CN113583447A - Organic silicon reinforcing additive, preparation method thereof and organic silicon material - Google Patents
Organic silicon reinforcing additive, preparation method thereof and organic silicon material Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 40
- 239000010703 silicon Substances 0.000 title claims abstract description 40
- 239000002210 silicon-based material Substances 0.000 title abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000012758 reinforcing additive Substances 0.000 title description 10
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 34
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 75
- 229920001296 polysiloxane Polymers 0.000 claims description 20
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 230000035484 reaction time Effects 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 10
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 229910052723 transition metal Inorganic materials 0.000 claims description 7
- 150000003624 transition metals Chemical group 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 6
- 125000005375 organosiloxane group Chemical group 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-M hydrosulfide Chemical compound [SH-] RWSOTUBLDIXVET-UHFFFAOYSA-M 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 claims 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 2
- 239000011574 phosphorus Substances 0.000 abstract description 2
- 229920002379 silicone rubber Polymers 0.000 description 13
- 229920002050 silicone resin Polymers 0.000 description 9
- 238000004898 kneading Methods 0.000 description 6
- 239000004945 silicone rubber Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 229920002545 silicone oil Polymers 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- -1 titanate compound Chemical class 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- MOSXLDGILGBOSZ-UHFFFAOYSA-N ethenyl-methyl-phenylsilicon Chemical compound C=C[Si](C)C1=CC=CC=C1 MOSXLDGILGBOSZ-UHFFFAOYSA-N 0.000 description 1
- 229920005560 fluorosilicone rubber Polymers 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229920002529 medical grade silicone Polymers 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
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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
-
- 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
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K3/38—Boron-containing compounds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/0091—Complexes with metal-heteroatom-bonds
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides an organic silicon reinforcing aid, a preparation method thereof and an organic silicon material, wherein the organic silicon reinforcing aid comprises the following raw materials in parts by weight: 100-150 parts of an organic silicon base material; 1-50 parts of a catalyst; 1-50 parts of a crosslinking agent; 3-200 parts of a graft; the graft is one or the combination of two of phosphorus silicate and borosilicate, and the organic silicon material prepared by the product has good tearing resistance and wear resistance.
Description
Technical Field
The invention relates to the field of organic polymer silicon materials, in particular to an organic silicon enhancement additive, a preparation method thereof and an organic silicon material.
Background
The silicon rubber product has better high and low temperature resistance, mechanical property, biocompatibility and the like, but the products have poorer tearing resistance and wear resistance and stress resistance. The method for seeking the silicone rubber product to be more wear-resistant and tear-resistant becomes the key point of current research and development, and the organic silicon reinforcing additive obtained by the grafting modification method has excellent reworkability, good fluidity and dispersibility and low production cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides an organic silicon reinforcing aid, a preparation method thereof and an organic silicon material, and can solve the problem of poor wear resistance of the organic silicon material on the market at present.
In order to achieve the above objects and other objects, the present invention includes the following technical solutions: the invention provides an organic silicon reinforcing aid which comprises the following raw materials in parts by weight: 100-150 parts of an organic silicon base material; 1-50 parts of a catalyst; 1-50 parts of a crosslinking agent; 3-200 parts of a graft; the graft is one or two of phosphosilicate and borosilicate.
In one embodiment, the silicone substrate comprises a silicone resin and an organosiloxane in a weight ratio of 100: (1-50).
In one embodiment, the silicone resin is any one or combination of a plurality of silicone boron resin, M-D-Q resin, vinyl silicone resin and hydrogen-containing resin.
In one embodiment, the organosiloxane has the formula: [ R1R2SiO ] m [ R3R 4SiO ] n, wherein R1, R2, R3 and R4 are any one of hydrosulfide, methyl, ethyl, propyl, phenyl, vinyl, hydrogen atoms and hydroxyl, m and n are 0-10000, and m and n cannot be 0 at the same time.
In one embodiment, the cross-linking agent is a transition metal complex in a super-normal valence state, and the transition metal complex comprises any one or more of Ag, Pt and Pd.
In one embodiment, the catalyst is one or more of a titanate compound, dibutyltin dilaurate, dibutyltin diacetate, or a combination thereof.
In one embodiment, the grafting ratio of the organosilicon reinforcing auxiliary agent is 30-60%.
The invention also provides a preparation method of the organic silicon reinforcing additive, which comprises the following steps: the preparation method comprises the following steps: providing the silicone substrate and a graft; mixing the organic silicon substrate and the graft to obtain an organic silicon mixture; and reacting the organic silicon mixture with a catalyst and a crosslinking agent to obtain the organic silicon reinforcing aid.
In one embodiment, the reaction includes a gradient temperature reaction, the gradient temperature reaction is performed under a vacuum condition, and the gradient temperature reaction includes a first reaction, a second reaction, a third reaction, and a fourth reaction, which are performed sequentially.
In one embodiment, the reaction temperature of the first reaction is 120 ℃ to 160 ℃, the reaction time of the first reaction is 30 to 60 minutes, the reaction temperature of the second reaction is 170 ℃ to 175 ℃, the reaction time of the second reaction is 30 to 60 minutes, the reaction temperature of the third reaction is 175 ℃ to 180 ℃, the reaction time of the third reaction is 30 to 60 minutes, the reaction temperature of the fourth reaction is below 50 ℃, and the reaction time of the fourth reaction is 30 to 60 minutes.
In yet another aspect, the present invention also provides a silicone material comprising the silicone reinforcing aid as described above.
In one embodiment, the silicone material comprises a silicone tubing, shaped product.
In one embodiment, the silicone tube comprises any one of a medical tube, a peristaltic pump tube, a drug delivery tube, and a food delivery tube.
In one embodiment, the tear strength of the organosilicon material is greater than or equal to 40KN/m, and the abrasion resistance is greater than 900 ten thousand times.
The organic silicon reinforcing additive can effectively connect the rubber base material in the organic silicon material with other added raw material components, and the prepared organic silicon material has a more compact net structure through intermolecular attraction and a home position structure, so that the tearing performance and the wear resistance of the product are improved. The organic silicon reinforcing additive has excellent reworkability, good fluidity and dispersibility and low production cost. The product prepared by the invention can greatly improve the defects of organic silicon products and improve the tear resistance and wear resistance. The organosilicon reinforcing additive prepared by the invention can be widely applied to various products such as silica gel pipes, sheets, special-shaped materials and the like, and can be applied to a plurality of industries through adjustment.
The reinforcing additive prepared by the invention is different from the traditional reinforcing filler in use process and material performance selection, the reinforcing additive is obtained by synthetic grafting treatment and cross-linking grafting, and the super-normal transition metal Ag/Pt/Pd and phosphorus silicate or borosilicate are selected for grafting treatment, so that the reinforcing additive has excellent reinforcing performance, and the wear resistance of an organic silicon material product can be greatly improved by surface treatment.
Drawings
FIG. 1 shows a flow chart of the preparation method of the present invention.
Detailed Description
Referring to fig. 1, embodiments of the present invention are described below with specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention firstly provides an organic silicon reinforcing aid which comprises the following raw materials in parts by weight: 100-150 parts of an organic silicon base material; 1-50 parts of a catalyst; 1-50 parts of a crosslinking agent; 3-200 parts of a graft; the graft is one or two of phosphosilicate and borosilicate. Further, the graft may be borosilicate.
Further, the organic silicon reinforcing aid comprises the following raw materials in parts by weight: 100-120 parts of an organic silicon base material; 2-10 parts of a catalyst; 4-10 parts of a crosslinking agent; 30-150 parts of a graft.
The organic silicon substrate may include a silicon resin and an organic siloxane, and the weight ratio of the silicon resin to the organic siloxane may be 100: (1 to 50), further may be100: (5-20), further can be 100 (10-20), such as 100:10, 100:15, etc., the silicone resin is any one or combination of more of silicon boron resin, M-D-Q resin, vinyl silicone resin and hydrogen-containing resin. The organosiloxane may be of the general formula: [ R ]1R2SiO]m[R3R4SiO]n, wherein R1、R2、R3、R4Is one of hydrosulfide, methyl, ethyl, propyl, phenyl, vinyl, hydrogen atom and hydroxyl, m and n are 0-10000, and m and n can not be 0 at the same time, further m and n are 50-5000, and further m and n are 500-5000. The catalyst can be a transition metal complex in a super-normal valence state, and the transition metal complex can be any one or combination of Ag, Pt and Pd. The catalyst can be one or more of titanate compound, dibutyltin dilaurate and dibutyltin diacetate. The grafting ratio of the organosilicon reinforcing auxiliary agent can be 30-60%, and further, the grafting ratio can be 50-60%.
As shown in fig. 1, another aspect of the present invention also provides a method of preparing the silicone reinforcing adjuvant, which includes steps S1-S3:
-S1: providing the silicone substrate and a graft;
-S2: mixing the organic silicon substrate and the graft to obtain an organic silicon mixture;
-S3: and reacting the organic silicon mixture with a catalyst and a crosslinking agent to obtain the graft-modified organic silicon reinforcing agent.
In step S1, the silicone substrate and the graft may be placed in a high temperature kneader or reaction vessel for the next step.
In step S2, the mixing may be low-temperature mixing, the mixing may be a kneading process, and the temperature of the mixing may be 100 ℃. The mixing may form a liquid paste-like material.
In step S3, the reaction may include a gradient temperature reaction, where the gradient temperature reaction may be performed under vacuum, and the gradient temperature reaction may include a first reaction, a second reaction, a third reaction, and a fourth reaction, which are performed sequentially. The reaction temperature of the first reaction may be 120 to 160 ℃, for example, 120 ℃ or 150 ℃, the reaction time of the first reaction may be 30 to 60 minutes, for example, 45 minutes or 50 minutes, the degree of vacuum of the first reaction may be 0.7MPa or more, the reaction temperature of the second reaction may be 170 to 175 ℃, the reaction time of the second reaction may be 30 to 60 minutes, for example, 45 minutes or 50 minutes, the degree of vacuum of the second reaction may be 0.7MPa or more, the reaction temperature of the third reaction may be 175 to 180 ℃, the reaction time of the third reaction may be 30 to 60 minutes, for example, 40 minutes or 50 minutes, the degree of vacuum of the third reaction may be 0.7MPa or more, the reaction temperature of the fourth reaction may be 50 ℃ or less, for example, 40 ℃ or 30 ℃, the reaction time of the fourth reaction may be 30 to 60 minutes, for example, 45 minutes, 55 minutes, etc., the reinforcing aid after the gradient temperature reaction can gradually change from a liquid paste after mixing to a viscous paste material. The reinforcing aid obtained after the reaction can be cooled to obtain a finished reinforcing aid to be used. The grafting rate of the enhancement additive can be better controlled by controlling the temperature of the gradient temperature change reaction.
The organic silicon material can comprise the organic silicon reinforcing aid, and the specific gravity of the reinforcing aid can be 5-20% and further can be 5-10% based on 100% of the weight of the organic silicon material. In some embodiments, the organosilicon reinforcing assistant may be further subjected to a surface treatment before being mixed into the organosilicon material, the surface treatment agent may be one or a combination of more of a coupling agent 151, a coupling agent 171, hydrogen-containing silicone oil, silane, silazane, and hydroxyl-containing silicone oil, the surface treatment may improve the surface polarity and mechanical properties of the reinforcing assistant, and facilitate concentrated crosslinking of the organosilicon material, of course, the organosilicon material may also include organosilicon rubber, and may also include common assistants such as a forming assistant, a filler, and a crosslinking assistant, but is not limited thereto. In one embodiment, the silicone rubber comprises any one or more of intrinsic silicone rubber, methyl silicone rubber, vinyl silicone rubber, phenyl silicone rubber, silicon boron rubber and fluorosilicone rubber. Further, the organic silicon rubber comprises any one or more of methyl vinyl silicon rubber, dimethyl silicon rubber and methyl vinyl phenyl silicon rubber. In one embodiment, the filler is one or a combination of white carbon black and silica powder. In one embodiment, the forming aid is any one or combination of more of organic silicone oil, emulsified silicone oil and silicone oil paste mixture. The crosslinking assistant can be a platinum two-component crosslinking agent.
The tear resistance strength of the organosilicon material is more than or equal to 40KN/m, the wear resistance is more than 900 ten thousand times, the organosilicon material can be applied to products which are required to be extruded, molded and injected, and particularly has good application prospect in the aspect of medical polymer consumables. The application fields of the medical silicon rubber tube and the medical tube can comprise products such as a medical silicone tube, a medical tube, a peristaltic pump tube, a medicine flow guide tube and a food flow guide tube, and can also be applied to various tube materials and special-shaped material products which are contacted with people, medicines and food. But may of course also be applied in fields such as insulation protection, wire and cable connections, waterproof sealing, etc.
Note that "%" and "part(s)" shown herein mean "% by mass" and "part(s) by mass", respectively, unless otherwise specified.
Hereinafter, the present invention will be more specifically explained by referring to examples, which should not be construed as limiting. Appropriate modifications may be made within the scope consistent with the gist of the present invention, and all of them fall within the technical scope of the present invention.
Examples of the invention
Example 1
A preparation method of an organosilicon reinforcing auxiliary agent comprises the following steps:
(1) pre-mixing 100 parts of vinyl silicone resin and 50 parts of borosilicate in a high-temperature kneader or a reaction kettle at a low temperature, wherein the mixing temperature is less than or equal to 100 ℃;
(2) adding 2 parts of catalyst and 4 parts of cross-linking agent into reaction equipment, uniformly mixing, and kneading at normal temperature for 10-20 minutes to form a liquid paste material;
(3) mixing and reacting the formed liquid paste material, gradually heating, controlling the temperature at 150 ℃, kneading for 30-60 minutes, vacuumizing in the reaction process, and keeping the vacuum degree to be more than or equal to-0.7 MPa to form a viscous paste material;
(4) mixing and reacting the material which forms the thick paste, gradually heating, controlling the temperature at 170 ℃, kneading for 30-60 minutes, vacuumizing in the reaction process, and keeping the vacuum degree to be more than or equal to-0.7 MPa to form the material which forms the thick paste;
(5) mixing and reacting the material which forms the thick paste, gradually heating, controlling the temperature at 175 ℃, kneading for 30-60 minutes, vacuumizing in the reaction process, and keeping the vacuum degree to be more than or equal to-0.7 MPa to form a thick paste material;
(6) the material forming the viscous dough is mixed and reacted, and is gradually cooled, spontaneously combusted and cooled, the temperature is controlled below 50 ℃, and kneading treatment is carried out for 30-60 minutes to form the viscous dough-shaped material;
(7) and (4) removing the bulk material obtained by the reaction in the step (6) out of the reaction equipment, and cooling to obtain a reinforcing auxiliary agent sample 1, wherein the grafting rate of the sample 1 is 55%.
Example 2
The reinforcing aid of example 2 was prepared in a similar manner to example 1, except that the silicone base material was changed to a mixture of 100 parts of vinyl silicone resin and 10 parts of organosiloxane to give reinforcing aid sample 2, sample 2 having a grafting rate of 60%.
Example 3
The reinforcing aid of example 3 was prepared in a similar manner to example 1, except that the silicone base material was changed to a mixture of 100 parts of vinyl silicone resin and 100 parts of organosiloxane to give reinforcing aid sample 3, sample 3 having a grafting ratio of 50%.
Example 4
The reinforcing aid of example 4 was prepared in a manner similar to that of example 1, except that the graft was changed to phosphosilicate to give reinforcing aid sample 4, and the graft ratio of sample 4 was 52%.
Example 5
The reinforcing aid of example 5 was prepared in a similar manner to example 1, with the borosilicate in an amount of 180 parts by weight, giving reinforcing aid sample 5, sample 5 having a degree of grafting of 35%.
Evaluation of
Mixing the reinforcing auxiliary agent obtained from the samples 1-5 to form the organic silicon material, and evaluating the performance of the organic silicon material, wherein the formula of the organic silicon material is as follows: 100 parts of organic silicon rubber, 20 parts of organic siloxane, 30 parts of filler white carbon black, 3 parts of forming aid, 10 parts of reinforcing aid and 3 parts of crosslinking aid by mass, wherein the formula of a comparison sample is the same as that of the organic silicon material, the reinforcing aid is vinyl silicone resin without grafting reaction, and the evaluation results are shown in table 1.
TABLE 1 summary of performance indices for organosilicon materials
Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value. The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. An organosilicon reinforcing auxiliary agent, which is characterized in that: the organic silicon reinforcing aid comprises the following raw materials in parts by weight:
100-150 parts of an organic silicon base material;
1-50 parts of a catalyst;
1-50 parts of a crosslinking agent;
3-200 parts of a graft;
the graft is one or two of phosphosilicate and borosilicate.
2. The silicone reinforcing aid of claim 1, wherein: the organic silicon substrate comprises silicon resin and organic siloxane, wherein the weight ratio of the silicon resin to the organic siloxane is 100: (1-50).
3. The silicone reinforcing aid of claim 2, wherein: the silicon resin is any one or combination of a plurality of silicon boron resin, M-D-Q resin, vinyl silicon resin and hydrogen-containing resin.
4. The silicone reinforcing aid of claim 2, wherein: the organosiloxane has the general formula: [ R ]1R2SiO]m[R3 R4SiO]n, wherein R1、R2、R3、R4Is any one of hydrosulfide, methyl, ethyl, propyl, phenyl, vinyl, hydrogen atom and hydroxyl, and m and n are 0-10000, wherein m and n cannot be 0 at the same time.
5. The silicone reinforcing aid of claim 1, wherein: the cross-linking agent is a transition metal complex with a super-normal valence state, and the transition metal complex comprises any one or combination of Ag, Pt and Pd.
6. The silicone reinforcing aid of claim 1, wherein: the catalyst is one or a combination of a plurality of titanate compounds, dibutyltin dilaurate and dibutyltin diacetate.
7. A method of preparing the silicone reinforcing aid of any of claims 1 to 6, wherein: the method comprises the following steps:
providing the silicone substrate and a graft;
mixing the organic silicon substrate and the graft to obtain an organic silicon mixture;
and reacting the organic silicon mixture with a catalyst and a crosslinking agent to obtain the organic silicon reinforcing aid.
8. The method of claim 7, wherein: the reaction comprises a gradient temperature change reaction, wherein the gradient temperature change reaction is carried out under the condition of vacuumizing, and the gradient temperature change reaction comprises a first reaction, a second reaction, a third reaction and a fourth reaction which are sequentially carried out.
9. The method of claim 8, wherein: the reaction temperature of the first reaction is 120-160 ℃, the reaction time of the first reaction is 30-60 minutes, the reaction temperature of the second reaction is 170-175 ℃, the reaction time of the second reaction is 30-60 minutes, the reaction temperature of the third reaction is 175-180 ℃, the reaction time of the third reaction is 30-60 minutes, the reaction temperature of the fourth reaction is below 50 ℃, and the reaction time of the fourth reaction is 30-60 minutes.
10. An organosilicon material, characterized by: the organosilicon material comprises the organosilicon reinforcing auxiliary agent as set forth in any one of claims 1 to 6.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1356926A (en) * | 1999-03-05 | 2002-07-03 | 雷斯特克公司 | Surface modification of solid supports through thermal decomposition and functionalization of silanes |
| JP2005132855A (en) * | 2003-10-28 | 2005-05-26 | Sanyo Chem Ind Ltd | Grout material composition |
| CN105492501A (en) * | 2013-05-03 | 2016-04-13 | 拉姆兰特有限公司 | Crosslinked siloxanyl polymer compositions |
| CN109369977A (en) * | 2018-09-12 | 2019-02-22 | 南京亚通橡塑有限公司 | A kind of abrasive rubber material and preparation method thereof |
| US20190092993A1 (en) * | 2017-09-27 | 2019-03-28 | Momentive Performance Materials Inc. | Thermal interface composition comprising ionically modified siloxane |
-
2021
- 2021-08-18 CN CN202110946490.4A patent/CN113583447A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1356926A (en) * | 1999-03-05 | 2002-07-03 | 雷斯特克公司 | Surface modification of solid supports through thermal decomposition and functionalization of silanes |
| JP2005132855A (en) * | 2003-10-28 | 2005-05-26 | Sanyo Chem Ind Ltd | Grout material composition |
| CN105492501A (en) * | 2013-05-03 | 2016-04-13 | 拉姆兰特有限公司 | Crosslinked siloxanyl polymer compositions |
| US20190092993A1 (en) * | 2017-09-27 | 2019-03-28 | Momentive Performance Materials Inc. | Thermal interface composition comprising ionically modified siloxane |
| CN109369977A (en) * | 2018-09-12 | 2019-02-22 | 南京亚通橡塑有限公司 | A kind of abrasive rubber material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蓝敏杰等: "（含氟树脂接枝玻璃微珠(HGB)的制备与表征", 《表面技术》 * |
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