CN106832956A - A kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber - Google Patents
A kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber Download PDFInfo
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- CN106832956A CN106832956A CN201710073269.6A CN201710073269A CN106832956A CN 106832956 A CN106832956 A CN 106832956A CN 201710073269 A CN201710073269 A CN 201710073269A CN 106832956 A CN106832956 A CN 106832956A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention belongs to organosilicon polymer field of new, there is provided a kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber, comprise the following steps：By vinyl silicone oil, hydroxy silicon oil, reinforced filling, fire-retardant filler and antistructurizing agent, it is heat-treated, is cooled to room temperature and obtains base rubber；The base rubber is taken, viscosity modifier and catalyst is added, stirring obtains A glue；The base rubber is taken, viscosity modifier, crosslinking agent and inhibitor is added, stirring obtains B glue；By A glue, B glue with mass ratio be 1:Room temperature foamed solidification after 1 mixing, obtains the flame retardant type cold curing foaming liquid silicon rubber.The preparation method is by choosing the flame retardant type cold curing foaming liquid rubber composition that suitable feedstock and preparation condition are obtained, with proportion is small by 0.1~0.9, resilience is high by 70%~90%, asepsis environment-protecting, anti-flammability reaches UL94 V0 grades, whole Making programme is simple, and production efficiency is high.
Description
Technical field
The invention belongs to organosilicon polymer field of new, and in particular to a kind of flame retardant type cold curing foaming liquid silicon
The preparation method of rubber.
Background technology
Current foamed silastic application is very universal, because of the soft and elasticity of the existing general sponge of foamed silastic, also has
There is a series of characteristic such as heat-resisting, cold-resistant, ageing-resistant, corrosion-resistant of silicon rubber, in daily necessities, electric power, electronics, automobile, work
The fields such as industry, precision instrument are widely used.Because silastic material is to human and environment nontoxic pollution-free, and with very
Good application, so application surface is also more and more extensive.With carrying for the pay attention to day by day to safety problem, particularly awareness of the importance of fire prevention
Height, foamed material poor fire, fire has greatly safety to the people hidden to the security of the lives and property of country
Suffer from, the flame retardant rating of foamed material turns into the important indicator that we apply, although common foamed silastic is with certain fire-retardant
Property, but the not up to flame retardant effect of UL94-V0 ranks, however it remains potential safety hazard.
Therefore, the prior art is defective, need to improve.
The content of the invention
To overcome the defect of prior art, the invention provides a kind of system of flame retardant type cold curing foaming liquid silicon rubber
Preparation Method.
The present invention is achieved in that a kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber, including such as
Lower step：
The vinyl silicone oil of 20~100 mass parts, the hydroxy silicon oil of 1~60 mass parts, the reinforcement of 1~50 mass parts are filled out
Material, the fire-retardant filler of 1~80 mass parts, the antistructurizing agent of 1~60 mass parts, and it is heat-treated 0.5 at 90 DEG C~160 DEG C
~6 hours, it is cooled to room temperature and obtains base rubber；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, 0.005~5 mass parts are added
Platinum catalyst, stirring, obtain A glue；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, the friendship of 1~60 mass parts is added
Connection agent, the inhibitor of 0.0001~5 mass parts, stirring, obtain B glue；
By A glue and B glue with mass ratio be 1:Room temperature foamed solidification after 1 mixing, obtains the flame retardant type cold curing foaming
Liquid silastic.
Beneficial effect：The preparation method of flame retardant type cold curing foaming liquid silicon rubber provided in an embodiment of the present invention, with
The dehydrogenation foaming under the catalysis of platinum complex of containing hydrogen silicone oil and hydroxy silicon oil, coordinates the fire-retardant filler with flame retardant effect, reachable
To the use requirement of flame retardant type cold curing foaming liquid silicon rubber.Its Making programme is simple, and production efficiency is high, and to environment
It is nontoxic pollution-free, low production cost, room temperature foamed solidification, it is not necessary to heat, proportion is small to be capable of achieving 0.1~0.9；Obtain
Flame retardant type cold curing foaming liquid silicon rubber, is remarkably improved the flame retardant rating of foamed silastic, can reach UL94-V0 grades,
The resilience of foamed silastic is also remarkably improved, more than 70% can be reached, in addition with the universal of common foamed silastic
Characteristic；Fire-retardant, filling, damping, buffering, sealing, sound insulation, anti-high and low-temp can be widely used in.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
The embodiment of the present invention provides a kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber, including following step
Suddenly：
The vinyl silicone oil of 20~100 mass parts, the hydroxy silicon oil of 1~60 mass parts, the reinforcement of 1~50 mass parts are filled out
Material, the fire-retardant filler of 1~80 mass parts, the antistructurizing agent of 1~60 mass parts, and it is heat-treated 0.5 at 90 DEG C~160 DEG C
~6 hours, it is cooled to room temperature and obtains base rubber；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, 0.005~5 mass parts are added
Platinum catalyst, stirring, obtain A glue；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, the friendship of 1~60 mass parts is added
Connection agent, the inhibitor of 0.0001~5 mass parts, stirring, obtain B glue；
By A glue and B glue with mass ratio be 1:Room temperature foamed solidification after 1 mixing, obtains the flame retardant type cold curing foaming
Liquid silastic.
The preparation method of flame retardant type cold curing foaming liquid silicon rubber provided in an embodiment of the present invention, with containing hydrogen silicone oil and
Hydroxy silicon oil dehydrogenation foaming under the catalysis of platinum complex, coordinates the fire-retardant filler with flame retardant effect, can reach flame retardant type room
The use requirement of temperature solidification foaming liquid silicon rubber.Its Making programme is simple, and production efficiency is high, and to the nontoxic nothing of environment
Pollution, low production cost, room temperature foamed solidification, it is not necessary to heat, proportion is small to be capable of achieving 0.1~0.9；The flame retardant type room temperature for obtaining
Solidification foaming liquid silicon rubber, is remarkably improved the flame retardant rating of foamed silastic, can reach UL94-V0 grades, can also significantly carry
The resilience of high-foaming silicon rubber, can reach more than 70%.
Specifically, the vinyl silicone oil is that straight-chain ethylene base blocks polymethyl siloxane, and ethene is contained in center section
Base chain link, the structural formula of the vinyl silicone oil is as follows：
Wherein, m is that 50~1000, n is 0~5.
The viscosity of the vinyl silicone oil be 500MPa.s~150000MPa.s, preferably 1000MPa.s~
100000MPa.s。
Specifically, the hydroxy silicon oil is that structural formula end group as follows is hydroxy-end capped dimethyl silicone polymer：
Wherein, n is 10~1000.
The viscosity of the hydroxy silicon oil is 100MPa.s~10000MPa.s, preferably 1000MPa.s~5000MPa.s.
Specifically, the reinforced filling includes at least one in aerosil, precipitated silica；The gas phase
Silica, the specific surface area of precipitated silica are preferably 150m2/ more than g, more preferably 300~400m2/g。
Specifically, the fire-retardant filler include aluminium hydroxide, zinc oxide, strontium hydroxide, magnesium hydroxide and carbon black in extremely
Few one kind.The particle diameter of the fire-retardant filler is preferably 1800~18000 mesh, more preferably 2500~12500 mesh.
Specifically, the content of platinum is 500~5000ppm in the platinum catalyst；Preferably 2000~4000ppm, enters
One step is preferably 3000~4000ppm.
Specifically, the crosslinking agent is blocked containing hydrogen silicone oil, with the structure that following structural formula is represented：
Wherein, m is that 0~20, n is 0~50.
The hydrogen content of the blocked containing hydrogen silicone oil is preferably 1.2%~1.6%, more preferably 1.4%~
1.6%.
Specifically, the inhibitor be alkynol, propilolic alcohol, phenylacetylene and divinyl tetramethyl disiloxane at least
One kind, preferably alkynol.
Specifically, the antistructurizing agent includes diphenyl glycol, dimethyldialkylammonium TMOS and the silicon of hexamethyl two
At least one in azane.
Specifically, the viscosity modifier is vinyl silicone oil or hydroxy silicon oil.The viscosity of the viscosity modifier is preferred
It is 10MPa.s~10000MPa.s, more preferably 100MPa.s~1000MPa.s.
The preparation method of flame retardant type cold curing foaming liquid silicon rubber provided in an embodiment of the present invention is suitable by choosing
The flame retardant type cold curing foaming liquid rubber composition that raw material and preparation condition are obtained, with proportion it is small by 0.1~0.9, return
Bullet is high by 70%~90%, asepsis environment-protecting, and anti-flammability reaches UL94-V0, and whole Making programme is simple, and production efficiency is high.
Embodiment 1
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the diphenyl silanediol of 12 mass parts, and heat treatment 5 hours at 140 DEG C, cooling
Base rubber is obtained to room temperature；The base rubber of 70 mass parts is taken, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, plus
Enter the platinum catalyst that 1 mass parts Pt contents are 4000ppm, stir, obtain A glue；The another base rubber for taking 70 mass parts, plus
Enter the hydroxy silicon oil that 30 mass parts viscosity are 1000mPa.s, add containing hydrogen silicone oil, 0.02 that 10 mass parts hydrogen contents are 1.5%
The alkynol of mass parts, stirs, and obtains B glue；By A glue and B glue with mass ratio be 1:Room temperature foamed solidification after 1 mixing, obtains institute
State flame retardant type cold curing foaming liquid rubber composition.
Embodiment 2
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the aluminium hydroxide and carbon black of 5 mass parts, the diphenyl silanediol of 14 mass parts, and
It is heat-treated 5 hours at 140 DEG C, is cooled to room temperature and obtains base rubber；The base rubber of 70 mass parts is taken, 30 mass parts viscosity of addition are
The hydroxy silicon oil of 1000mPa.s, it is the platinum catalyst of 4000ppm to add 1 mass parts Pt contents, is stirred, and obtains A glue；Separately
The base rubber of 70 mass parts is taken, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, adds 10 mass parts hydrogen contents
For 1.6% containing hydrogen silicone oil, 0.02 mass parts alkynol, stir, obtain B glue；By A glue, B glue with mass ratio be 1:1 mixing
Room temperature foamed solidification, obtains the flame retardant type cold curing foaming liquid rubber composition afterwards.
Embodiment 3
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the aluminium hydroxide and carbon black of 10 mass parts, the diphenyl silanediol of 16 mass parts, and
It is heat-treated 5 hours at 140 DEG C, is cooled to room temperature and obtains base rubber；The base rubber of 70 mass parts is taken, 30 mass parts viscosity are added
It is the hydroxy silicon oil of 1000mPa.s, it is the platinum catalyst of 4000ppm to add 1 mass parts Pt contents, is stirred, and obtains A glue；
The another base rubber for taking 70 mass parts, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, adds 10 mass parts hydrogen to contain
Containing hydrogen silicone oil, the alkynol of 0.02 mass parts for 1.6% are measured, is stirred, obtain B glue；By A glue, B glue with mass ratio be 1:1 mixes
Room temperature foamed solidification after conjunction, obtains the flame retardant type cold curing foaming liquid rubber composition.
Embodiment 4
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the aluminium hydroxide and carbon black of 15 mass parts, the diphenyl silanediol of 18 mass parts, and
It is heat-treated 5 hours at 140 DEG C, is cooled to room temperature and obtains base rubber；The base rubber of 70 mass parts is taken, 30 mass parts viscosity are added
It is the hydroxy silicon oil of 1000mPa.s, it is the platinum catalyst of 4000ppm to add 1 mass parts Pt contents, is stirred, and obtains A glue；
The another base rubber for taking 70 mass parts, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, adds 10 mass parts hydrogen to contain
Containing hydrogen silicone oil, the alkynol of 0.02 mass parts for 1.6% are measured, is stirred, obtain B glue；By A glue, B glue with mass ratio be 1:1 mixes
Room temperature foamed solidification after conjunction, obtains the flame retardant type cold curing foaming liquid rubber composition.
Embodiment 5
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the aluminium hydroxide and carbon black of 20 mass parts, the diphenyl silanediol of 20 mass parts, and
It is heat-treated 5 hours at 140 DEG C, is cooled to room temperature and obtains base rubber；The base rubber of 70 mass parts is taken, 30 mass parts viscosity are added
It is the hydroxy silicon oil of 1000mPa.s, it is the platinum catalyst of 4000ppm to add 1 mass parts Pt contents, is stirred, and obtains A glue；
The another base rubber for taking 70 mass parts, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, adds 10 mass parts hydrogen to contain
Containing hydrogen silicone oil, the alkynol of 0.02 mass parts for 1.6% are measured, is stirred, obtain B glue；By A glue, B glue with mass ratio be 1:1 mixes
Room temperature foamed solidification after conjunction, obtains the flame retardant type cold curing foaming liquid rubber composition.
Embodiment 6
By the vinyl silicone oil of the viscosity of 100 mass parts 70,000, the hydroxy silicon oil of 500 viscosity of 40 mass parts, 30 mass parts ratios
Surface area is 380 fume colloidal silica, the aluminium hydroxide and carbon black of 25 mass parts, the diphenyl silanediol of 22 mass parts, and
It is heat-treated 5 hours at 140 DEG C, is cooled to room temperature and obtains base rubber；The base rubber of 70 mass parts is taken, 30 mass parts viscosity are added
It is the hydroxy silicon oil of 1000mPa.s, it is the platinum catalyst of 4000ppm to add 1 mass parts Pt contents, is stirred, and obtains A glue；
The another base rubber for taking 70 mass parts, it is the hydroxy silicon oil of 1000mPa.s to add 30 mass parts viscosity, adds 10 mass parts hydrogen to contain
Containing hydrogen silicone oil, the alkynol of 0.02 mass parts for 1.6% are measured, is stirred, obtain B glue；By A glue, B glue with mass ratio be 1:1 mixes
Room temperature foamed solidification after conjunction, obtains the flame retardant type cold curing foaming liquid rubber composition.
The flame retardant type cold curing foaming liquid rubber composition that embodiment 1~6 is obtained is done into test piece, performance survey is carried out
Examination (hardness, tensile strength, tearing strength, elongation, resilience, proportion and flame out time), as a result as shown in table 1.
Table 1
From table 1 it follows that when the aluminium hydroxide and carbon black of 15 mass parts is added in formula, with the knot of 18 mass parts
During the room temperature foamed solidification liquid silastic of structure controlling agent diphenyl silanediol production, combination property reaches most preferably.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber, it is characterised in that comprise the following steps：
By the vinyl silicone oil of 20~100 mass parts, the hydroxy silicon oil of 1~60 mass parts, the reinforced filling of 1~50 mass parts, 1
The fire-retardant filler of~80 mass parts, the antistructurizing agent of 1~60 mass parts, and 0.5~6 is heat-treated at 90 DEG C~160 DEG C
Hour, it is cooled to room temperature and obtains base rubber；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, the platinum of 0.005~5 mass parts is added
Au catalyst, stirring, obtains A glue；
The base rubber of 100 mass parts is taken, the viscosity modifier of 1~70 mass parts is added, the crosslinking of 1~60 mass parts is added
Agent, the inhibitor of 0.0001~5 mass parts, stirring, obtain B glue；
By A glue and B glue with mass ratio be 1:Room temperature foamed solidification after 1 mixing, obtains the flame retardant type cold curing foaming liquid
Silicon rubber.
2. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Vinyl silicone oil is that straight-chain ethylene base blocks polymethyl siloxane, and vinyl chain link, the vinyl silicon are contained in center section
The structural formula of oil is as follows：
Wherein, m is that 50~1000, n is 0~5.
3. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Hydroxy silicon oil is that structural formula end group as follows is hydroxy-end capped dimethyl silicone polymer：
Wherein, n is 10~1000.
4. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Reinforced filling includes at least one in aerosil, precipitated silica.
5. the preparation method of the flame retardant type cold curing foaming liquid silicon rubber as described in claim 1 or 4, it is characterised in that
The fire-retardant filler includes at least one in aluminium hydroxide, zinc oxide, strontium hydroxide, magnesium hydroxide and carbon black.
6. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
The content of platinum is 500~5000ppm in platinum catalyst.
7. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Crosslinking agent is blocked containing hydrogen silicone oil, with the structure that following structural formula is represented：
Wherein, m is that 0~20, n is 0~50.
8. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Inhibitor is at least one in alkynol, propilolic alcohol, phenylacetylene and divinyl tetramethyl disiloxane.
9. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that described
Antistructurizing agent includes at least one in diphenyl silanediol, dimethyldialkylammonium TMOS and HMDS.
10. the preparation method of flame retardant type cold curing foaming liquid silicon rubber as claimed in claim 1, it is characterised in that institute
Viscosity modifier is stated for vinyl silicone oil or hydroxy silicon oil.
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