CN110437617A - A kind of preparation method of organosilicone elastic gel - Google Patents
A kind of preparation method of organosilicone elastic gel Download PDFInfo
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- CN110437617A CN110437617A CN201810410157.XA CN201810410157A CN110437617A CN 110437617 A CN110437617 A CN 110437617A CN 201810410157 A CN201810410157 A CN 201810410157A CN 110437617 A CN110437617 A CN 110437617A
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- elastic gel
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- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention belongs to organosilicon material fields, and in particular to a kind of preparation method of organosilicone elastic gel.A kind of preparation method of organosilicone elastic gel, including following preparation step: the alkadienes that organic solvent, containing hydrogen silicone oil, the polysiloxanes of at least two vinyl or both ends are unsaturated double-bond is added in reactor, catalyst is added after being uniformly mixed, is warming up to 50~90 DEG C of progress precipitation polymerizations and reacts 2~9h；It is cooled to 40 DEG C or less after the reaction was completed, filtering, obtained solid powder is through drying, obtain elastomer silicone powder, then elastomer silicone powder is diluted swelling with diluent, and stabilizer is added, 1~2h, which is stirred, at 70~90 DEG C, under the conditions of 30~90rpm obtains the organosilicone elastic gel；The organic solvent refers to that the volatile organic solvent that can dissolve reaction raw materials but insoluble polymeric reaction product, product can mutually be mixed in a shear condition with arbitrary proportion with the oil in formula.
Description
Technical field
The invention belongs to organosilicon material fields, and in particular to a kind of preparation method of organosilicone elastic gel.
Background technique
Elastomer silicone refers to and contains polymeric silicon with different cross-linked networks.According to the difference of state, can divide
Are as follows: elastomer silicone powder, silicone elastomer emulsions, organosilicone elastic gel.Dimethicone crosspolymers with
The mixture of diluent, referred to as organosilicone elastic gel are that have the organosilicon crosslinked polymer of tridimensional network and small point
The mixture of sub- solvent.Organosilicone elastic gel can assign unique skin sense as skin " velvet " and therefore be widely used in
The daily cosmetics such as skin care, color make-up, antiperspirant field.
The preparation process flow of traditional organosilicone elastic gel has following two methods:
Method (1): the nascent gel of elastomer silicone is first prepared, then nascent gel mechanical is sheared and is crushed, then is used
Gel swelling is diluted to required solid content by diluent, finally obtains uniform organosilicone elastic gel by mixed at high speed.
Method (2): spray solidification technology.This method is that liquid charging stock is sprayed into hot setting room using spraying device to carry out
Solidification obtains elastomer silicone powder, then elastomer powder swelling is diluted to required solid content with diluent, finally passes through
Mixed at high speed obtains uniform organosilicone elastic gel.
As 104244920 B of patent CN prepares organosilicon elastic gel using the above method (1): first will be in addition to catalyst
All the components be added, be slowly stirred, until obtaining uniform mixture, then catalyst be added, is continuously stirred, until mixed
Object gel is closed, then gel is homogenized by high shear mixing technology to emulsifiable paste shape, additional diluent is eventually adding and carries out
Diluted swelling obtains product.Patent CN 105980448 A, CN 105829405 A, CN 103619915 B, CN
101686901 A etc. also prepare organosilicon elastic gel using similar method.But the technique has some disadvantages: nascent gel
Preparation process system is in viscoelastic state, is not easy to be dispersed with stirring, reaction unit is not easily cleaned；Nascent gel is crushed through mechanical shearing
Afterwards, the elastomer powder particle size obtained is inhomogenous, and product sophistication is uneven.
106633076 A of patent CN refers to spray solidification technology and prepares organosilicon elastic gel, but there are bright for the technique
Aobvious disadvantage: equipment requirement is more complex, and spray solidification room needs periodic cleaning, and otherwise elastomer powder can cause to block up to pipeline
Plug.
Summary of the invention
Present invention aims at provide a kind of preparation method of organosilicone elastic gel for prior art deficiency, produce
Product can mutually be mixed in a shear condition with arbitrary proportion with the oil in formula, low for equipment requirements, easy to operate, production cost
It is low.
In order to solve the above-mentioned technical problem, technical scheme is as follows:
A kind of preparation method of organosilicone elastic gel, including following preparation step: by organic solvent, containing hydrogen silicone oil, extremely
The polysiloxanes of few two vinyl or both ends are that the alkadienes of unsaturated double-bond is added in reactor, after being uniformly mixed
Catalyst is added, is warming up to 50~90 DEG C of progress precipitation polymerizations and reacts 2~9h；Be cooled to after the reaction was completed 40 DEG C hereinafter, filtering,
Obtained solid powder obtains elastomer silicone powder through drying, then carries out elastomer silicone powder with diluent dilute
Swelling is released, and stabilizer is added, at 70~90 DEG C, it is solidifying to obtain the organosilicone elastic by 1~2h of stirring under the conditions of 30~90rpm
Glue；The organic solvent refers to the volatile organic solvent that can dissolve reaction raw materials but insoluble polymeric reaction product.
Preferred scheme, the containing hydrogen silicone oil refer to hydrogeneous mass fraction be 0.05%~0.5%, viscosity be 5~
The containing hydrogen silicone oil of 50mpa.s.
Preferred scheme, the polysiloxanes that the intramolecular contains at least two vinyl refer to that vinyl mass fraction is
The dimethyl silicone polymer of 0.1%~10% ethenyl blocking；The both ends are that the alkadienes of unsaturated double-bond includes 1,3-
Butadiene, 1,4- pentadiene, 1,5- hexadiene, 1,6- heptadiene, 1,7- octadiene or 1,9- decadinene.
Preferred scheme, the catalyst refer to Pt or Pd catalyst or its complex compound.
Preferred scheme, the stabilizer refer to iron oxide yellow.
Preferred scheme, the organic solvent refer to isopropanol or normal propyl alcohol.
Preferred scheme, the diluent includes cyclosiloxane or viscosity is the polydimethylsiloxanes of 2~20mpa.s
Alkane.
A kind of organosilicone elastic gel is prepared using the method as described in any of the above item.
Compared with prior art, the invention has the following beneficial effects:
(1) present invention prepares elastomer silicone powder by precipitation polymerization process using specific organic solvent, then uses
Elastomer powder swelling dilution is obtained uniform organosilicone elastic gel by diluent.Gained organosilicone elastic gel skin sense is salubrious
Non-greasy, dumb light sense are good, and product can mutually be mixed in a shear condition with arbitrary proportion with the oil in formula.
(2) present invention prepares elastomer silicone powder by precipitation polymerization process using specific organic solvent, compares
Existing directly to react in diluent, polymeric reaction product is directly precipitated in organic solvent, and gained elastomer powder partial size is big
Small uniform, product sophistication is uniform.
(3) present invention prepares elastomer silicone powder, gained by precipitation polymerization process using specific organic solvent
Elastomer silicone powder compares existing spray solidification through simple filtering, drying, low for equipment requirements, easy to operate,
Production cost is low.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment one
A kind of preparation method of organosilicone elastic gel, including following preparation step: (1) by 535.23g normal propyl alcohol,
Containing hydrogen silicone oil that 200.00g hydrogen content is 0.43%, 29.24g Isosorbide-5-Nitrae-pentadiene are added in 1000ml three-necked flask, and unlatching is stirred
It mixes, after mixing, 0.38g Pt catalyst is added dropwise to three-necked flask under agitation, catalyst amount 500ppm,
Heating is started simultaneously at, then under agitation in 70 DEG C of reactions 3h, revolving speed 80rpm.
(2) after having reacted, stop heating, after reactant is cooled to 40 DEG C or less, through solid powder is obtained by filtration.
(3) by obtained solid powder in 120 DEG C, vacuum degree: dry 3h under -0.95MPa, stirring condition is obtained organic
Silicone elastomer powder.
(4) three-necked flask, In is added for dimethyl silicone polymer, the 400g iron oxide yellow of 10mpa.s in 535.23g viscosity
90 DEG C, under the conditions of 80rpm, three-necked flask is added in elastomer silicone powder obtained by step (3), stirring 2h is swollen, most
After obtain uniform translucent organosilicone elastic gel.
Embodiment two
A kind of preparation method of organosilicone elastic gel, including following preparation step: (1) by 888.16g normal propyl alcohol,
Containing hydrogen silicone oil, 22.04g 1 of the 200.00g hydrogen content for 0.2%, 7- octadiene are added in 1000ml three-necked flask, and unlatching is stirred
It mixes, after mixing, 0.67gPt catalyst is added dropwise to three-necked flask under agitation, catalyst amount 600ppm, together
When start to warm up, then under agitation in 90 DEG C of reactions 8h, revolving speed 120rpm.
(2) after having reacted, stop heating, after reactant is cooled to 40 DEG C or less, through solid powder is obtained by filtration.
(3) by obtained solid powder in 140 DEG C, vacuum degree: dry 2h under -0.95MPa, stirring condition is obtained organic
Silicone elastomer powder.
(4) three-necked flask, In is added for dimethyl silicone polymer, the 250g iron oxide yellow of 5mpa.s in 888.16g viscosity
80 DEG C, under the conditions of 70rpm, three-necked flask is added in elastomer silicone powder obtained by step (3), stirring 2h is swollen, most
After obtain uniform translucent organosilicone elastic gel.
Embodiment three
A kind of preparation method of organosilicone elastic gel, including following preparation step: (1) by 840g isopropanol, 200.00g
The poly dimethyl silicon for the ethenyl blocking that containing hydrogen silicone oil that hydrogen content is 0.06%, 360.00g vinyl mass fraction are 0.9%
Oxygen alkane is added in 1000ml three-necked flask, opens stirring, and after mixing, 0.16g Pd catalyst is added dropwise under agitation
To three-necked flask, catalyst amount 120ppm starts simultaneously at heating, then under agitation in 90 DEG C of reaction 8h, revolving speed
For 90rpm.
(2) after having reacted, stop heating, after reactant is cooled to 40 DEG C or less, through solid powder is obtained by filtration.
(3) by obtained solid powder in 110 DEG C, vacuum degree: dry 2h under -0.95MPa, stirring condition is obtained organic
Silicone elastomer powder.
(4) three-necked flask, at 70 DEG C, 80rpm condition is added in 840g decamethylcyclopentaandoxane, 300g iron oxide yellow
Under, three-necked flask is added in elastomer silicone powder obtained by step (3), stirring 3h is swollen, and is finally obtained uniformly semi-transparent
Bright shape organosilicone elastic gel.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, In
Under the premise of not departing from present inventive concept, architectural form cans be flexible and changeable, can be with derivative series product.It only makes several
Simple deduction or replace all shall be regarded as belonging to present invention scope of patent protection determined by the appended claims.Though
So the present invention is disclosed as above with preferred embodiment, and however, it is not to limit the invention, anyone skilled in the art, not
It is detached from the spirit and scope of the present invention, when can make a little modification and perfect, therefore protection scope of the present invention is when with right
Subject to claim is defined.
Claims (8)
1. a kind of preparation method of organosilicone elastic gel, which is characterized in that including following preparation step: by organic solvent, containing
Hydrogen silicone oil, the polysiloxanes of at least two vinyl or both ends are that the alkadienes of unsaturated double-bond is added in reactor, are stirred
Catalyst is added after mixing, is warming up to 50~90 DEG C of progress precipitation polymerizations and reacts 2~9h；It is cooled to 40 DEG C after the reaction was completed
Hereinafter, filtering, obtained solid powder obtains elastomer silicone powder through drying, then by elastomer silicone powder with dilute
It releases agent and is diluted swelling, and stabilizer is added, at 70~90 DEG C, 1~2h of stirring is obtained described organic under the conditions of 30~90rpm
Silicon elastic gel；The organic solvent refers to that the volatile that can dissolve reaction raw materials but insoluble polymeric reaction product is organic
Solvent.
2. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: the Silicon Containing Hydrogen
Oil refers to the containing hydrogen silicone oil that hydrogeneous mass fraction is 0.05%~0.5%, viscosity is 5~50mpa.s.
3. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: the molecule includes
There is the polysiloxanes of at least two vinyl to refer to that vinyl mass fraction is the poly- diformazan of 0.1%~10% ethenyl blocking
Radical siloxane；The both ends are that the alkadienes of unsaturated double-bond includes 1,3- butadiene, 1,4- pentadiene, 1,5- hexadiene, 1,
6- heptadiene, 1,7- octadiene or 1,9- decadinene.
4. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: the catalyst
Refer to Pt or Pd catalyst or its complex compound.
5. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: the stabilizer
Refer to iron oxide yellow.
6. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: described is organic molten
Agent refers to isopropanol or normal propyl alcohol.
7. a kind of preparation method of organosilicone elastic gel according to claim 1, it is characterised in that: the diluent
The dimethyl silicone polymer for being 2~20mpa.s including cyclosiloxane or viscosity.
8. a kind of organosilicone elastic gel, it is characterised in that: described in any item methods are prepared according to claim 1~8.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214487A (en) * | 2021-04-23 | 2021-08-06 | 广东赛安特新材料有限公司 | Organic silicon elastomer and synthesis method and application thereof |
| CN113456506A (en) * | 2021-06-23 | 2021-10-01 | 长兴电子（苏州）有限公司 | Organic silicon gel composition and preparation method and application thereof |
| CN115926464A (en) * | 2022-11-15 | 2023-04-07 | 清远高能结加改性材料科技有限公司 | Preparation method of silicon rubber reinforced particles and reinforced rubber powder |
-
2018
- 2018-05-02 CN CN201810410157.XA patent/CN110437617A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214487A (en) * | 2021-04-23 | 2021-08-06 | 广东赛安特新材料有限公司 | Organic silicon elastomer and synthesis method and application thereof |
| CN113456506A (en) * | 2021-06-23 | 2021-10-01 | 长兴电子（苏州）有限公司 | Organic silicon gel composition and preparation method and application thereof |
| CN113456506B (en) * | 2021-06-23 | 2024-07-30 | 长兴电子（苏州）有限公司 | Organosilicon gel composition and preparation method and application thereof |
| CN115926464A (en) * | 2022-11-15 | 2023-04-07 | 清远高能结加改性材料科技有限公司 | Preparation method of silicon rubber reinforced particles and reinforced rubber powder |
| CN115926464B (en) * | 2022-11-15 | 2023-09-26 | 清远高能结加改性材料科技有限公司 | Preparation method of silicon rubber reinforced particles and reinforced rubber powder |
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