CN107868470A - A kind of ageing-resistant liquid silastic and preparation method thereof - Google Patents
A kind of ageing-resistant liquid silastic and preparation method thereof Download PDFInfo
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- CN107868470A CN107868470A CN201611030645.5A CN201611030645A CN107868470A CN 107868470 A CN107868470 A CN 107868470A CN 201611030645 A CN201611030645 A CN 201611030645A CN 107868470 A CN107868470 A CN 107868470A
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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
- 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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to silastic material technical field, is related to a kind of ageing-resistant liquid silastic and preparation method thereof.The present invention is prepared by the raw material of following parts by weight：Prestox cyclosiloxane（Purity >=97%）80 100 parts, tetramethyl tetravinyl cyclosiloxane（Purity >=95%）13 parts, tetraphenyl tetramethyl-ring siloxanes（Purity >=98%）0.1 0.3 parts of 15 25 parts, 10 20 parts of reinforcing agent and ionic catalyst.The advantages that present invention is high with intensity, elastic good, preferable heat endurance, and ageing-resistant performance is strong, preparation manipulation is simple.
Description
Technical field
The invention belongs to silastic material technical field, is related to a kind of ageing-resistant liquid silastic and preparation method thereof.
Background technology
With the fast development of society, organosilicon material field makes much progress, synthetically prepared for different field
Organosilicon material with specified chemical, physical property is had the liquid of specific function performance by social favor extensively, synthesis
Body silicon rubber turns into the study hotspot of silicone rubber art.Liquid silastic is the complex compound based on polysiloxanes, room temperature bar
Reaction is crosslinked under part with air vapor, or is acted under heating condition with filler, auxiliary agent, additive in metallic platinum catalyst
Lower generation vulcanization crosslinking reaction.Liquid silastic has a good heat conductivity, reduced TG inversion temperature, excellent ageing-resistant
Performance, it is widely used in the fields such as aircraft equipment, electronic equipment, medical device, machine-building, articles for daily use.
With the development of functional liquid silicon rubber, the liquid silastic performance prepared to complex compound based on polysiloxanes
It is required that the chemical property such as more and more higher, liquid silastic macroscopic property, heat endurance, caking property and hardness is increasingly by society
It can pay close attention to, but still suffer from that heat resisting temperature is low, thermodynamic property is unstable, polymer mechanical strength is not high, is easy to the system of aging etc. one
Row problem, wherein heat resistance difference are one of its major influence factors.Therefore, a kind of good liquid silicon rubber of ageing-resistant performance is developed
Glue is very important.
The content of the invention
The problem of existing for prior art, it is an object of the invention to provide a kind of ageing-resistant liquid silastic and its
Preparation method.The ageing-resistant liquid silastic of the present invention has intensity height, elastic good, preferable heat endurance, ageing-resistant performance
The advantages that strong；Preparation method of the present invention is simple to operate.
In order to solve the above technical problems, the technical solution adopted by the present invention：
A kind of ageing-resistant liquid silastic, is prepared by the raw material of following parts by weight：Prestox cyclosiloxane（Purity >=
97%）80-100 parts, tetramethyl tetravinyl cyclosiloxane（Purity >=95%）1-3 parts, tetraphenyl tetramethyl-ring siloxanes（Purity
≥98%）15-25 parts, reinforcing agent 10-20 parts and ionic catalyst 0.1-0.3 parts.
A preferred embodiment of the present invention, it is prepared by the raw material of following parts by weight：Prestox cyclosiloxane（Purity
≥97%）95 parts, tetramethyl tetravinyl cyclosiloxane（Purity >=95%）2 parts, tetraphenyl tetramethyl-ring siloxanes（Purity >=
98%）0.2 part of 18 parts, 15 parts of reinforcing agent and ionic catalyst.
The ionic catalyst is alkaline hydrated oxide.
The ionic catalyst is in sodium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, TMAH
One kind.
The reinforcing agent is N- methyl polysilicon azane
A kind of preparation method of ageing-resistant liquid silastic, step are as follows：
（1）Prestox cyclosiloxane, tetramethyl tetravinyl cyclosiloxane, tetraphenyl tetramethyl-ring silica are weighed in parts by weight
Alkane and reinforcing agent are added in reactor, and temperature is 50-70 DEG C, reaction time 1-3h, and alkali ion catalyst is added after dehydration, are risen
Temperature is warming up to 150-160 DEG C, reaction time 1-2h, into colloidal state again to 90-95 DEG C, vacuum reaction 1-2h；
（2）By step（1）Colloid react 0.5-1.2h at 160-190 DEG C, naturally cool to normal temperature, get product.
Beneficial effects of the present invention：The present invention has preferable thermal stability, preferable ageing properties.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
Respectively by each component specified in table 1 below, prestox cyclosiloxane, tetramethyl tetravinyl cyclosiloxane, four are weighed
Phenyl tetramethyl-ring siloxanes and reinforcing agent are added in reactor, and temperature is 50-70 DEG C, reaction time 1-3h, is added after dehydration
Alkali ion catalyst, 90-95 DEG C, vacuum reaction 1-2h is warming up to, is warming up to 150-160 DEG C, reaction time 1-2h again, into
Colloidal state；By step（1）Colloid react 0.5-1.2h at 160-190 DEG C, naturally cool to normal temperature, get product.It is right
It carries out physical and mechanical property indexs inspection.Test result is listed in table 1.
Embodiment 2
The method that embodiment 1 is repeated by each component content specified in table 1 below, test result is listed in table 1.
Embodiment 3
The method that embodiment 1 is repeated by each component content specified in table 1 below, test result is listed in table 1.
Embodiment 4
The method that embodiment 1 is repeated by each component content specified in table 1 below, test result is listed in table 1.
Embodiment 5
The method that embodiment 1 is repeated by each component content specified in table 1 below, test result is listed in table 1.
The embodiment 1-3 of table 1 each component table.
| Numbering/project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Prestox cyclosiloxane（Purity >=97%） | 85 parts | 88 parts | 95 parts | 98 parts | 100 parts |
| Tetramethyl tetravinyl cyclosiloxane（Purity >=95%） | 2 parts | 2 parts | 2 parts | 2 parts | 2 parts |
| Tetraphenyl tetramethyl-ring siloxanes（Purity >=98%） | 16 parts | 17 parts | 18 parts | 20 parts | 23 parts |
| N- methyl polysilicon azane | 12 parts | 14 parts | 15 parts | 17 parts | 18 parts |
| Sodium hydroxide | 0.2 part | 0 part | 0 part | 0 part | 0 part |
| Potassium hydroxide | 0 part | 0.2 part | 0 part | 0 part | 0 part |
| Calcium hydroxide | 0 part | 0 part | 0.2 part | 0 part | 0 part |
| Barium hydroxide | 0 part | 0 part | 0 part | 0.2 part | 0 part |
| TMAH | 0 part | 0 part | 0 part | 0 part | 0.2 part |
First, performance detection
Hardness（Shao Er A）Tested according to GB/T 531-1999；Tensile strength and elongation rate of tensile failure are according to GB/T 528-
1998 are tested；Thermogravimetic analysis (TGA) is tested according to ISO11358-1997.
1st, carry out performance detection to ageing-resistant liquid silastic prepared by embodiment 1-3, and with national standard and other places of production
Product compares, comparing result such as table 2.
Ageing-resistant liquid silastic rationality index prepared by the embodiment 1-3 of table 2 contrasts with national standard and other place of production products
Table.
| Project/numbering | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Jilin Chemical institute | Foreign standard |
| Tensile strength/MPa | 7.5 | 8.3 | 8.4 | 8.3 | 8.4 | 6.2 | ≥5 |
| Elongation rate of tensile failure/% | 411 | 426 | 415 | 426 | 412 | 336 | ≥100 |
| Hardness（Shao Er A） | 67 | 65 | 64 | 64 | 64 | 56 | 75-85 |
| Elongation rate of tensile failure change/%（300 DEG C × 48h agings） | -28 | -26 | -28 | -25 | -28 | 29 | - 45 to 25 |
| Firmness change rate, % | -4.33 | -3.69 | -3.75 | -3.65 | -3.86 | -10.66 | |
| Tensile strength rate of change, % | -13.5 | -13.7 | -13.5 | -13.6 | -13.5 | -23.56 |
As shown in Table 2, the firmness change rate of the invention after 300 DEG C × 48h agings is drawn between -3.7% and -4.4%
Stretch change rate of strength between -13 and -14, less than Jilin Chemical institute firmness change rate -10.66% and tensile strength rate of change -
23.56%, illustrate that the high temperature ageing performance of the high-temperature resistant rubber of the present invention is good.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical scheme described by inventive embodiments, it will be understood by those within the art that, still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (6)
- A kind of 1. ageing-resistant liquid silastic, it is characterised in that：It is prepared by the raw material of following parts by weight：Prestox ring Siloxanes（Purity >=97%）80-100 parts, tetramethyl tetravinyl cyclosiloxane（Purity >=95%）1-3 parts, tetraphenyl tetramethyl Cyclosiloxane（Purity >=98%）15-25 parts, reinforcing agent 10-20 parts and ionic catalyst 0.1-0.3 parts.
- 2. ageing-resistant liquid silastic according to claim 1, it is characterised in that：By the raw material system of following parts by weight It is standby to form：Prestox cyclosiloxane（Purity >=97%）95 parts, tetramethyl tetravinyl cyclosiloxane（Purity >=95%）2 parts, four Phenyl tetramethyl-ring siloxanes（Purity >=98%）0.2 part of 18 parts, 15 parts of reinforcing agent and ionic catalyst.
- 3. ageing-resistant liquid silastic according to claim 1, it is characterised in that：The ionic catalyst is alkaline hydrogen Oxide.
- 4. ageing-resistant liquid silastic according to claim 3, it is characterised in that：The alkaline hydrated oxide is hydrogen-oxygen Change one kind in sodium, potassium hydroxide, calcium hydroxide, barium hydroxide, TMAH.
- 5. ageing-resistant liquid silastic according to claim 1, it is characterised in that：The reinforcing agent is N- methyl polysilicons Azane.
- A kind of 6. preparation method of any ageing-resistant liquid silastic according to claim 1-5, it is characterised in that：Step It is rapid as follows：（1）Prestox cyclosiloxane, tetramethyl tetravinyl cyclosiloxane, tetraphenyl tetramethyl-ring silica are weighed in parts by weight Alkane and reinforcing agent are added in reactor, and temperature is 50-70 DEG C, reaction time 1-3h, and alkali ion catalyst is added after dehydration, are risen Temperature is warming up to 150-160 DEG C, reaction time 1-2h, into colloidal state again to 90-95 DEG C, vacuum reaction 1-2h；（2）By step（1）Colloid react 0.5-1.2h at 160-190 DEG C, naturally cool to normal temperature, get product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611030645.5A CN107868470A (en) | 2016-11-22 | 2016-11-22 | A kind of ageing-resistant liquid silastic and preparation method thereof |
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|---|---|---|---|
| CN201611030645.5A CN107868470A (en) | 2016-11-22 | 2016-11-22 | A kind of ageing-resistant liquid silastic and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60163887A (en) * | 1984-02-07 | 1985-08-26 | Toyo Soda Mfg Co Ltd | Cyclosiloxane derivative |
| CN102850551A (en) * | 2012-09-25 | 2013-01-02 | 中国工程物理研究院化工材料研究所 | Method for synthesizing methyl monophenyl vinyl high temperature heat vulcanized silicone rubber |
| CN104761912A (en) * | 2015-04-07 | 2015-07-08 | 山东大学 | Damping silicon rubber with relatively small temperature effect and preparation method thereof |
-
2016
- 2016-11-22 CN CN201611030645.5A patent/CN107868470A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60163887A (en) * | 1984-02-07 | 1985-08-26 | Toyo Soda Mfg Co Ltd | Cyclosiloxane derivative |
| CN102850551A (en) * | 2012-09-25 | 2013-01-02 | 中国工程物理研究院化工材料研究所 | Method for synthesizing methyl monophenyl vinyl high temperature heat vulcanized silicone rubber |
| CN104761912A (en) * | 2015-04-07 | 2015-07-08 | 山东大学 | Damping silicon rubber with relatively small temperature effect and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周重光等: ""填充聚硅氮烷提高室温硫化型硅橡胶的性能"", 《合成橡胶工业》 * |
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