CN114591536A - Silicone rubber retarder, silicone rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicone rubber synthetic leather - Google Patents
Silicone rubber retarder, silicone rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicone rubber synthetic leather Download PDFInfo
- Publication number
- CN114591536A CN114591536A CN202210339104.XA CN202210339104A CN114591536A CN 114591536 A CN114591536 A CN 114591536A CN 202210339104 A CN202210339104 A CN 202210339104A CN 114591536 A CN114591536 A CN 114591536A
- Authority
- CN
- China
- Prior art keywords
- silicone rubber
- retarder
- mixture
- synthetic leather
- alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 115
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 96
- 239000002649 leather substitute Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 238000005265 energy consumption Methods 0.000 title abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000003054 catalyst Substances 0.000 claims abstract description 42
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 42
- VBPSVYDSYVJIPX-UHFFFAOYSA-N pent-2-en-2-ol Chemical class CCC=C(C)O VBPSVYDSYVJIPX-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002775 capsule Substances 0.000 claims abstract description 37
- 238000002360 preparation method Methods 0.000 claims abstract description 35
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000003795 desorption Methods 0.000 claims abstract description 19
- -1 alkali metal salt Chemical class 0.000 claims abstract description 17
- ACIAHEMYLLBZOI-ZZXKWVIFSA-N Unsaturated alcohol Chemical compound CC\C(CO)=C/C ACIAHEMYLLBZOI-ZZXKWVIFSA-N 0.000 claims abstract description 14
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 7
- 238000010534 nucleophilic substitution reaction Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 44
- 239000010410 layer Substances 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 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
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 22
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 229920002545 silicone oil Polymers 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 18
- 239000002585 base Substances 0.000 claims description 17
- 239000004744 fabric Substances 0.000 claims description 17
- 235000021355 Stearic acid Nutrition 0.000 claims description 15
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 15
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 15
- 239000008117 stearic acid Substances 0.000 claims description 15
- 239000011247 coating layer Substances 0.000 claims description 14
- 239000011162 core material 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
- 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
- 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
- 239000000463 material Substances 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 239000008096 xylene Substances 0.000 claims description 8
- HNVRRHSXBLFLIG-UHFFFAOYSA-N 3-hydroxy-3-methylbut-1-ene Chemical compound CC(C)(O)C=C HNVRRHSXBLFLIG-UHFFFAOYSA-N 0.000 claims description 7
- 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
- 239000000386 donor Substances 0.000 claims description 7
- 239000002667 nucleating agent Substances 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
- 238000004821 distillation Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 150000004820 halides Chemical class 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 150000002978 peroxides Chemical class 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000013268 sustained release Methods 0.000 claims description 5
- 239000012730 sustained-release form Substances 0.000 claims description 5
- 239000002253 acid Substances 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
- 238000005406 washing Methods 0.000 claims description 4
- 210000001124 body fluid Anatomy 0.000 claims description 3
- 239000010839 body fluid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 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
- 239000007787 solid Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000004073 vulcanization Methods 0.000 abstract description 36
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 14
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 125000000304 alkynyl group Chemical group 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 125000003342 alkenyl group Chemical group 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000010668 complexation reaction Methods 0.000 abstract description 2
- 238000010092 rubber production Methods 0.000 abstract description 2
- AKOWCUWKQQMMFB-UHFFFAOYSA-N CCC(Cl)=C(C)O Chemical compound CCC(Cl)=C(C)O AKOWCUWKQQMMFB-UHFFFAOYSA-N 0.000 abstract 1
- 239000000446 fuel Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 19
- 230000003111 delayed effect Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 238000013329 compounding Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000008187 granular material Substances 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
- 239000002803 fossil fuel Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005987 sulfurization reaction Methods 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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-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
- 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
- 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
- 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
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007342 radical addition reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- 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 desorbent slow-release capsule, wherein the unsaturated alcohol composite preparation is formed by mixing methyl butynol and methyl butenol derivatives, and the methyl butenol derivatives are products of nucleophilic substitution reaction between alkali metal salt with carboxyl alcohol and chloro methyl butenol. The method utilizes the complexation of the platinum catalyst on the alkynyl, alkenyl, hydroxyl, carboxyl and other groups to limit the catalytic activity of the platinum catalyst, and is beneficial to delaying the time of the vulcanization reaction of the silicon rubber. Meanwhile, the retarder can realize desorption without increasing the temperature and prolonging the heating time, so that the energy consumption of a vulcanization process is reduced, the use of petrochemical fuels is reduced, and the effects of low carbon and environmental protection are realized.
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 a synthetic rubber with excellent performance, and is one of the research hotspots in the rubber field in recent decades. The addition type liquid silicone rubber is novel silicone rubber developed under the background, and has the advantages of aging resistance, no toxicity, no odor, good insulating property and the like, and also has the advantages of small shrinkage rate in the vulcanization process, simple and convenient deep vulcanization operation and the like relative to other synthetic rubbers. In the synthesis of addition type liquid silicone rubber, adsorption catalysis is generally performed using a platinum catalyst, and since the platinum catalyst has extremely high catalytic activity, it is generally necessary to add a retarder to the raw material of 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 by using 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 forms a complex adsorption layer on the surface of the platinum catalyst, so that adsorption between the platinum catalyst and the silicon rubber monomer is hindered, and occurrence of vulcanization reaction is delayed.
In view of the above-mentioned related art, the inventors of the present invention have considered 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 maintain the adsorption of methylbutynol for a long time, and the effect of delaying the occurrence of the vulcanization reaction of methylbutynol is not good.
Disclosure of Invention
In the related technology, the platinum catalyst is difficult to keep the adsorption of the methylbutinol for a long time, so that the effect of delayed vulcanization reaction of the methylbutinol is poor.
In a first aspect, the present application provides a silicone rubber retarder, which adopts the following technical scheme:
a 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 methyl butynol and a methyl butenol derivative, the methyl butenol derivative is obtained by carrying out nucleophilic substitution reaction on a halogen atom in an addition product of the methyl butynol and hydrogen halide and an organic chain segment donor, the organic chain segment donor comprises an alkali metal alkoxide, and the alcohol corresponding to the alkali metal alkoxide is monohydric alcohol with carboxyl; the desorption agent slow-release capsule comprises persulfate.
By adopting the technical scheme, the methyl butynol is modified, the monohalide of the methyl butynol is obtained through the addition reaction, then the nucleophilic substitution reaction is carried out on the halogen atom and the alkali metal alkoxide, and the methyl butynol derivative is obtained after the alkali metal halide is removed. The alkenyl and alkynyl in the methyl butenol derivative can form a complex with a platinum catalyst similarly. Meanwhile, carboxyl is introduced into the methylbutinol derivative through nucleophilic substitution reaction, and both the newly introduced carboxyl and hydroxyl inherited from methylbutinol can form a complex with a platinum catalyst, so that the modified methylbutinol has more coordination groups compared with methylbutinol. After the methylbutenol derivative is used for partially replacing methylbutinol, the obtained retarder has higher stability and is beneficial to delaying the time of the vulcanization reaction of the silicon rubber. Meanwhile, because the methyl butenol derivative introduced with the carboxyl is easier to form a hydrogen bond, the possibility of thermal desorption of the methyl butenol is reduced, and the time of the vulcanization reaction of the silicone rubber is further prolonged. After the vulcanization is started, the desorbent slow-release capsule gradually releases the persulfate as the heating is carried out. After reaching the vulcanization temperature, the persulfate is completely released, and the unsaturated bond in the methyl butynol and methyl butenol derivative complexed on the surface of the platinum catalyst is oxidized, so that the coordination bond between the unsaturated bond and the platinum catalyst is broken, and the rapid desorption of the retarder is realized. After that, the catalytic activity of the platinum catalyst is recovered, and the normal running 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 slow-release capsule.
By adopting the technical scheme, the proportion of the unsaturated alcohol compound preparation in the retarder is optimized, and the improvement of the delayed effect on the vulcanization reaction is facilitated.
Preferably, the methylbutenol derivative is prepared according to the following method:
(1) uniformly mixing methyl butynol, a peroxide initiator and xylene, introducing hydrogen halide into the mixture, heating in a water bath, and purifying the mixture by reduced pressure distillation after heating to obtain a halide of the methyl butenol; in the step, the hydrogen halide is hydrogen chloride or hydrogen bromide;
(2) mixing methyl butenol halide, an organic chain segment donor, xylene and sodium hydroxide, heating and refluxing, carrying out acid washing and liquid separation on liquid obtained by refluxing after refluxing is finished, and carrying out continuous extraction and reduced pressure distillation on an organic phase obtained by liquid separation to obtain the methyl butenol derivative.
By adopting the technical scheme, under the initiation of a peroxide initiator, the methyl butynol and hydrogen halide are subjected to free radical addition to obtain a halide of the methyl butenol, and the halide of the methyl butenol and alkali metal alkoxide are subjected to nucleophilic substitution reaction under the catalysis of sodium hydroxide to eliminate halogen atoms, so that the methyl butenol derivative is obtained.
Preferably, the organic segment donor is prepared as follows:
(1) uniformly mixing alcohol, dimethylbenzene, water and sodium hydroxide, and then heating and refluxing the mixture; the alcohol used in this step is a monohydric alcohol having a carboxyl group;
(2) and after the reflux is finished, performing reduced pressure evaporation on the reflux product, removing water and xylene, filtering out solid impurities, and dissolving the residue by using absolute ethyl alcohol to obtain the organic chain segment donor.
By adopting the technical scheme, the mixture of sodium alkoxide and alcohol is prepared by co-heating sodium hydroxide and alcohol in aqueous xylene, and the sodium alkoxide also has the property of sodium carboxylate for 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 a mixture of disodium glycolate and glycolic acid, and the glycolic acid has chelating capacity and can form a chelate with a platinum catalyst, thereby being beneficial to reducing the catalytic activity of the platinum catalyst and prolonging the time for the silicon rubber to generate vulcanization reaction. Further, since glycolic acid is decomposed under the temperature condition of the sulfurization reaction, glycolic acid can automatically desorb from the surface of the platinum catalyst, and the normal progress of the sulfurization reaction is ensured.
Preferably, the desorbent slow-release capsule is prepared by the following method:
(1) uniformly mixing stearic acid and absolute ethyl alcohol, and then heating the mixture under the condition of constant-temperature water bath until the stearic acid is molten to obtain a wall material precursor body fluid;
(2) adding a core material into the wall material precursor liquid, uniformly stirring, cooling to room temperature, performing reduced pressure evaporation to remove ethanol, and screening the residual solid product to obtain a desorbent sustained-release capsule; in this step, the components of the core material include persulfate and a nucleating agent.
By adopting the technical scheme, stearic acid is used as a wall material, the stearic acid and absolute ethyl alcohol are mixed and heated to obtain a mixed solution of liquid stearic acid and absolute ethyl alcohol, then the core material is heated and the mixed solution is cooled, and the desorption agent slow-release capsule containing persulfate in the core material is obtained after decompression evaporation and screening. The wall material of the desorption agent 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 the persulfate is realized.
Preferably, the nucleating agent is bentonite containing crystal water.
Through adopting above-mentioned technical scheme, the core when desorption agent slowly-releasing capsule solidification shaping can be regarded as to bentonite on the one hand, and on the other hand, the crystallization water in the bentonite can resume mobility when being heated, and the crystallization water that resumes mobility 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 composition of the core material further comprises calcium acetate.
Through adopting above-mentioned technical scheme, calcium acetate can make partly ethanol take place to solidify, can also react with stearic acid at bentonite granule surface through calcium acetate and produce calcium stearate to promote the solidification of wall material, increased the density of capsule wall, help reducing the loss of persulfate, strengthened the storage effect of desorption agent sustained-release capsule to persulfate.
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, and 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 any one of the silicone rubber delay agents.
By adopting the technical scheme, the silicone rubber layer is prepared by taking 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 as raw materials, and the silicone rubber layer is compounded with the base cloth layer to obtain the silicone rubber synthetic leather containing the retarder.
In a third aspect, the application provides a manufacturing process of the silicone rubber synthetic leather, which adopts the following technical scheme.
A manufacturing process of silicon rubber synthetic leather comprises the following steps:
(1) mixing branched vinyl silicone oil, white carbon black and silazane, and then 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 delay agents to obtain a silicone rubber mixture;
(2) coating a 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.
According to the technical scheme, the method comprises the steps of mixing branched vinyl silicone oil, white carbon black and silazane, 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 delay agent to obtain a silicone rubber mixture, vulcanizing and molding the silicone rubber mixture between release paper and a base cloth layer, and compounding the silicone rubber layer and the base cloth layer to obtain the silicone rubber synthetic leather.
The silicon rubber retarder realizes the automatic invalidation of the retarder through the oxidation of persulfate when the delayed vulcanization reaction occurs, so that the desorption of the retarder from the surface of a platinum catalyst is not required to be promoted in a mode of increasing the temperature and prolonging the heating time, the energy consumption of a vulcanization process is reduced, the use of fossil fuel is reduced, and the effect of low carbon and environmental protection is realized.
In summary, the present application has the following beneficial effects:
1. according to the method, methylbutinol and methylbutenol derivatives are used as main components in the retarder, and the catalytic activity of the platinum catalyst is limited by utilizing the complexation of the platinum catalyst on alkynyl, alkenyl, hydroxyl, carboxyl and other groups, so that the time of the vulcanization reaction of the silicon rubber is delayed. Simultaneously, desorbent sustained-release capsule in the delay agent of this application can release the desorbent under the vulcanization temperature, helps guaranteeing the normal emergence of vulcanization reaction.
2. In the application, the alcohol substance preferably used for preparing the organic chain segment donor is glycolic acid, and 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 glycolic 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 silicon rubber layer is attached to the base cloth layer while vulcanization molding is carried out, the silicon rubber layer and the base cloth layer are compounded finally, and the preparation of the silicon rubber synthetic leather is completed. The silicon rubber retarder does not need to promote desorption of the retarder from the surface of a platinum catalyst in a mode of increasing the temperature and prolonging the heating time, so that the energy consumption of a vulcanization process is reduced, the use of fossil fuels is reduced, and the effects of low carbon and environmental protection are realized.
Detailed Description
The present application will be described in further detail with reference to examples, preparations and comparative examples, and all of the starting materials mentioned in the present application are commercially available.
Preparation example of Methylbutenol derivative
The following will explain preparation example 1 as an example.
Preparation example 1
The preparation example provides an organic chain segment donor and a methyl butenol derivative, wherein the structure of the methyl butenol derivative is shown as the formula (1):
in this preparation, the organic segment donor was prepared as follows:
(1) uniformly mixing 10kg of glycolic acid, 25kg of dimethylbenzene, 8kg of water and 12kg of sodium hydroxide, and heating and refluxing the mixture at 75 ℃ for 4 hours;
(2) after the reflux, the reflux product was evaporated under reduced pressure to remove water and xylene, and then filtered to remove solid impurities, and the residue was dissolved with 10kg of anhydrous ethanol to obtain an organic segment donor.
In this preparation, the methylbutenol derivative was prepared by 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 mixture at the speed of 2L/min, heating in a water bath at 85 ℃, and separating out the residual hydrogen halide, dimethylbenzene and methylbutinol in a reaction system by reduced pressure distillation after heating for 1h to obtain a halide of the methylbutinol; in the step, the hydrogen halide is hydrogen chloride, and the peroxide initiator is dibenzoyl peroxide;
(2) mixing 5kg of methyl butenol halide, 10kg of organic chain segment donor, 20kg of dimethylbenzene and 8kg of sodium hydroxide, heating and refluxing for 3 hours at 80 ℃, carrying out acid washing and liquid separation on liquid obtained by refluxing after the refluxing is finished, and then carrying out continuous extraction and reduced pressure distillation on an organic phase obtained by liquid separation to obtain a methyl butenol derivative; in the step, a reagent selected in acid washing is hydrochloric acid with the mass fraction of 10%, and an extracting agent is petroleum ether.
Preparation example 2
This production example is different from production example 1 in that the hydrogen chloride gas in step (1) of producing a methylbutenol derivative is replaced with hydrogen bromide gas.
Preparation example of Desorption agent sustained Release Capsule
Preparation example 3
The preparation example provides a desorption agent slow-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 body fluid;
(2) adding 4.5kg of core material into the wall material precursor liquid, stirring uniformly, then gradually cooling to room temperature at the speed of 10 ℃/h, then removing ethanol by reduced pressure evaporation, screening the rest solid product, and screening the part with the grain diameter of 200-350 mu m to obtain the desorbent slow-release capsule; in the step, the components of the core material comprise 2kg of persulfate; in the step, the core material comprises 3kg of persulfate and 1.5kg of nucleating agent, and the nucleating agent is calcined and dehydrated bentonite.
Preparation example 4
The difference between this preparation example and preparation example 3 is that the nucleating agent is bentonite containing crystal water, and the mass fraction of crystal water in the bentonite is 18%.
Preparation example 5
The difference between the preparation example and the preparation example 4 is that the components of the core material further comprise 0.5kg of calcium acetate.
Examples
Examples 1 to 5
The following description will be given by taking example 1 as an example.
Example 1
This example provides a silicone rubber retarder comprising 8kg of an unsaturated alcohol complex formulation and 4kg of the desorbent-releasing capsule of preparation example 3, wherein the unsaturated alcohol complex formulation is obtained by mixing 4kg of methylbutynol and 4kg of the methylbutenol derivative of preparation example 1.
The embodiment also provides the silicone rubber synthetic leather containing the 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 color paste pigment, 8g of silicone rubber retarder prepared in the embodiment, wherein the silane coupling agent is KH 560.
In this example, the 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 3h, heating to 150 ℃ and mixing for 2h, waiting for the mixed product to be cooled to room temperature, and mixing and stirring the mixed product of polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, silane coupling agent, platinum catalyst, color paste pigment and silicone rubber retarder in a planetary mixer for 10min to obtain a silicone rubber mixture;
(2) coating a 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 to 5 are different mainly in that the silicone rubber retarder is formed by mixing unsaturated alcohol complex formulations and desorbent slow-release capsules of different weights.
TABLE 1
| Sample(s) | Unsaturated alcohol composite preparation/kg | Desorption agent slow release capsule/kg |
| Example 1 | 8 | 4 |
| Example 2 | 9 | 4.5 |
| Examples3 | 10 | 5 |
| Example 4 | 11 | 5.5 |
| Example 5 | 12 | 6 |
Example 6
This example is different 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 example is different from example 3 in that the desorbent slow-release capsule is the desorbent slow-release capsule of preparation example 4.
Example 8
This example is different from example 7 in that the desorbent slow-release capsule is the desorbent slow-release capsule of preparation example 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 color paste pigment and 8g of silicone rubber retarder, wherein the silicone rubber retarder is methyl butynol, and the silane coupling agent is KH 560.
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 3h, heating to 150 ℃ for mixing for 2h, waiting for the mixed product to be cooled to room temperature, and mixing and stirring the mixed product of polyacrylate modified phenyl silicone resin, hydrogen-containing silicone oil, silane coupling agent, platinum catalyst, pigment paste and methyl butynol in a planetary mixer for 10min to obtain a silicone rubber mixture;
(2) coating a 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
The difference between the comparative example and the example 3 is that the components of the silicone rubber retarder do not comprise desorption agent slow release capsules, and the silicone rubber retarder in the silicone rubber synthetic leather only comprises 8g of unsaturated alcohol complexing agent.
Comparative example 3
The difference between the comparative example and the comparative example 1 is that the silicone rubber retarder is formed by compounding the methylbutinol and the desorbent slow-release capsule of the preparation example 3 according to the weight ratio of 2:1, and the total weight of the methylbutinol 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 using a vulcanizer specified in GB/T16584, and the results are shown in Table 2.
TABLE 2
As can be seen by combining examples 1-5 with comparative example 1 and by combining Table 2, T measured in examples 1-510Compared with the comparative example 1, the results show that after carboxyl is further introduced into the methylbutenol derivative through nucleophilic substitution reaction, the newly introduced carboxyl and the hydroxyl inherited from the methylbutenol can form a complex with a platinum catalyst, so that the modified methylbutynol has more coordination groups than the methylbutynol, and the silicon rubber retarder obtained by compounding the methylbutynol and the methylbutenol derivative has the effect of vulcanizing silicon rubberBetter delay effect. T measured in examples 1 to 590All are smaller than the comparative example 1, which shows that the silicon rubber retarder realizes desorption treatment of platinum catalyst by means of the oxidation effect of persulfate through the compounding of the unsaturated alcohol composite preparation and the desorption agent slow-release capsule, and accelerates the vulcanization rate of the silicon rubber.
As can be seen by combining example 3 with comparative example 2 and by combining Table 2, T measured in example 310Close to comparative example 2, and T90Compared with the comparative example 2, the result shows that under the condition that no desorption agent slow-release capsule is added, the methylbutenol derivative in the silicone rubber retarder has a good inhibition effect on the catalytic activity of a platinum catalyst, and the methylbutenol derivative is difficult to spontaneously separate from the surface of the platinum catalyst, so that the vulcanization rate of silicone rubber is slowed down while the vulcanization reaction is delayed.
As can be seen by combining example 3 and comparative example 3 with Table 2, T measured in comparative example 310Close to comparative example 1, and T90Smaller than comparative example 1, it is demonstrated that after the application of the desorbent slow-release capsule of the present application, with the gradual release of the persulfate component in the desorbent, the persulfate gradually oxidizes the methylbutynol, so that the methylbutynol is separated from the surface of the platinum catalyst, the catalytic activity of the platinum catalyst is recovered, and the vulcanization rate is accelerated.
As can be seen by combining example 3 and example 6 with Table 2, T was measured in example 690And T10All are close to example 3, which shows that the properties of the methylbutenol derivative obtained by changing the kind of the hydrogen halide are not obviously changed.
As can be seen by combining examples 3 and 7 with Table 2, T measured in example 710Greater than example 3, and T90Less than example 3, it is demonstrated that the crystal water released by the bentonite when heated promotes the combination of the bentonite and the persulfate, and improves the coating effect of stearic acid on the persulfate, thereby reducing the total amount of the persulfate which is released by the desorbent slow-release capsule in advance and helping to maintain the delayed effect of the retarder on the vulcanization of the silicone rubber. At the same time, since persulfate is released in advanceThe total amount is reduced, so that the desorption effect of the persulfate on the platinum catalyst is better, and the vulcanization rate of the silicone rubber is accelerated.
As can be seen by combining example 8, example 7 and Table 2, T was measured in example 810Greater than example 7, and T90Smaller than example 7, it is shown in example 8 that calcium acetate is added to the core material, and calcium stearate particles are formed by combining calcium acetate and stearic acid on the premise that crystal water is released from bentonite, so that the solidification of the capsule wall of the desorbent slow-release capsule is promoted, the coating effect of the desorbent slow-release capsule on persulfate is improved, the delayed effect of the retarder on the vulcanization of silicone rubber is maintained, and the vulcanization rate of the silicone rubber is accelerated.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
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 methyl butynol and a methyl butenol derivative, the methyl butenol derivative is obtained by carrying out nucleophilic substitution reaction on a halogen atom in an addition product of the methyl butynol and hydrogen halide and an organic chain segment donor, the organic chain segment donor comprises an alkali metal alkoxide, and the alcohol corresponding to the alkali metal alkoxide is monohydric alcohol with carboxyl; the desorption agent slow-release capsule comprises persulfate.
2. The silicone rubber retarder of claim 1, comprising the following components in parts by weight: 9-11 parts of unsaturated alcohol compound preparation and 4-6 parts of desorbent slow-release capsule.
3. The silicone rubber retarder of claim 1, wherein the methylbutenol derivative is prepared according to the following method:
(1) uniformly mixing methyl butynol, a peroxide initiator and xylene, introducing hydrogen halide into the mixture, heating in a water bath, and purifying the mixture by reduced pressure distillation after heating to obtain a halide of the methyl butenol; in the step, the hydrogen halide is hydrogen chloride or hydrogen bromide;
(2) mixing methyl butenol halide, an organic chain segment donor, xylene and sodium hydroxide, heating and refluxing, carrying out acid washing and liquid separation on liquid obtained by refluxing after refluxing is finished, and carrying out continuous extraction and reduced pressure distillation on an organic phase obtained by liquid separation to obtain the methyl butenol derivative.
4. The silicone rubber retarder of claim 3, wherein the organic segment donor is prepared by:
(1) uniformly mixing alcohol, dimethylbenzene, water and sodium hydroxide, and then heating and refluxing the mixture; the alcohol used in this step is a monohydric alcohol having a carboxyl group;
(2) and after the reflux is finished, performing reduced pressure evaporation on the reflux product, removing water and xylene, filtering out solid impurities, and dissolving the residue by using absolute ethyl alcohol to obtain the organic chain segment donor.
5. The silicone rubber retarder according to claim 4, wherein in the step (1) of preparing the organic segment donor, the monohydric alcohol having a carboxyl group is glycolic acid.
6. The silicone rubber delay agent of claim 1, wherein the desorbent slow-release capsule is prepared according to the following method:
(1) uniformly mixing stearic acid and absolute ethyl alcohol, and then heating the mixture under the condition of constant-temperature water bath until the stearic acid is molten to obtain a wall material precursor body fluid;
(2) adding a core material into the wall material precursor liquid, uniformly stirring, cooling to room temperature, performing reduced pressure evaporation to remove ethanol, and screening the residual solid product to obtain a desorbent sustained-release capsule; in this step, the components of the core material include persulfate and a nucleating agent.
7. The silicone rubber retarder of claim 6, wherein the nucleating agent is bentonite containing water of crystallization.
8. The silicone rubber delay of claim 7, wherein the composition of the core material further comprises calcium acetate.
9. 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 to 8.
10. The manufacturing process of the silicon rubber synthetic leather is characterized by comprising the following steps:
(1) mixing branched vinyl silicone oil, white carbon black and silazane, and then 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 delay agent according to any one of claims 1 to 8 to obtain a silicone rubber mixture;
(2) coating a 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210339104.XA CN114591536B (en) | 2022-04-01 | 2022-04-01 | Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210339104.XA CN114591536B (en) | 2022-04-01 | 2022-04-01 | Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114591536A true CN114591536A (en) | 2022-06-07 |
| CN114591536B CN114591536B (en) | 2024-05-03 |
Family
ID=81811766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210339104.XA Active CN114591536B (en) | 2022-04-01 | 2022-04-01 | Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114591536B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2022
- 2022-04-01 CN CN202210339104.XA patent/CN114591536B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 张自义;: "炔属化合物的自由基加成反应", 兰州大学学报(自然科学版), no. 02 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114591536B (en) | 2024-05-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108586266B (en) | Synthesis process of dimethylamine borane | |
| CN114591536B (en) | Silicon rubber retarder, silicon rubber synthetic leather containing retarder and low-energy-consumption manufacturing process of silicon rubber synthetic leather | |
| CN116375575B (en) | Palladium acetate and preparation method of compound thereof | |
| CN103232364A (en) | Process for producing hydrazone compound | |
| GB2451384A (en) | 2-cyanophenylboronic acid with reduced impurities or ester thereof,and production method thereof | |
| CN105294403A (en) | Preparation process of tert-butylhydroquinone | |
| CN113582821B (en) | Preparation method of 8-methyldecanal | |
| CN105924404B (en) | A kind of preparation method of Ultraviolet Absorber UV-P | |
| CN109865521B (en) | Mixed metal catalyst for preparing tert-butylhydroquinone and preparation method of tert-butylhydroquinone | |
| CN113004124A (en) | Purification method of 3,3 ', 5,5 ' -tetrasubstituted-2, 2 ' -biphenol | |
| CN100420692C (en) | Iridium complex and its synthesis method | |
| CN103709039A (en) | Method for synthesizing methyl (ethyl) gallate through catalysis of Cu-mordenite | |
| JP2007051042A (en) | METHOD FOR PRODUCTION OF HAFNIUM COMPOUND, HAFNIUM COMPOUND WITH IMPURITY Zr OF 50 PPM OR LESS, AND METHOD OF FORMING HAFNIUM-BASED FILM | |
| CN111375417B (en) | Catalyst for preparing high-carbon alcohol by CO hydrogenation and preparation method thereof | |
| CN107382688B (en) | Method for efficiently synthesizing ruthenium tris (acetylacetonate) and application thereof | |
| CN108190858B (en) | Preparation method of graphite fluoride | |
| CN101293857B (en) | Process for preparing diphenyl sulphone formyl paraquinone dioxime | |
| CN108863913B (en) | Method for improving stability of nicotinaldehyde | |
| JP2010524870A (en) | Palladium (0) -dibenzylideneacetone complex | |
| KR20140061434A (en) | Method for producing aluminum alkoxide | |
| CN102977151B (en) | The preparation method of two (tricyclohexyl phosphine) palladium chloride | |
| JP5984624B2 (en) | Extraction method of asymmetric β-diketone compound from β-diketone compound | |
| CN115466255B (en) | Tropine and synthetic method thereof | |
| CN101993468A (en) | Synthesis method for improving dienogest | |
| KR102125041B1 (en) | Method of synthesis of ferrocene derivatives |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |