CN110229525A - A kind of preparation ionizing low deformation organosilicon foam material - Google Patents
A kind of preparation ionizing low deformation organosilicon foam material Download PDFInfo
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- CN110229525A CN110229525A CN201910525123.XA CN201910525123A CN110229525A CN 110229525 A CN110229525 A CN 110229525A CN 201910525123 A CN201910525123 A CN 201910525123A CN 110229525 A CN110229525 A CN 110229525A
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/05—Polysiloxanes containing silicon bound to hydrogen
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
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Abstract
The present invention provides a kind of preparation methods for ionizing low deformation organosilicon foam material.Pass through the synthesis of citrate silane coupling agent, and its further participate in polymerizable organosilicon reaction, highly polar ionic bond is grafted in silicone molecules chain, the strong interaction between ionic bond can be with restriction molecule chain creep, to reduce deformation of the material in ageing process.Foamed material prepared by the present invention has many advantages, such as that ageing-resistant, deformation is low and excellent in mechanical performance.
Description
Technical field
The invention belongs to technical field of polymer materials, specifically, the present invention relates to ionize low deformation organosilicon bubble
The preparation method of cotton material.
Background technique
Containing " silicon-oxygen-silicon " structure in the main chain of organosilicon material, side chain contains the organic groups such as methyl, phenyl, because
And it has both organic and inorganic material two-fold advantage.Using organosilicon polymer as matrix, using technique appropriate and foaming body
System can prepare Silicone foam, can keep organosilicon polymer high-low temperature resistant, insulation and weather resistance and light
The features such as quantization, sound absorption, damping, waterproof and sealing, is expected to replace or part replaces carbon-based high molecular foam material, has wide
Application prospect.
Organosilicon foam material has been more and more widely used, close as damping especially in batteries of electric automobile packet
Packing proposes harsher requirement to permanent deformation after its heat ageing, so preparing a kind of anti-aging, low deformation organosilicon bubble
Foam material is just particularly important.
Improving the main method of organosilicon foam material at present is that crosslinking agent, thermostabilization are largely added in organosilicon systems
Agent and antioxidant are affected to organosilicon material comprehensive performance, are unfavorable for although improving to ageing properties
Prepare the organosilicon foam material of excellent combination property.
In consideration of it, urgently finding out a kind of organic-silicon-modified method at present, the organosilicon foam of anti-aging, low deformation is prepared
Material.
Summary of the invention
It is an object of the invention to carry out Ionization Modification to silicone molecules chain, low deformation organosilicon foamed cotton material is prepared
Material is suitable for the fields such as batteries of electric automobile packet gasket.
The present invention provides a kind of preparation methods for ionizing low deformation organosilicon foam material.To reduce organosilicon foam
Deformation of the material in ageing process, present invention design introduce ionization citrate in silicone molecules chain, are divided with reducing
The deformation of subchain.
The preparation for ionizing low deformation organosilicon foam material includes following raw material: citrate silane coupling agent, silicone oil,
Crosslinking agent, curing agent, foaming agent, reinforcing agent.
Preferably, the preparation of the citrate silane coupling agent includes the following raw material: citrate, silane coupling agent.
Preferably, the citrate silane coupling agent includes the raw material of following molar part: 1 mole of the silane coupling agent
Part, the silane coupling agent 1-2 molar part.
Preferably, the citrate is one of sodium dihydrogen citrate, disodium citrate, zinc citrate, calcium citrate
Or compounding.
Preferably, the silane coupling agent is one of amino trimethoxy silane, amino triethoxysilane or answers
Match.
Preferably, the silicone oil is one of hydroxy silicon oil, vinyl silicone oil, containing hydrogen silicone oil.
Preferably, the preparation method of the citrate silane coupling agent is that reflux condensing tube, blender, temperature are being housed
In the four-hole bottle of degree meter and logical nitrogen device, the citrate and silane coupling agent of molar ratio 1:1 to 1:2 is added, in 100-150
It DEG C is stirred to react 2-4h, up to product after natural cooling filtering.
Preferably, the preparation method of the low deformation foam material is by silicone oil, citrate silane coupling agent, to foam
The presoma of agent, crosslinking agent, curing agent, reinforcing agent after mixing evenly is coated between two layers of release film, solidification foaming to get.
Low deformation organosilicon foam is ionized in the application of Material Field.
Compared with the prior art, the present invention has the following beneficial effects:
Present invention design carries out Ionization Modification to silicone molecules chain.Citrate silicon is grafted on silicone molecules chain
Alkane coupling agent controls the creep of ageing process middle-molecular-weihydroxyethyl so that the side chain in silicone molecules chain introduces polar ion key, into
And prepare the low deformation organosilicon foam material of ionization.Operation of the present invention is simple, and the foam material of preparation has ageing-resistant, shape
It is lower and the advantages that excellent in mechanical performance
Specific embodiment
The person that is not specified actual conditions in various embodiments of the present invention, carries out according to conventional conditions or manufacturer's recommended conditions.
Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.It is used in each embodiment
Raw material is that market is bought.
The producer of used raw material and information in 1 embodiment of table
It should be noted that above-mentioned raw materials of the invention may be used also the above is only the source of the raw material used in the present embodiment
Using other commercially available conventional products, different manufacturers, model raw material have no effect on the implementation and technology of technical solution of the present invention
The realization of effect.
Embodiment 1
The preparation of the low deformation organosilicon foam material of ionization of the present embodiment, is grafted citric acid on silicone molecules chain
Salt silane coupling agent introduces polar ion key, reduces organosilicon foam material in the deformation of ageing process.
The preparation of the citrate silane coupling agent includes the raw material of following parts by weight: the citrate 29.1g,
The silane coupling agent 33.2g.Wherein the citrate is sodium dihydrogen citrate;The silane coupling agent is amino triethoxy
Silane coupling agent.
It include the raw material of following parts by weight: silicone oil 100g, curing agent 4g, crosslinking agent 6g, lemon in the organosilicon foam
Hydrochlorate silane coupling agent 4g, foaming agent 2g, reinforcing agent 5g.Wherein, the silicone oil is vinyl base silicone oil;The vinyl base silicon
Oil is silicone oil of the viscosity in 50000Cst.The curing agent is azodiisobutyronitrile;The crosslinking agent is 2,5- dimethyl -2,5-
Bis(t-butylperoxy) hexane;The foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
The low deformation organosilicon foam of the ionization the preparation method is as follows:
(1) in the four-hole bottle equipped with reflux condensing tube, blender, thermometer and logical nitrogen device, selected weight is added
The sodium dihydrogen citrate and amino triethoxysilane for measuring part, 3h are stirred to react in 110 DEG C, natural cooling is up to citrate silane
Coupling agent.
(2) silicone oil of selected parts by weight is placed in container, is being added described in selected parts by weight thereto
Crosslinking agent, citrate silane coupling agent, foaming agent, curing agent, reinforcing agent, 0.5h is to uniform for stirring, obtains organosilicon forerunner
Then body is coated between the tetrafluoro nethike embrane, in baking oven 130 DEG C of foaming 0.5h, 180 DEG C of solidification 1h to get.
As the interchangeable embodiment of the present embodiment, the sodium dihydrogen citrate could alternatively be disodium citrate, lemon
One of sour zinc, calcium citrate or compounding;The amino triethoxysilane coupling agent could alternatively be amino trimethoxy
Silane coupling agent or compounding.
Embodiment 2
The preparation of the low deformation organosilicon foam material of ionization of the present embodiment, is grafted citric acid on silicone molecules chain
Salt silane coupling agent introduces polar ion key, reduces Silicone foam in the deformation of ageing process.
The preparation of the citrate silane coupling agent includes the raw material of following parts by weight: the citrate 29.1g,
The silane coupling agent 36.5g.Wherein the citrate is sodium dihydrogen citrate;The silane coupling agent is amino triethoxy
Silane coupling agent.
It include the raw material of following parts by weight: silicone oil 100g, curing agent 4g, crosslinking agent 6g, lemon in the organosilicon foam
Hydrochlorate silane coupling agent 4g, foaming agent 2g, reinforcing agent 5g.Wherein, the silicone oil is hydroxy silicon oil;The hydroxy silicon oil is viscosity
For the silicone oil of 40000Cst.The curing agent is to have dibutyl tin dilaurate;The crosslinking agent is tetramethoxy-silicane, described
Foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
The low deformation organosilicon foam material of the ionization the preparation method is as follows:
(1) in the four-hole bottle equipped with reflux condensing tube, blender, thermometer and logical nitrogen device, selected weight is added
The sodium dihydrogen citrate and amino triethoxysilane for measuring part, 2.5h are stirred to react in 120 DEG C, natural cooling is up to citrate silicon
Alkane coupling agent.
(2) silicone oil of selected parts by weight is placed in container, is being added described in selected parts by weight thereto
Citrate silane coupling agent, foaming agent, reinforcing agent, 0.5h is to uniform for stirring, obtains the mixture containing organic silicone oil, is added solid
Agent, crosslinking agent are uniformly mixing to obtain rapidly presoma, are then coated between the tetrafluoro nethike embrane, in baking oven
140 DEG C of foaming 0.4h, 180 DEG C of solidification 1h to get.
As the interchangeable embodiment of the present embodiment, the hydroxy silicon oil also can be replaced viscosity in 1000-
The hydroxy silicon oil of arbitrary value within the scope of 10000Cst.
Embodiment 3
The preparation of the low deformation organosilicon foam material of ionization of the present embodiment, is grafted citric acid on silicone molecules chain
Salt silane coupling agent introduces polar ion key, reduces Silicone foam in the deformation of ageing process.
The preparation of the citrate silane coupling agent includes the raw material of following parts by weight: the citrate 29.1g,
The silane coupling agent 40.1g.Wherein the citrate is that sodium dihydrogen citrate and disodium citrate are multiple according to molar ratio 1:1
Match;The silane coupling agent is amino triethoxysilane coupling agent.
It include the raw material of following parts by weight: silicone oil 100g, curing agent 4g, crosslinking agent 6g, lemon in the organosilicon foam
Hydrochlorate silane coupling agent 4g, foaming agent 2.2g, reinforcing agent 5g.Wherein, the silicone oil is vinyl silicone oil;The vinyl silicone oil
For viscosity 40000Cst silicone oil.The curing agent is benzoyl peroxide;The crosslinking agent is 2,5- dimethyl -2,5- double
(t-butylperoxy) hexane;The foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
The low deformation organosilicon foam material of the ionization the preparation method is as follows:
(1) in the four-hole bottle equipped with reflux condensing tube, blender, thermometer and logical nitrogen device, selected weight is added
Sodium dihydrogen citrate, disodium citrate and the amino triethoxysilane for measuring part, 2h are stirred to react in 130 DEG C, natural cooling to obtain the final product
Citrate silane coupling agent.
(2) silicone oil of selected parts by weight is placed in container, is being added described in selected parts by weight thereto
Crosslinking agent, citrate silane coupling agent, foaming agent, curing agent, reinforcing agent, 0.5h is to uniform for stirring, obtains organosilicon forerunner
Then body is coated between the tetrafluoro nethike embrane, in baking oven 130 DEG C of foaming 0.5h, 200 DEG C of solidification 0.5h to get.
As the interchangeable embodiment of the present embodiment, the vinyl silicone oil also can be replaced viscosity in 1000-
The vinyl silicone oil of arbitrary value within the scope of 10000Cst.
Embodiment 4
The preparation of the low deformation organosilicon foam material of ionization of the present embodiment, is grafted citric acid on silicone molecules chain
Salt silane coupling agent introduces polar ion key, reduces Silicone foam in the deformation of ageing process.
The preparation of the citrate silane coupling agent includes the raw material of following parts by weight: the citrate 29.1g,
The silane coupling agent 42g.Wherein the citrate is sodium dihydrogen citrate;The silane coupling agent is amino trimethoxy silicon
Alkane and amino triethoxysilane are compounded according to molar ratio 1:1.
Include the raw material of following parts by weight in the organosilicon foam: silicone oil 100g, curing agent 4g, citrate silane are even
Join agent 8g, reinforcing agent 5g.Wherein, the silicone oil is vinyl silicone oil and containing hydrogen silicone oil;The vinyl silicone oil is that viscosity exists
The silicone oil of 5000Cst, the containing hydrogen silicone oil are the silicone oil that viscosity is 8000Cst.The curing agent is azodiisobutyronitrile and tin
The compounding of class catalyst.
The low deformation organosilicon foam material of the ionization the preparation method is as follows:
(1) in the four-hole bottle equipped with reflux condensing tube, blender, thermometer and logical nitrogen device, selected weight is added
Sodium dihydrogen citrate, amino trimethoxy silane and the amino triethoxysilane for measuring part, are stirred to react 2.5h in 130 DEG C, natural
Cooling citrate silane coupling agent to obtain the final product.
(2) silicone oil of selected parts by weight is placed in container, is being added described in selected parts by weight thereto
Crosslinking agent, citrate silane coupling agent, foaming agent, curing agent, reinforcing agent, 0.5h is to uniform for stirring, obtains organosilicon forerunner
Then body is coated between the tetrafluoro nethike embrane, in room temperature curing 10min, be placed on 120 DEG C of foaming in baking oven
1h, after 180 DEG C solidification 1h to get.
As the interchangeable embodiment of the present embodiment, the vinyl silicone oil also can be replaced viscosity in 1000-
The vinyl silicone oil of arbitrary value within the scope of 10000Cst, the containing hydrogen silicone oil can be replaced viscosity in 1000-10000Cst
The containing hydrogen silicone oil of arbitrary value in range.
Comparative example 1
The difference of the organosilicon foam material and the low deformation organosilicon foam material in embodiment 1 of this comparative example only exists
In without using citrate silane coupling agent in preparation step, specific implementation process is as follows:
It include the raw material of following parts by weight in the organosilicon foam: silicone oil 100g, curing agent 4g, crosslinking agent 6g, foaming
Agent 2g, reinforcing agent 5g.Wherein, the silicone oil is vinyl base silicone oil;The vinyl base silicone oil is viscosity 50000Cst's
Silicone oil.The curing agent is azodiisobutyronitrile;The crosslinking agent be 2,5- dimethyl -2,5- bis(t-butylperoxy) oneself
Alkane;The foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
The organosilicon foam the preparation method is as follows:
The silicone oil of selected parts by weight is placed in container, in the crosslinking that selected parts by weight are added thereto
Agent, foaming agent, curing agent, reinforcing agent, are stirred until homogeneous, and obtain organosilane precursor, be then coated on tetrafluoro nethike embrane it
Between, in drying tunnel 160 DEG C of foaming 0.5h, 180 DEG C of solidification 1h to get.
Comparative example 2
The low deformation organosilicon foam material and the low deformation Silicone foam in embodiment 1 of this comparative example, difference
It is only that, citrate silane coupling agent is not used in preparation step, and equivalent heat stabilizer is added in the feed, be embodied
Process is as follows:
It include the raw material of following parts by weight in the organosilicon foam: silicone oil 100g, curing agent 4g, crosslinking agent 6g, foaming
Agent 2g, heat stabilizer 4g, reinforcing agent 5g.Wherein, the silicone oil is vinyl base silicone oil;The vinyl base silicone oil is that viscosity exists
The silicone oil of 50000Cst.The curing agent is azodiisobutyronitrile;The crosslinking agent is the bis- (tert-butyls of 2,5- dimethyl -2,5-
Peroxy) hexane;The foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
The organosilicon foam the preparation method is as follows:
The silicone oil of selected parts by weight is placed in container, in the crosslinking that selected parts by weight are added thereto
Agent, foaming agent, curing agent, heat stabilizer, reinforcing agent, are stirred until homogeneous, and obtain organosilane precursor, are then coated on four
Between fluorine nethike embrane, in drying tunnel 160 DEG C of foaming 0.5h, 180 DEG C of solidification 1h to get.
Comparative example 3
The low deformation organosilicon foam material and the low deformation Silicone foam in embodiment 1 of this comparative example, difference
It is only that, preparation method is different from embodiment 1, and without the step (1), specific implementation process is as follows:
It include the raw material of following parts by weight in the organosilicon foam: silicone oil 100g, curing agent 4g, crosslinking agent 6g, foaming
Agent 2g, reinforcing agent 5g, citrate 29.1g, silane coupling agent 33.2g.Wherein the citrate is sodium dihydrogen citrate;It is described
Silane coupling agent is aminopropyl triethoxysilane coupling agent;The silicone oil is vinyl base silicone oil;The vinyl base silicone oil
For viscosity 50000Cst silicone oil.The curing agent is azodiisobutyronitrile;The crosslinking agent is 2,5- dimethyl -2,5- double
(t-butylperoxy) hexane;The foaming agent is sodium bicarbonate;The reinforcing agent is white carbon black.
It is described have the low deformation organosilicon foam material of ionization the preparation method is as follows:
(1) silicone oil of selected parts by weight is placed in container, is being added described in selected parts by weight thereto
Crosslinking agent, citrate, silane coupling agent, foaming agent, curing agent, reinforcing agent, 0.5h is to uniform for stirring, before obtaining organosilicon
Body is driven, is then coated between the tetrafluoro nethike embrane, 130 DEG C of foaming 0.5h, 180 DEG C of solidification 1h in baking oven, i.e.,
?.
Effete test embodiment
For the Ionization Modification and its low deformation Silicone foam for verifying silicone molecules chain of the present invention
Technical effect carries out compliance test result experiment.
The deformation Silicone foam being prepared in Example 1-4, comparative example 1-3 carries out as follows respectively
Experiment:
It is 50% according to ASTM standard and according to decrement, under conditions of temperature is 100 DEG C, ageing time is 1000h,
Measure the compression set rate of the Silicone foam;
According to National Standard of the People's Republic of China GB/T 6343-2009/ISO 845:2006 to obtained described organic
Silicon foam material carries out apparent density test;
Then the tensile strength and elongation at break of the organosilicon foamed products are measured using universal tensile testing machine;
Its experimental result is as follows:
2 compliance test result experimental result of table
By above-mentioned experimental result it can be seen that comparative example 1-4 and comparative example 1-3, by silicone molecules chain ion
Changing organosilicon material that is modified and preparing has lower Compression Set and keeps preferable mechanical property, can prepare low
Deformation, high performance organosilicon foam material.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (7)
1. ionizing the preparation of low deformation organosilicon foam, which is characterized in that pass through carboxyl in citrate and amino silicone
Synthesizing citric acid silane coupling agent is reacted, and then participates in polymerizable organosilicon reaction, the introducing of highly polar ionic bond can in strand
Strand creep is controlled, the deformation after reducing Silicone foam aging.
2. the low deformation organosilicon foam of ionization according to claim 1, which is characterized in that the low shape of the low ionization
Become organosilicon foam preparation include following raw material: citrate silane coupling agent, silicone oil, crosslinking agent, curing agent, foaming agent,
Reinforcing agent.
3. according to claim 2 ionize low deformation organosilicon foam, which is characterized in that the citrate silane
Coupling agent is amino trimethoxy silicon by the preparation of the amidation process of silane coupling agent and citrate, the silane coupling agent
One kind or compounding of alkane, amino triethoxysilane;The citrate be sodium dihydrogen citrate, disodium citrate, zinc citrate,
One of calcium citrate or compounding.
4. according to claim 3 ionize low deformation organosilicon foam, which is characterized in that the citrate silane
The preparation method of coupling agent is, in the four-hole bottle equipped with reflux condensing tube, blender, thermometer and logical nitrogen device, is added
The citrate and silane coupling agent of molar ratio 1:1 to 1:2 is stirred to react 2-4h in 100-150 DEG C, and natural cooling, filtering is admittedly
After body impurity, liquid is up to product.
5. according to claim 1 ionize low deformation organosilicon foam, which is characterized in that described to ionize low deformation
The preparation method of organosilicon foam is, after mixing evenly by silicone oil, citric acid silane coupling agent, foaming agent, crosslinking agent, reinforcing agent
Presoma be coated between two layers of release film, solidification foaming, be prepared density be 300-600kg/m3 organosilicon foamed cotton material
Material.
6. according to claim 5 ionize low deformation organosilicon foam, which is characterized in that described to ionize low deformation
Organosilicon foam includes but is not limited to use hydroxy silicon oil, vinyl silicone oil and containing hydrogen silicone oil, by physically or chemically foaming
The organosilicon foam arrived.
7. a kind of ionize low deformation organosilicon foam in the application of Material Field.
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