temperature 110 ~ 120 DEG C dissolving.Until completely dissolved, adding 45molmol catalyzer---trifluoromethayl sulfonic acid, after keeping temperature 120 DEG C reaction 12h, closing volume, slowly opens vacuum hydro-extraction, and keep temperature 120 DEG C, vacuum tightness-0.09 ~-0.1MPa reacts 5h.Add neutralizing agent sodium bicarbonate after reaction terminates and adjust pH value to 7, vacuumizing dehydration is 0.5% to water ratio, and discharging obtains 865kg ester type waxes, and transformation efficiency is 99.70%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 3 ester type waxes 4kg, antistructurizing agent (hydroxy silicon oil) 15kg, silane coupling agent 2kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
Embodiment 4:
1, the preparation of ester type waxes: 1000mol citric acid and 100L water are simultaneously added in reactor, opens and stirs, and opens reflux backflow, be warmed up to 70 ~ 80 DEG C of dissolvings, after material dissolves completely, then add the fatty alcohol of 3100molC16 ~ 18, be warming up to temperature 110 ~ 120 DEG C dissolving.Until completely dissolved, adding 50molmol catalyzer---sulfuric acid, after keeping temperature 110 DEG C reaction 14h, closing volume, slowly opens vacuum hydro-extraction, and keep temperature 110 DEG C, vacuum tightness-0.09 ~-0.1MPa reacts 9h.After reaction terminates, add neutralizing agent sodium carbonate and adjust pH value to 7, vacuumizing dehydration is 0.1% to water ratio, and discharging obtains 928kg ester type waxes, and transformation efficiency is 99.61%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 4 ester type waxes 2 parts, antistructurizing agent (hydroxy silicon oil) 15kg, silane coupling agent 4kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
Embodiment 5:
1, the preparation of ester type waxes: 1000mol citric acid and 100L water are simultaneously added in reactor, opens and stirs, and opens reflux backflow, be warmed up to 70 ~ 80 DEG C of dissolvings, after material dissolves completely, then add 3300molC18 ~ 20 fatty alcohol, be warming up to temperature 110 ~ 120 DEG C dissolving.Until completely dissolved, adding 40molmol catalyzer---tosic acid, after keeping temperature 130 DEG C reaction 11h, closing volume, slowly opens vacuum hydro-extraction, and keep temperature 130 DEG C, vacuum tightness-0.09 ~-0.1MPa reacts 7h.After reaction terminates, add neutralizing agent sodium bicarbonate and adjust pH value to 7, vacuumizing dehydration is 0.2% to water ratio, and discharging obtains 1072kg ester type waxes, and transformation efficiency is 99.70%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 5 ester type waxes 3kg, antistructurizing agent (hydroxy silicon oil) 15kg, silane coupling agent 3kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
Embodiment 6:
1, the preparation of ester type waxes: 1000mol citric acid and 100L water are simultaneously added in reactor, opens and stirs, and opens reflux backflow, be warmed up to 70 ~ 80 DEG C of dissolvings, after material dissolves completely, then add the fatty alcohol of 3400molC14-16, be warming up to temperature 110 ~ 120 DEG C dissolving.Until completely dissolved, adding 45molmol catalyzer---trifluoromethayl sulfonic acid, after keeping temperature 110 DEG C reaction 13h, closing volume, slowly opens vacuum hydro-extraction, and keep temperature 120 DEG C, vacuum tightness-0.09 ~-0.1MPa reacts 6h.After reaction terminates, add neutralizing agent liquid caustic soda and adjust pH value to 7, vacuumizing dehydration is 0.15% to water ratio, and discharging obtains 910kg ester type waxes, and transformation efficiency is 99.65%.
2, the preparation of flame-proof silicon rubber: methyl vinyl silicone rubber 100kg, gas-phase silica 50kg, aluminium hydroxide 40kg, magnesium hydroxide 50kg, zinc borate 10kg, embodiment 6 ester type waxes 4kg, antistructurizing agent (hydroxy silicon oil) 15kg, silane coupling agent 2kg are added in kneader, the cylinder cap opening device that closes is mixing to shaping, be warming up to 130 DEG C after mixing and molding, stop Vacuum discharge after vacuumizing 20 minutes and obtain thick product; Again thick product is put into mill repeatedly to open refining and obtain extrusion type flame-proof silicon rubber.
The silicone rubber products made by above 6 examples all without tell white, tell wet goods phenomenon, and the separability of reinforced insulation layer and conductor, reach the effect that processing characteristics release property is good, product surface is smooth improving finished product cable.
Claims (3)
1. be the preparation method of the extrusion type flame-proof silicon rubber of releasing agent with ester type waxes, it is characterized in that methyl vinyl silicone rubber 100 parts, gas-phase silica 50 parts, 40 parts, aluminium hydroxide, magnesium hydroxide 50 parts, zinc borate 10 parts, ester type waxes 2 ~ 4 parts, antistructurizing agent 15 parts and silane coupling agent 2 ~ 4 parts to refine through banburying and opening; Described ester type waxes is under the effect of acid catalyst, take water as solvent, fatty alcohol and citric acid is prepared after dissolving, esterification, neutralization reaction, dehydration successively.
2. preparation method according to claim 1, methyl vinyl silicone rubber, gas-phase silica, aluminium hydroxide, magnesium hydroxide, zinc borate, ester type waxes, antistructurizing agent and silane coupling agent is it is characterized in that to add in kneader, after shaping, 130 DEG C are warming up to through mixing, stop vacuum after vacuumizing 20 minutes, discharging obtains thick product; Again thick product is put into mill to carry out opening refining at least three times and obtain extrusion type flame-proof silicon rubber.
3. preparation method according to claim 1 or 2, is characterized in that described antistructurizing agent is hydroxy silicon oil.
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Citations (6)
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| JP3080622B1 (en) * | 1999-11-24 | 2000-08-28 | 石川ミルコン株式会社 | Mold release agent for concrete |
| JP3442317B2 (en) * | 1999-07-26 | 2003-09-02 | 花王株式会社 | Full color toner |
| JP2006335884A (en) * | 2005-06-02 | 2006-12-14 | Sumitomo Dow Ltd | Flame-retardant polycarbonate resin composition |
| JP2007045908A (en) * | 2005-08-09 | 2007-02-22 | Sumitomo Dow Ltd | Flame-retardant polycarbonate resin composition |
| CN101787846A (en) * | 2010-03-05 | 2010-07-28 | 浙江凌志精细化工有限公司 | Flame-retardant high-temperature vulcanized silicone rubber strips for doors and windows of buildings and preparation method thereof |
| CN102010599A (en) * | 2010-10-28 | 2011-04-13 | 华南理工大学 | Expanded flame-retardant silicon rubber and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3442317B2 (en) * | 1999-07-26 | 2003-09-02 | 花王株式会社 | Full color toner |
| JP3080622B1 (en) * | 1999-11-24 | 2000-08-28 | 石川ミルコン株式会社 | Mold release agent for concrete |
| JP2006335884A (en) * | 2005-06-02 | 2006-12-14 | Sumitomo Dow Ltd | Flame-retardant polycarbonate resin composition |
| JP2007045908A (en) * | 2005-08-09 | 2007-02-22 | Sumitomo Dow Ltd | Flame-retardant polycarbonate resin composition |
| CN101787846A (en) * | 2010-03-05 | 2010-07-28 | 浙江凌志精细化工有限公司 | Flame-retardant high-temperature vulcanized silicone rubber strips for doors and windows of buildings and preparation method thereof |
| CN102010599A (en) * | 2010-10-28 | 2011-04-13 | 华南理工大学 | Expanded flame-retardant silicon rubber and preparation method thereof |
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