CN114591536B - Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather - Google Patents
Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather Download PDFInfo
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- CN114591536B CN114591536B CN202210339104.XA CN202210339104A CN114591536B CN 114591536 B CN114591536 B CN 114591536B CN 202210339104 A CN202210339104 A CN 202210339104A CN 114591536 B CN114591536 B CN 114591536B
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- silicone rubber
- retarder
- synthetic leather
- alcohol
- methylbutinol
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 118
- 239000002649 leather substitute Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 238000005265 energy consumption Methods 0.000 title abstract description 8
- 239000004945 silicone rubber Substances 0.000 claims abstract description 104
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000003054 catalyst Substances 0.000 claims abstract description 43
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 42
- 239000002775 capsule Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- -1 alkali metal salt Chemical class 0.000 claims abstract description 23
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 14
- ACIAHEMYLLBZOI-ZZXKWVIFSA-N Unsaturated alcohol Chemical compound CC\C(CO)=C/C ACIAHEMYLLBZOI-ZZXKWVIFSA-N 0.000 claims abstract description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 7
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 238000010534 nucleophilic substitution reaction Methods 0.000 claims abstract description 7
- 239000010410 layer Substances 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 36
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 24
- 235000019441 ethanol Nutrition 0.000 claims description 21
- 229920002545 silicone oil Polymers 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 19
- 239000002585 base Substances 0.000 claims description 17
- 239000004744 fabric Substances 0.000 claims description 17
- VBPSVYDSYVJIPX-UHFFFAOYSA-N pent-2-en-2-ol Chemical class CCC=C(C)O VBPSVYDSYVJIPX-UHFFFAOYSA-N 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 15
- 235000021355 Stearic acid Nutrition 0.000 claims description 14
- 239000011247 coating layer Substances 0.000 claims description 14
- 239000011162 core material Substances 0.000 claims description 14
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 14
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 14
- 239000008117 stearic acid Substances 0.000 claims description 14
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical group O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 239000000440 bentonite Substances 0.000 claims description 12
- 229910000278 bentonite Inorganic materials 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910000039 hydrogen halide Inorganic materials 0.000 claims description 11
- 239000012433 hydrogen halide Substances 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 238000013268 sustained release Methods 0.000 claims description 11
- 239000012730 sustained-release form Substances 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 10
- 239000000049 pigment Substances 0.000 claims description 10
- 229920000058 polyacrylate Polymers 0.000 claims description 10
- 229920002050 silicone resin Polymers 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
- 238000000034 method Methods 0.000 claims description 8
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 7
- 239000001639 calcium acetate Substances 0.000 claims description 7
- 229960005147 calcium acetate Drugs 0.000 claims description 7
- 235000011092 calcium acetate Nutrition 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000002667 nucleating agent Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 150000002978 peroxides Chemical class 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- HNVRRHSXBLFLIG-UHFFFAOYSA-N 3-hydroxy-3-methylbut-1-ene Chemical compound CC(C)(O)C=C HNVRRHSXBLFLIG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 125000005843 halogen group Chemical group 0.000 claims description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
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- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 abstract description 38
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 14
- 238000003795 desorption Methods 0.000 abstract description 11
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 125000000304 alkynyl group Chemical group 0.000 abstract description 4
- 125000003342 alkenyl group Chemical group 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 230000000536 complexating effect Effects 0.000 abstract description 3
- 238000010092 rubber production Methods 0.000 abstract description 2
- INTUQSXPAMDVSB-UHFFFAOYSA-N 1-chloropent-2-en-2-ol Chemical compound CCC=C(O)CCl INTUQSXPAMDVSB-UHFFFAOYSA-N 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 19
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000003111 delayed effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
- 239000008116 calcium stearate Substances 0.000 description 2
- 235000013539 calcium stearate Nutrition 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000000979 retarding effect Effects 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- JBTWBPVTDXPHFG-UHFFFAOYSA-L disodium;2-hydroxyacetate Chemical compound [Na+].[Na+].OCC([O-])=O.OCC([O-])=O JBTWBPVTDXPHFG-UHFFFAOYSA-L 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Substances OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 238000007342 radical addition reaction Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
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- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
-
- 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
- C08K3/30—Sulfur-, selenium- or tellurium-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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0059—Organic ingredients with special effects, e.g. oil- or water-repellent, antimicrobial, flame-resistant, magnetic, bactericidal, odour-influencing agents; perfumes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/28—Artificial leather
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Textile Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application relates to the technical field of silicone rubber production, and particularly discloses a silicone rubber retarder, silicone rubber synthetic leather containing the retarder and a low-energy-consumption manufacturing process of the silicone rubber synthetic leather. The components of the silicone rubber retarder comprise an unsaturated alcohol composite preparation and a desorption agent slow-release capsule, wherein the unsaturated alcohol composite preparation is formed by mixing methylbutylenol and a methylbutylenol derivative, and the methylbutylenol derivative is a product of nucleophilic substitution reaction of alkali metal salt with carboxyl alcohol and chloromethylbutenol. The application utilizes the complexing action of the platinum catalyst on groups such as alkynyl, alkenyl, hydroxyl, carboxyl and the like to limit the catalytic activity of the platinum catalyst, thereby being beneficial to delaying the time of the vulcanization reaction of the silicone rubber. Meanwhile, the retarder can realize desorption without increasing the temperature and prolonging the heating time, thereby reducing the energy consumption of the vulcanization process, being beneficial to reducing the use of petrochemical fuel and realizing the effect of low carbon and environmental protection.
Description
Technical Field
The application relates to the technical field of silicone rubber production, in particular to a silicone rubber retarder, silicone rubber synthetic leather containing the retarder and a low-energy-consumption manufacturing process of the silicone rubber synthetic leather.
Background
Silicone rubber is an excellent synthetic rubber, and is one of the research hot spots in the rubber field for decades. The addition type liquid silicone rubber is the novel silicone rubber developed under the background, and has the advantages of aging resistance, no toxicity, no smell, good insulating property and the like, and has the advantages of small shrinkage rate in the vulcanization process, simple and convenient deep vulcanization operation and the like compared with other synthetic rubbers. In the synthesis of addition type liquid silicone rubber, adsorption catalysis is usually performed by using a platinum catalyst, and since the catalytic activity of the platinum catalyst is extremely high, it is generally necessary to add a retarder to the raw material of the silicone rubber to appropriately reduce the catalytic activity of the platinum catalyst, thereby allowing time for vulcanization processing.
In the related art, a silicone rubber retarder is prepared from methylbutynol as a main component. The methyl butynol is unsaturated alcohol, alkynyl and hydroxyl in the methyl butynol can be adsorbed with platinum catalyst, iron and other metals, and after the methyl butynol is added into the silicon rubber raw material, the methyl butynol is adsorbed on the surface of the platinum catalyst, and a complex adsorption layer is formed on the surface of the platinum catalyst, so that the adsorption between the platinum catalyst and the silicon rubber monomer is blocked, and the vulcanization reaction is delayed.
In view of the above-mentioned related art, the inventors believe that, although methylbutynol in the related art has a certain effect of delaying the occurrence of the vulcanization reaction, methylbutynol is easily volatilized at the initial stage of vulcanization, and therefore the platinum catalyst is difficult to retain the adsorption of methylbutynol for a long period of time, resulting in poor effect of the occurrence of the vulcanization reaction after delay of methylbutynol.
Disclosure of Invention
In the related art, the platinum catalyst is difficult to maintain for a long time to adsorb the methylbutynol, so that the effect of the methylbutynol on the delayed vulcanization reaction is poor, and in order to overcome the defect, the application provides a silicone rubber retarder, silicone rubber synthetic leather containing the retarder and a low-energy-consumption manufacturing process of the silicone rubber synthetic leather.
In a first aspect, the present application provides a silicone rubber retarder, which adopts the following technical scheme:
The silicone rubber retarder comprises the following components in parts by weight: 8-12 parts of an unsaturated alcohol composite preparation and 4-6 parts of a desorbent slow release capsule, wherein the unsaturated alcohol composite preparation is formed by mixing methylbutinol and a methylbutinol derivative, the methylbutinol derivative is obtained by nucleophilic substitution reaction of halogen atoms in an addition product of methylbutinol and hydrogen halide and an organic chain segment donor, the components of the organic chain segment donor comprise alkali metal alkoxide, and alcohol corresponding to the alkali metal alkoxide is monohydric alcohol with carboxyl; the components of the desorbent slow release capsule comprise persulfate.
According to the technical scheme, methyl butynol is modified, a monohalogenated compound of methyl butynol is obtained through an addition reaction, nucleophilic substitution reaction is carried out between halogen atoms and alkali metal alkoxide, and alkali metal halide is removed to obtain the methyl butynol derivative. Alkenyl groups in the methylbutyl alcohol derivatives are similar to alkynyl groups and can form complexes with platinum catalysts. Meanwhile, since carboxyl is also introduced into the methylbutinol derivative by nucleophilic substitution reaction, and the newly introduced carboxyl and the hydroxyl inherited from the methylbutinol can form a complex with a platinum catalyst, the modified methylbutinol has more coordination groups compared with the methylbutinol. After the methylbutylenol derivative is used for partially replacing the methylbutylenol, the obtained retarder has higher stability, and is beneficial to delaying the time for the vulcanization reaction of the silicone rubber. Meanwhile, the methyl butenol derivative with carboxyl is easier to form hydrogen bonds, so that the possibility of thermal desorption of methyl butynol is reduced, and the time for the vulcanization reaction of the silicon rubber is further prolonged. After the start of vulcanization, the desorbent slow release capsule gradually releases persulfate as heating proceeds. After the vulcanization temperature is reached, the persulfate is completely released, and unsaturated bonds in the methylbutyl alcohol and methylbutyl alcohol derivatives which are subjected to complexing on the surface of the platinum catalyst are oxidized, so that coordination bonds between the unsaturated bonds and the platinum catalyst are broken, and the rapid desorption of the retarder is realized. After that, the catalytic activity of the platinum catalyst is recovered, and the normal operation of the vulcanization reaction is ensured.
Preferably, the silicone rubber retarder comprises the following components in parts by weight: 9-11 parts of unsaturated alcohol compound preparation and 4-6 parts of desorbent sustained-release capsule.
By adopting the technical scheme, the proportion of the unsaturated alcohol compound preparation in the retarder is optimized, and the retarding effect on the vulcanization reaction is improved.
Preferably, the methyl butenol derivative is prepared as follows:
(1) Uniformly mixing methylbutinol, a peroxide initiator and dimethylbenzene, then introducing hydrogen halide into the mixture, heating in a water bath, and purifying the mixture by reduced pressure distillation after heating is finished to obtain a halogenated compound of methylbutinol; in this step, the hydrogen halide is hydrogen chloride or hydrogen bromide;
(2) Mixing the methyl butenol halogenide, an organic chain segment donor, dimethylbenzene and sodium hydroxide, heating and refluxing, pickling and separating liquid obtained by refluxing after the refluxing, and continuously extracting and distilling an organic phase obtained by separating liquid under reduced pressure to obtain the methyl butenol derivative.
By adopting the technical scheme, the application causes the free radical addition of the methylbutynol and the hydrogen halide under the initiation of the peroxide initiator to obtain the halogenated compound of the methylbutylenol, and then causes the halogenated compound of the methylbutylenol and the alkali metal alkoxide to generate nucleophilic substitution reaction to eliminate halogen atoms through the catalysis of sodium hydroxide to obtain the methylbutylenol derivative.
Preferably, the organic segment donor is prepared as follows:
(1) Uniformly mixing alcohol, dimethylbenzene, water and sodium hydroxide, and then heating and refluxing the mixed product; the alcohol used in this step is a monohydric alcohol having a carboxyl group;
(2) After the completion of the reflux, the refluxed product was evaporated under reduced pressure, water and xylene were removed, and then solid impurities were filtered off, and the residue was dissolved with absolute ethanol to obtain an organic segment donor.
By adopting the technical scheme, the sodium alkoxide and alcohol mixture is prepared in the aqueous dimethylbenzene by the way of co-heating sodium hydroxide and alcohol, and the sodium alkoxide has the property of sodium carboxylate for the monohydric alcohol with carboxyl.
Preferably, in the step (1) of preparing the organic segment donor, the monohydric alcohol having a carboxyl group is glycolic acid.
By adopting the technical scheme, when the glycolic acid is selected to prepare the organic chain segment donor, the organic chain segment donor is the mixture of disodium glycolate and glycolic acid, and the glycolic acid has chelating capacity and can form chelate with the platinum catalyst, so that the catalytic activity of the platinum catalyst is reduced, and the time for the vulcanization reaction of the silicone rubber is prolonged. In addition, the glycollic acid is decomposed under the temperature condition of the vulcanization reaction, so that the glycollic acid can automatically release the adsorption with the surface of the platinum catalyst, and the normal operation of the vulcanization reaction is ensured.
Preferably, the desorbent sustained release capsule is prepared according to the following method:
(1) Uniformly mixing stearic acid and absolute ethyl alcohol, and heating under the condition of constant-temperature water bath until the stearic acid is melted to obtain wall material precursor liquid;
(2) Adding core materials into wall material precursor liquid, uniformly stirring, cooling to room temperature, performing reduced pressure evaporation to remove ethanol, and sieving the rest solid products to obtain desorbent sustained-release capsules; in this step, the components of the core material include persulfates and nucleating agents.
By adopting the technical scheme, stearic acid is used as a wall material, the wall material is firstly mixed with absolute ethyl alcohol and heated to obtain a liquid stearic acid and absolute ethyl alcohol mixed solution, then the core material is heated and cooled, and the desorption agent slow-release capsule containing persulphate in the core material is obtained after decompression evaporation and screening. The wall material of the desorbent slow-release capsule is stearic acid, and the stearic acid is gradually melted under the heating condition of vulcanization reaction, so that the release of persulfate is realized.
Preferably, the nucleating agent is bentonite containing crystal water.
Through adopting above-mentioned technical scheme, bentonite can regard as the core when desorbent slowly-releasing capsule solidification shaping on the one hand, and on the other hand, the crystallization water in the bentonite can resume the mobility when being heated, resumes the crystallization water of mobility and can increase the humidity on bentonite granule surface to promoted the combination of bentonite granule and persulfate, be favorable to realizing the cladding of stearic acid to the persulfate.
Preferably, the component of the core material further comprises calcium acetate.
By adopting the technical scheme, the calcium acetate can solidify a part of ethanol, and the calcium acetate can react with stearic acid on the surface of bentonite particles to generate calcium stearate, so that the solidification of wall materials is promoted, the density of the capsule wall is increased, the loss of persulfate is reduced, and the storage effect of the desorbing agent slow-release capsule on the persulfate is enhanced.
In a second aspect, the application provides a silicone rubber synthetic leather containing a retarder, which adopts the following technical scheme:
The silicone rubber synthetic leather comprises a base cloth layer and a silicone rubber layer, wherein raw materials for preparing the silicone rubber layer comprise branched vinyl silicone oil, white carbon black, silazane, polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a pigment paste and any one of the silicone rubber retarders.
By adopting the technical scheme, the silicone rubber layer is prepared from the branched vinyl silicone oil, the white carbon black, the silazane, the polyacrylate modified phenyl silicone resin, the hydrogen-containing silicone oil, the silane coupling agent, the platinum catalyst, the color paste pigment and the silicone rubber retarder, and the silicone rubber layer and the base cloth layer are compounded to obtain the silicone rubber synthetic leather containing the retarder.
In a third aspect, the application provides a manufacturing process of silicone rubber synthetic leather, which adopts the following technical scheme.
A manufacturing process of silicone rubber synthetic leather comprises the following steps:
(1) Mixing branched vinyl silicone oil, white carbon black and silazane, and uniformly mixing polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a color paste pigment and any one of the silicone rubber retarders to obtain a silicone rubber mixture;
(2) Coating the silicone rubber mixture on release paper to obtain a mixture coating layer, then attaching a base cloth layer and the mixture coating layer, and heating the base cloth layer, the mixture coating layer and the release paper together until the mixture coating layer is vulcanized to obtain a silicone rubber layer;
(3) And after the silicone rubber layer is cooled to room temperature, removing the release paper to obtain the silicone rubber synthetic leather.
By adopting the technical scheme, the method comprises the steps of firstly mixing the branched vinyl silicone oil, the white carbon black and the silazane, then mixing the polyacrylate modified phenyl silicone resin, the hydrogen-containing silicone oil, the silane coupling agent, the platinum catalyst, the color paste pigment and the silicone rubber retarder to obtain a silicone rubber mixture, then vulcanizing and forming the silicone rubber mixture between release paper and a base cloth layer, and simultaneously completing the compounding of the silicone rubber layer and the base cloth layer to obtain the silicone rubber synthetic leather.
The silicon rubber retarder provided by the application realizes automatic failure of the retarder through the oxidation of persulfate while the vulcanization reaction is delayed, so that the desorption of the retarder from the surface of the platinum catalyst is promoted without increasing the temperature and prolonging the heating time, the energy consumption of the vulcanization process is reduced, the use of fossil fuel is reduced, and the low-carbon and environment-friendly effects are realized.
In summary, the application has the following beneficial effects:
1. According to the application, methylbutinol and methylbutinol derivatives are used as main components in the retarder, and the platinum catalyst is used for limiting the catalytic activity of the platinum catalyst by complexing groups such as alkynyl, alkenyl, hydroxyl and carboxyl groups, so that the time for the vulcanization reaction of the silicone rubber is prolonged. Meanwhile, the desorbing agent slow-release capsule in the retarder can release the desorbing agent at the vulcanization temperature, and is beneficial to ensuring the normal occurrence of vulcanization reaction.
2. In the application, the alcohol substance selected for preparing the organic chain segment donor is preferably glycolic acid, and on one hand, the glycolic acid can be complexed with the platinum catalyst, so that the limitation on the catalytic activity of the platinum catalyst is realized. On the other hand, the glycollic acid can automatically decompose under the temperature condition of the vulcanization reaction, thereby ensuring the normal occurrence of the vulcanization reaction.
3. According to the method, the lamination of the silicone rubber layer and the base cloth layer is realized during vulcanization molding, and the composition of the silicone rubber layer and the base cloth layer is finally obtained, so that the preparation of the silicone rubber synthetic leather is completed. The silicon rubber retarder does not need to promote desorption of the retarder from the surface of the platinum catalyst in a mode of increasing temperature and prolonging heating time, so that energy consumption of a vulcanization process is reduced, use of fossil fuel is reduced, and low-carbon and environment-friendly effects are realized.
Detailed Description
The present application will be described in further detail with reference to examples, preparations and comparative examples, and the raw materials according to the present application are all commercially available.
Preparation of methylbutenol derivatives
The following is an example of preparation 1.
Preparation example 1
The preparation example provides an organic chain segment donor and a methylbutyl alcohol derivative, wherein the structure of the methylbutyl alcohol derivative is shown as a formula (1):
In this preparation, the organic segment donor was prepared as follows:
(1) Uniformly mixing 10kg of glycolic acid, 25kg of xylene, 8kg of water and 12kg of sodium hydroxide, and then heating and refluxing the mixture at 75 ℃ for 4 hours;
(2) After completion of the reflux, the refluxed product was evaporated under reduced pressure, water and xylene were removed, and then solid impurities were removed by filtration, and the residue was dissolved with 10kg of absolute ethanol to obtain an organic segment donor.
In this preparation, the methylbutenol derivative is prepared according to the following method:
(1) Uniformly mixing 10kg of methylbutinol, 0.1kg of peroxide initiator and 18kg of dimethylbenzene, then introducing hydrogen halide gas into the mixed product at a rate of 2L/min, heating in a water bath at 85 ℃ for 1h, and separating residual hydrogen halide, dimethylbenzene and methylbutinol in a reaction system by reduced pressure distillation to obtain halogenated products of methylbutinol; in the step, hydrogen halide is hydrogen chloride, and peroxide initiator is dibenzoyl peroxide;
(2) Mixing 5kg of methyl butenol halogenide, 10kg of organic chain segment donor, 20kg of dimethylbenzene and 8kg of sodium hydroxide, heating and refluxing for 3 hours at 80 ℃, pickling and separating liquid obtained by refluxing after the refluxing, and continuously extracting and distilling an organic phase obtained by separating liquid to obtain methyl butenol derivatives; in the step, the reagent selected during acid washing is hydrochloric acid with the mass fraction of 10%, and the extractant is petroleum ether.
Preparation example 2
This preparation example differs from preparation example 1 in that the hydrogen chloride gas in step (1) of preparing the methylbutenol derivative is replaced with a hydrogen bromide gas.
Preparation example of desorbent sustained-release capsule
Preparation example 3
The preparation example provides a desorbent sustained-release capsule, which is prepared according to the following method: (1) Uniformly mixing 5kg of stearic acid and 10kg of absolute ethyl alcohol, heating to 75 ℃ under the condition of constant-temperature water bath, and preserving heat until the stearic acid is melted to obtain wall material precursor liquid;
(2) Adding 4.5kg of core material into the wall material precursor liquid, stirring uniformly, gradually cooling to room temperature at a speed of 10 ℃/h, evaporating under reduced pressure to remove ethanol, screening the rest solid product, and screening the part with the particle size of 200-350 mu m to obtain a desorption agent slow-release capsule; in the step, the components of the core material comprise 2kg of persulfate; in this step, the core material comprised 3kg persulfate and 1.5kg nucleating agent, which was calcined and dehydrated bentonite.
Preparation example 4
The present preparation example differs from preparation example 3 in that the nucleating agent is bentonite containing water of crystallization, and the mass fraction of water of crystallization in bentonite is 18%.
Preparation example 5
This preparation differs from preparation 4 in that the core material further comprises 0.5kg of calcium acetate.
Examples
Examples 1 to 5
The following description will take example 1 as an example.
Example 1
This example provides a silicone rubber retarder comprising 8kg of an unsaturated alcohol compound and 4kg of the desorbent sustained release capsule of preparation example 3, wherein the unsaturated alcohol compound is obtained by mixing 4kg of methylbutinol and 4kg of the methylbutinol derivative of preparation example 1.
The embodiment also provides a silicone rubber synthetic leather containing a retarder, which comprises a base cloth layer and a silicone rubber layer, wherein the silicone rubber layer is prepared from the following raw materials: 6kg of branched vinyl silicone oil, 1.5kg of white carbon black, 0.25kg of silazane, 1.5kg of polyacrylate modified phenyl silicone resin, 2kg of hydrogen-containing silicone oil, 0.15kg of silane coupling agent, 30g of platinum catalyst, 1kg of pigment paste, 8g of silicone rubber retarder prepared in the embodiment, and KH560 as the silane coupling agent.
In this example, a silicone rubber synthetic leather was prepared according to the following steps:
(1) Mixing a mixture of branched vinyl silicone oil, white carbon black and silazane at 60 ℃ for 3 hours, heating to 150 ℃ for mixing for 2 hours, and mixing and stirring polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a pigment paste and a silicone rubber retarder in a planetary mixer for 10 minutes after cooling a mixed product to room temperature to obtain a silicone rubber mixture;
(2) Coating the silicone rubber mixture on release paper to obtain a mixture coating layer, then attaching a base cloth layer and the mixture coating layer, placing the base cloth layer, the mixture coating layer and the release paper in a tunnel furnace, and heating and vulcanizing at 130 ℃ for 15min to obtain a silicone rubber layer;
(3) And after the silicone rubber layer is cooled to room temperature, removing the release paper to obtain the silicone rubber synthetic leather.
As shown in Table 1, examples 1-5 differ mainly in that the silicone rubber retarders were mixed by unsaturated alcohol complex formulations and desorbent slow-release capsules of different weights.
TABLE 1
| Sample of | Unsaturated alcohol composite preparation/kg | Desorbing agent slow-release capsule/kg |
| Example 1 | 8 | 4 |
| Example 2 | 9 | 4.5 |
| Example 3 | 10 | 5 |
| Example 4 | 11 | 5.5 |
| Example 5 | 12 | 6 |
Example 6
This example differs from example 3 in that the methylbutenol derivative in the unsaturated alcohol complex formulation is the methylbutenol derivative of preparation example 2.
Example 7
The present embodiment is different from embodiment 3 in that the desorbent slow release capsule is a desorbent slow release capsule of preparation example 4.
Example 8
The present embodiment is different from embodiment 7 in that the desorbent slow release capsule is a desorbent slow release capsule of preparation 5.
Comparative example
Comparative example 1
The silicone rubber synthetic leather containing the retarder comprises a base cloth layer and a silicone rubber layer, wherein the silicone rubber layer is prepared from the following raw materials: 6kg of branched vinyl silicone oil, 1.5kg of white carbon black, 0.25kg of silazane, 1.5kg of polyacrylate modified phenyl silicone resin, 2kg of hydrogen-containing silicone oil, 0.15kg of silane coupling agent, 30g of platinum catalyst, 1kg of pigment paste, 8g of silicone rubber retarder, wherein the silicone rubber retarder is methyl butynol, and the silane coupling agent is KH560.
The silicone rubber synthetic leather is prepared according to the following steps:
(1) Mixing a mixture of branched vinyl silicone oil, white carbon black and silazane at 60 ℃ for 3 hours, heating to 150 ℃ for mixing for 2 hours, and mixing and stirring polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a pigment paste and methyl butynol in a planetary mixer for 10 minutes after cooling a mixed product to room temperature to obtain a silicone rubber mixture;
(2) Coating the silicone rubber mixture on release paper to obtain a mixture coating layer, then attaching a base cloth layer and the mixture coating layer, placing the base cloth layer, the mixture coating layer and the release paper in a tunnel furnace, and heating and vulcanizing at 130 ℃ for 15min to obtain a silicone rubber layer;
(3) And after the silicone rubber layer is cooled to room temperature, removing the release paper to obtain the silicone rubber synthetic leather.
Comparative example 2
This comparative example is different from example 3 in that the component of the silicone rubber retarder does not include a desorbent slow-release capsule, and the silicone rubber retarder in the silicone rubber synthetic leather includes only 8g of an unsaturated alcohol complexing agent.
Comparative example 3
The comparative example is different from comparative example 1 in that the silicone rubber retarder is compounded by methylbutynol and the desorbent sustained-release capsule of preparation example 3 according to the application according to the weight ratio of 2:1, and the total weight of the methylbutynol is unchanged.
Performance detection test method
The vulcanization characteristics of the silicone rubbers of the examples and comparative examples of the present application were measured by a vulcanizing machine prescribed in GB/T16584, and the results are shown in Table 2.
TABLE 2
As can be seen from the combination of examples 1 to 5 and comparative example 1 and table 2, T 10 measured in examples 1 to 5 is greater than that in comparative example 1, indicating that the silicone rubber retarder compounded with methylbutynol and methylbutynol derivatives has a better retarding effect on vulcanization of silicone rubber after the carboxyl groups are also introduced into the methylbutynol derivatives by nucleophilic substitution reaction, because the newly introduced carboxyl groups and the hydroxyl groups inherited from the methylbutynol can form complexes with platinum catalyst, the modified methylbutynol has more coordinating groups than the methylbutynol. T 90 measured in examples 1-5 is smaller than that in comparative example 1, which shows that the silicone rubber retarder realizes desorption treatment of a platinum catalyst by means of oxidation effect of persulfate through compounding of an unsaturated alcohol compound preparation and a desorption agent slow-release capsule, and accelerates vulcanization rate of silicone rubber.
As can be seen from the combination of example 3 and comparative example 2 and the combination of table 2, the T 10 measured in example 3 is close to comparative example 2, while T 90 is smaller than comparative example 2, which shows that the catalyst activity of the platinum catalyst is well inhibited by the methylbutenol derivative in the silicone rubber retarder of the present application without adding the desorbent slow-release capsule, and the methylbutenol derivative is difficult to spontaneously detach from the surface of the platinum catalyst, so that the vulcanization rate of the silicone rubber is also slowed down while the vulcanization reaction is delayed.
As can be seen from the combination of example 3 and comparative example 3 and table 2, the T 10 measured in comparative example 3 is close to comparative example 1, and T 90 is smaller than comparative example 1, which means that after the desorbent sustained-release capsule of the present application is applied, the persulfate gradually oxidizes the methylbutinol along with the gradual release of the persulfate component in the desorbent, thereby separating the methylbutinol from the surface of the platinum catalyst, recovering the catalytic activity of the platinum catalyst, and thus accelerating the sulfidation rate.
As can be seen from a combination of example 3 and example 6 and from table 2, both T 90 and T 10 measured in example 6 are similar to example 3, indicating no significant change in the properties of the methylbutyl alcohol derivatives obtained by varying the hydrogen halide species.
As can be seen in combination with example 3, example 7 and table 2, T 10 measured in example 7 is greater than example 3, and T 90 is less than example 3, indicating that the release of crystal water from bentonite when heated promotes the combination of bentonite and persulfate, improving the coating effect of stearic acid on persulfate, thereby reducing the total amount of persulfate released in advance by the desorbent slow release capsule, and helping to maintain the delay effect of the delay agent on the vulcanization of silicone rubber. Meanwhile, the total quantity of the persulfate released in advance is reduced, so that the persulfate has a better desorption effect on the platinum catalyst, and the vulcanization rate of the silicone rubber is accelerated.
As can be seen from the combination of example 8 and example 7 and the combination of table 2, T 10 measured in example 8 is greater than example 7, and T 90 is less than example 7, which shows that in example 8, calcium acetate and stearic acid are combined to form calcium stearate particles on the premise that the bentonite releases crystal water by adding calcium acetate into the core material, thereby promoting the solidification of the capsule wall of the desorbent slow-release capsule, improving the coating effect of the desorbent slow-release capsule on persulfate, helping to maintain the delay effect of the delay agent on the vulcanization of the silicone rubber and accelerating the vulcanization rate of the silicone rubber.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (9)
1. The silicone rubber retarder is characterized by comprising the following components in parts by weight: 8-12 parts of an unsaturated alcohol composite preparation and 4-6 parts of a desorbent slow release capsule, wherein the unsaturated alcohol composite preparation is formed by mixing methylbutinol and a methylbutinol derivative, the methylbutinol derivative is obtained by nucleophilic substitution reaction of halogen atoms in an addition product of methylbutinol and hydrogen halide and an organic chain segment donor, the components of the organic chain segment donor comprise alkali metal alkoxide, and alcohol corresponding to the alkali metal alkoxide is monohydric alcohol with carboxyl; the components of the desorbent slow release capsule comprise persulfate;
The desorbent sustained release capsule is prepared according to the following method:
(1) Uniformly mixing stearic acid and absolute ethyl alcohol, and heating under the condition of constant-temperature water bath until the stearic acid is melted to obtain wall material precursor liquid;
(2) Adding core materials into wall material precursor liquid, uniformly stirring, cooling to room temperature, performing reduced pressure evaporation to remove ethanol, and sieving the rest solid products to obtain desorbent sustained-release capsules; in this step, the components of the core material include persulfates and nucleating agents.
2. The silicone rubber retarder according to claim 1, comprising the following components in parts by weight: 9-11 parts of unsaturated alcohol compound preparation and 4-6 parts of desorbent sustained-release capsule.
3. The silicone rubber retarder according to claim 1, wherein the methylbutenol derivative is prepared according to the following method:
(1) Uniformly mixing methylbutinol, a peroxide initiator and dimethylbenzene, then introducing hydrogen halide into the mixture, heating in a water bath, and purifying the mixture by reduced pressure distillation after heating is finished to obtain a halogenated compound of methylbutinol; in this step, the hydrogen halide is hydrogen chloride or hydrogen bromide;
(2) Mixing the methyl butenol halogenide, an organic chain segment donor, dimethylbenzene and sodium hydroxide, heating and refluxing, pickling and separating liquid obtained by refluxing after the refluxing, and continuously extracting and distilling an organic phase obtained by separating liquid under reduced pressure to obtain the methyl butenol derivative.
4. A silicone rubber retarder according to claim 3, wherein the organic segment donor is prepared according to the following method:
(1) Uniformly mixing alcohol, dimethylbenzene, water and sodium hydroxide, and then heating and refluxing the mixed product; the alcohol used in this step is a monohydric alcohol having a carboxyl group;
(2) After the completion of the reflux, the refluxed product was evaporated under reduced pressure, water and xylene were removed, and then solid impurities were filtered off, and the residue was dissolved with absolute ethanol to obtain an organic segment donor.
5. The silicone rubber retarder according to claim 4, wherein in step (1) of preparing the organic segment donor, the monohydric alcohol having a carboxyl group is glycolic acid.
6. The silicone rubber retarder of claim 1, wherein the nucleating agent is bentonite containing water of crystallization.
7. The silicone rubber retarder of claim 6, wherein the core material further comprises calcium acetate.
8. The silicone rubber synthetic leather containing the retarder is characterized by comprising a base cloth layer and a silicone rubber layer, wherein raw materials for preparing the silicone rubber layer comprise branched vinyl silicone oil, white carbon black, silazane, polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a color paste pigment and the silicone rubber retarder according to any one of claims 1-7.
9. The manufacturing process of the silicone rubber synthetic leather is characterized by comprising the following steps of:
(1) Mixing branched vinyl silicone oil, white carbon black and silazane, and uniformly mixing polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, a silane coupling agent, a platinum catalyst, a color paste pigment and the silicone rubber retarder according to any one of claims 1-7 to obtain a silicone rubber mixture;
(2) Coating the silicone rubber mixture on release paper to obtain a mixture coating layer, then attaching a base cloth layer and the mixture coating layer, and heating the base cloth layer, the mixture coating layer and the release paper together until the mixture coating layer is vulcanized to obtain a silicone rubber layer;
(3) And after the silicone rubber layer is cooled to room temperature, removing the release paper to obtain the silicone rubber synthetic leather.
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| JP2007217693A (en) * | 2007-02-15 | 2007-08-30 | Shin Etsu Chem Co Ltd | Silicone rubber composite material and method for producing the same |
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| CN108951182A (en) * | 2018-07-13 | 2018-12-07 | 广东天跃新材料股份有限公司 | Mirror surface woven fabric silicon rubber synthetic leather and its manufacturing technology |
| CN113667293A (en) * | 2021-09-06 | 2021-11-19 | 深圳市力信陆南实业有限公司 | Flame-retardant polyurethane high-tenacity rubber prepolymer and preparation method thereof |
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| JP2007217693A (en) * | 2007-02-15 | 2007-08-30 | Shin Etsu Chem Co Ltd | Silicone rubber composite material and method for producing the same |
| CN106189258A (en) * | 2016-08-09 | 2016-12-07 | 天津凯华绝缘材料股份有限公司 | Adjustable silicon composition of curing rate and its preparation method and application |
| CN108951182A (en) * | 2018-07-13 | 2018-12-07 | 广东天跃新材料股份有限公司 | Mirror surface woven fabric silicon rubber synthetic leather and its manufacturing technology |
| CN113667293A (en) * | 2021-09-06 | 2021-11-19 | 深圳市力信陆南实业有限公司 | Flame-retardant polyurethane high-tenacity rubber prepolymer and preparation method thereof |
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