CN110408082A - A kind of preparation method of rubber softener used additives - Google Patents
A kind of preparation method of rubber softener used additives Download PDFInfo
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- CN110408082A CN110408082A CN201910539885.5A CN201910539885A CN110408082A CN 110408082 A CN110408082 A CN 110408082A CN 201910539885 A CN201910539885 A CN 201910539885A CN 110408082 A CN110408082 A CN 110408082A
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- used additives
- rubber softener
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 70
- 239000005060 rubber Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000000654 additive Substances 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 58
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 230000003213 activating effect Effects 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000002893 slag Substances 0.000 claims abstract description 10
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- 239000000203 mixture Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical class C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 12
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 12
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 12
- 239000012046 mixed solvent Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 12
- 238000002390 rotary evaporation Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 235000011037 adipic acid Nutrition 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 241000207199 Citrus Species 0.000 claims description 6
- 244000236655 Diospyros kaki Species 0.000 claims description 6
- 235000008597 Diospyros kaki Nutrition 0.000 claims description 6
- 241000196324 Embryophyta Species 0.000 claims description 6
- 150000001279 adipic acids Chemical class 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000020971 citrus fruits Nutrition 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 6
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- -1 hexamethylene diamines Chemical class 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 230000009514 concussion Effects 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims 1
- 150000002460 imidazoles Chemical group 0.000 claims 1
- 239000004902 Softening Agent Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 5
- 229910021536 Zeolite Inorganic materials 0.000 abstract description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000010457 zeolite Substances 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N 1H-imidazole Chemical group C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 15
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 5
- 239000001361 adipic acid Substances 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 5
- 239000011280 coal tar Substances 0.000 description 5
- 239000012975 dibutyltin dilaurate Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 4
- 241000018646 Pinus brutia Species 0.000 description 3
- 125000002252 acyl group Chemical group 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 229920000126 latex Polymers 0.000 description 3
- 239000004816 latex Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000011297 pine tar Substances 0.000 description 2
- 229940068124 pine tar Drugs 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005183 environmental health Effects 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 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
- C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
- C08K11/005—Waste materials, e.g. treated or untreated sewage sludge
-
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/08—Ingredients of unknown constitution and ingredients covered by the main groups C08K3/00 - C08K9/00
-
- 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
- C08K3/16—Halogen-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
- C08K3/28—Nitrogen-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
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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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
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to rubber chemicals technical fields, and in particular to a kind of preparation method of rubber softener used additives.The present invention passes through using blast furnace slag, kaolin and diatomite as raw material, pass through the effect using sodium hydroxide, form class zeolite molecules sieve structure, and magnetic texure is contained in inside, then mixed by its modifying agent, it is grafted by modification, then the polymer in modifying agent is modified by activating agent, it is set to carry out active group, finally mixed with natural extract, to form rubber softener used additives, solves the problem of current existing softening agent bating effect is bad, and softening agent is easily moved out.
Description
Technical field
The invention belongs to rubber chemicals technical fields, and in particular to a kind of preparation method of rubber softener used additives.
Background technique
Rubber industry is one of important foundation industry of national economy.Rubber not only for people provide daily life can not or
The scarce light industrys rubber product such as daily, medical, and to the heavy industry such as digging, traffic, building, machinery, electronics and new industry
Various rubber system production equipments or rubber components are provided.As it can be seen that the product category of rubber industry is various, prospect is very wide.
Rubber is divided into natural rubber and synthetic rubber by raw material；It is divided into blocky raw rubber, latex, liquid rubber and powder rubber end rubber by form
Glue.Latex is the colloidal aqueous dispersion of rubber；Liquid rubber is the oligomer of rubber, generally sticky liquid before unvulcanized
Body；Powdered rubber be latex is processed into it is powdered, with sharp ingredient and processing and fabricating.The thermoplasticity rubber of exploitation the 1960s
Glue is not necessarily to chemical cure, and the processing method for using thermoplastic shapes.Rubber is by using and be divided into universal and Special type
Two classes.
Softening agent is very important auxiliary agent in a kind of reclaimed rubber production, is convenient for the calendering and molding of reclaimed rubber,
And facilitate other auxiliary agents and be scattered in reclaimed rubber, rubber kneading temperature is reduced, the flow temperature and glass of rubber are lowered
Change temperature, improves the resistance to low temperature of rubber.Currently, the softening agent used is mostly coal tar system softening agent, feature is exactly soft
It is good to change effect, it is at low cost.But coal tar system softening agent will affect workers ' health and endanger Environmental Health, and use coal tar
The reclaimed rubber of oil system softening agent production, harmful substance contents are big.The main function of rubber softener is that rubber is made to divide chain greatly
Between active force reduce, sizing material it is easy to process and improve clothes material certain performances.
Rubber must use softening agent in process, in the past rubber softening used in tyre industry at home and abroad
Agent is mainly aromatic naphtha (DAE).Since aromatic naphtha (DAE) contains a large amount of condensed-nuclei aromatics (being also polycyclic aromatic hydrocarbon), and aromatic naphtha
Use in tire technical process can make to contain condensed-nuclei aromatics in tire.Condensed-nuclei aromatics has been shown to have biggish toxicity.
Eco-toxicity and the environmental science committee (CSTEE), which have had proven to many substances contained in condensed-nuclei aromatics, has significant cause
Carcinous, mutagenicity and reproductive system toxic.For rubber product containing aromatic naphtha during by use, condensed-nuclei aromatics is just
Inevitably be diffused into environment and and human contact, thus jeopardize human health and poison environment.
Rubber softener mainly includes the petroleum as composed by alkane, cycloalkane, aromatic hydrocarbons；Include by coal coking
The mineral oil system of the compositions such as coal tar, coumarone indene resin and coal tar pitch；The product obtained by plant pine tree, as pine tar, rosin,
The Pine plants oil system three categories of the compositions such as tall oil.The poisonous and harmful problem of its Minerals coal tar system is larger, usage amount by
It is decrescence few.Pine tar is smaller and smaller due to the exhaustion of raw materials for production pine stump and the rise application amount of rosin price.Petroleum Production
Softening agent is main rubber softener to be applied in current rubber industry, and the most commonly used with aromatic naphtha softening agent.Aromatic naphtha comes
Derived from the petroleum for non-renewable resources, resource is not also rich in the long term.Traditional mainstay produces aromatic naphtha, due in base
Containing there is more carcinogenic polycyclic aromatic hydrocarbon compounds to human body.Traditional rubber softener, due to production technology complexity, bating effect is not
It is good, and softening agent is easily moved out, affect in rubber product the extensive use in especially tire.
Summary of the invention
The technical problems to be solved by the invention: bad for current existing softening agent bating effect, softening agent is easily moved out
The problem of, the present invention provides a kind of preparation methods of rubber softener used additives.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of rubber softener used additives, the preparation method include the following steps:
(1) hybrid particles, pretreating agent 1:4~6 in mass ratio are taken to be uniformly mixed, ultrasonic vibration, filtering is collected filter residue, will be filtered
Slag, mixed molysite solution 7:15~18 in mass ratio are uniformly mixed, and adjust pH to 9.0~9.5 using sodium hydroxide solution, quiet
It sets；
(2) after standing, the ammonium hydroxide of filter residue quality 10~15% is added, stirs evenly, is put into reaction kettle, nitrogen is protected
Shield, is warming up to 90~95 DEG C, boosts to 1.3~1.5MPa, stirs, is cooled to room temperature, and discharges, collects out material, filters, washes
It washs, is freeze-dried, collect dried object；
(3) dried object, modifying agent and extract 7~9:2:7~10 in mass ratio are mixed, collects mixture, will mixes
Object is put into reactor, is added 6~9 times of dried object quality of toluene, is stirred evenly, preheating；
(4) after wait preheat, the formaldehyde of dried object quality 10~15%, the morpholine of dried object quality 4~7% is added, heats up,
Stirring heat preservation, cooling discharging, evaporative removal solvent, washing are dry to get rubber softener used additives.
Hybrid particles are blast furnace slag, kaolin and diatomite 1:5~7:2 in mass ratio mixing in the step (1), are ground
Mill is to get mixture.
In the step (1) pretreating agent the preparation method comprises the following steps: by sodium hexametaphosphate, triethylamine and water in mass ratio 1:
1:14~16 mix.
Mixed molysite is that frerrous chloride, ferric nitrate and water 4:2~4:20 in mass ratio are mixed in the step (1).
In the step (3) modifying agent be according to parts by weight, take 80~90 parts of tetrahydrofurans, 30~40 parts of adipic acids,
25~28 parts of hexamethylene diamines, 18~33 parts of caprolactams, 18~29 portions of activating agents, 15~17 parts of ethylene glycol, 4~8 parts of polyethylene glycol
And 3~6 parts of catalyst, adipic acid, hexamethylene diamine, caprolactam, ethylene glycol and catalyst are put into reaction kettle first, added
Heat, cooling, adds tetrahydrofuran, activating agent, polyethylene glycol, is stirred to react, and discharges, rotary evaporation, collection residue, and with
Methanol 1:6 in mass ratio~8 mixing is stood, filtering, collects filter residue to get modifying agent.
The activating agent is glyoxaline cation glycol.
The catalyst be dibutyl tin dilaurate, butyl titanate by etc. mass ratioes mixed.
In the step (3) extract the preparation method comprises the following steps: will extract raw material, mixed solvent 4:7 in mass ratio~9 carry out
Mixing, concussion heating, is filtered while hot, collects filtrate, and rotary evaporation collects residue to get extract.
The mixed plant particle is citrus, Pericarpium Kaki 7:5~9 in mass ratio mix.
The mixed solvent is that 4:1~3 mix by volume for alcohol solvent and acetone.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is by by the effect using sodium hydroxide, forming using blast furnace slag, kaolin and diatomite as raw material
Class zeolite molecules sieve structure, and magnetic texure is contained in inside, then mixes by its modifying agent, by it is modified to its into
Row grafting, then the polymer in modifying agent is modified by activating agent, make its progress active group, finally with naturally mention
Object is taken to be mixed, to form rubber softener used additives；
(2) present invention in use, by class zeolite molecular sieve structural load magnetic-particle, can be effectively catalyzed in rubber
Portion carries out desulfurization, improves bating effect, and internal crystallization water during particles by heat is distributed, and expansion destroys it
In sulfide linkage, secondly the and combination degree of the enhancing particle and storeroom by the polymer of particle surface utilizes or poly-
The competition for closing object and sulfide linkage further destroys internal structure, enhances bating effect.
Specific embodiment
Hybrid particles are blast furnace slag, kaolin and diatomite 1:5~7:2 in mass ratio mixing, are milled with 800r/min
30min is to get mixture.
Pretreating agent the preparation method comprises the following steps: sodium hexametaphosphate, triethylamine are mixed with water 1:1:14~16 in mass ratio
It forms.
Mixed molysite is that frerrous chloride, ferric nitrate and water 4:2~4:20 in mass ratio are mixed.
Modifying agent be according to parts by weight, take 80~90 parts of tetrahydrofurans, 30~40 parts of adipic acids, 25~28 parts oneself two
Amine, 18~33 parts of caprolactams, 18~29 portions of activating agents, 15~17 parts of ethylene glycol, 4~8 parts of polyethylene glycol and 3~6 parts of catalysis
Adipic acid, hexamethylene diamine, caprolactam, ethylene glycol and catalyst are put into reaction kettle by agent first, are carried out being heated to 220 DEG C, be protected
Warm 7h is cooled to 40 DEG C, adds tetrahydrofuran, activating agent, polyethylene glycol, is stirred to react 8h, discharging, and rotary evaporation is collected
Residue, and mixed with methanol 1:6~8 in mass ratio and stand 10h, filtering collects filter residue to get modifying agent.
The activating agent is glyoxaline cation glycol.
Catalyst be dibutyl tin dilaurate, butyl titanate by etc. mass ratioes mixed.
Mixing the preparation method comprises the following steps: raw material, mixed solvent 4:7~9 in mass ratio will be extracted for extract, shakes at 90 DEG C
Heating 2h is swung, is filtered while hot, filtrate is collected, rotary evaporation collects residue to get extract.
Mixed plant particle is citrus, Pericarpium Kaki 7:5~9 in mass ratio mix.
Mixed solvent is that 4:1~3 mix by volume for 1.1mol/L alcohol solvent and acetone.
A kind of preparation method of rubber softener used additives, the preparation method include the following steps:
(1) hybrid particles, pretreating agent 1:4~6 in mass ratio is taken to be uniformly mixed, filter residue is collected in ultrasonic vibration 20min, filtering,
Filter residue, mixed molysite solution 7:15~18 in mass ratio are uniformly mixed, adjust pH to 9.0~9.5 using sodium hydroxide solution,
Stand 6h；
(2) after standing, the 0.6mol/L ammonium hydroxide of filter residue quality 10~15% is added, stirs evenly, is put into reaction kettle,
Nitrogen protection is warming up to 90~95 DEG C, boosts to 1.3~1.5MPa, stirs 7h, is cooled to room temperature, and discharges, collects out material,
Filtering, using water washing, dried object is collected in freeze-drying；
(3) dried object, modifying agent and extract 7~9:2:7~10 in mass ratio are mixed, collects mixture, will mixes
Object is put into reactor, is added 6~9 times of dried object quality of toluene, is stirred evenly, in 60 DEG C of preheating 40min；
(4) after wait preheat, the formaldehyde of dried object quality 10~15%, the morpholine of dried object quality 4~7%, heating is added
To 150 DEG C, stirring heat preservation 8h, cooling discharging, evaporative removal solvent, ethanol washing, drying is to get rubber softener used additives.
Embodiment 1
Hybrid particles be blast furnace slag, kaolin and diatomite 1:5:2 in mass ratio mixing, with 800r/min mill 30min to get
Mixture.
Pretreating agent the preparation method comprises the following steps: sodium hexametaphosphate, triethylamine and water 1:1:14 in mass ratio are mixed.
Mixed molysite is that frerrous chloride, ferric nitrate and water 4:2:20 in mass ratio are mixed.
Modifying agent is according to parts by weight, to take 80 parts of tetrahydrofurans, 30 parts of adipic acids, 25 parts of hexamethylene diamines, 18 parts of acyls in oneself
Amine, 18 portions of activating agents, 15 parts of ethylene glycol, 4 parts of polyethylene glycol and 3 parts of catalyst, first by adipic acid, hexamethylene diamine, caprolactam,
Ethylene glycol and catalyst are put into reaction kettle, be heated to 220 DEG C, are kept the temperature 7h, are cooled to 40 DEG C, add tetrahydrofuran,
Activating agent, polyethylene glycol are stirred to react 8h, discharging, and rotary evaporation collects residue, and mixes with methanol 1:6 in mass ratio quiet
10h is set, is filtered, collects filter residue to get modifying agent.
The activating agent is glyoxaline cation glycol.
Catalyst be dibutyl tin dilaurate, butyl titanate by etc. mass ratioes mixed.
Mixing the preparation method comprises the following steps: raw material, mixed solvent 4:7 in mass ratio will be extracted for extract, shakes at 90 DEG C
2h is heated, is filtered while hot, filtrate is collected, rotary evaporation collects residue to get extract.
Mixed plant particle is citrus, Pericarpium Kaki 7:5 in mass ratio is mixed.
Mixed solvent is that 4:1 is mixed by volume for 1.1mol/L alcohol solvent and acetone.
A kind of preparation method of rubber softener used additives, the preparation method include the following steps:
(1) hybrid particles, pretreating agent 1:4 in mass ratio is taken to be uniformly mixed, filter residue is collected in ultrasonic vibration 20min, filtering, will
Filter residue, mixed molysite solution 7:15 in mass ratio are uniformly mixed, and are adjusted pH to 9.0 using sodium hydroxide solution, are stood 6h；
(2) after standing, the 0.6mol/L ammonium hydroxide of filter residue quality 10% is added, stirs evenly, is put into reaction kettle, nitrogen
Protection, is warming up to 90 DEG C, boosts to 1.3MPa, stirs 7h, is cooled to room temperature, and discharges, collects out material, filters, uses washing
It washs, is freeze-dried, collect dried object；
(3) dried object, modifying agent and extract 7:2:7 in mass ratio are mixed, collects mixture, mixture is put into instead
It answers in device, adds 6 times of dried object quality of toluene, stir evenly, in 60 DEG C of preheating 40min；
(4) after wait preheat, the formaldehyde of dried object quality 10%, the morpholine of dried object quality 4% is added, is warming up to 150 DEG C,
Stirring heat preservation 8h, cooling discharging, evaporative removal solvent, ethanol washing are dry to get rubber softener used additives.
Embodiment 2
Hybrid particles be blast furnace slag, kaolin and diatomite 1:6:2 in mass ratio mixing, with 800r/min mill 30min to get
Mixture.
Pretreating agent the preparation method comprises the following steps: sodium hexametaphosphate, triethylamine and water 1:1:15 in mass ratio are mixed.
Mixed molysite is that frerrous chloride, ferric nitrate and water 4:3:20 in mass ratio are mixed.
Modifying agent is according to parts by weight, to take 85 parts of tetrahydrofurans, 35 parts of adipic acids, 26 parts of hexamethylene diamines, 25 parts of acyls in oneself
Amine, 23 portions of activating agents, 16 parts of ethylene glycol, 6 parts of polyethylene glycol and 5 parts of catalyst, first by adipic acid, hexamethylene diamine, caprolactam,
Ethylene glycol and catalyst are put into reaction kettle, be heated to 220 DEG C, are kept the temperature 7h, are cooled to 40 DEG C, add tetrahydrofuran,
Activating agent, polyethylene glycol are stirred to react 8h, discharging, and rotary evaporation collects residue, and mixes with methanol 1:7 in mass ratio quiet
10h is set, is filtered, collects filter residue to get modifying agent.
The activating agent is glyoxaline cation glycol.
Catalyst be dibutyl tin dilaurate, butyl titanate by etc. mass ratioes mixed.
Mixing the preparation method comprises the following steps: raw material, mixed solvent 4:8 in mass ratio will be extracted for extract, shakes at 90 DEG C
2h is heated, is filtered while hot, filtrate is collected, rotary evaporation collects residue to get extract.
Mixed plant particle is citrus, Pericarpium Kaki 7:7 in mass ratio is mixed.
Mixed solvent is that 4:2 is mixed by volume for 1.1mol/L alcohol solvent and acetone.
A kind of preparation method of rubber softener used additives, the preparation method include the following steps:
(1) hybrid particles, pretreating agent 1:5 in mass ratio is taken to be uniformly mixed, filter residue is collected in ultrasonic vibration 20min, filtering, will
Filter residue, mixed molysite solution 7:17 in mass ratio are uniformly mixed, and are adjusted pH to 9.2 using sodium hydroxide solution, are stood 6h；
(2) after standing, the 0.6mol/L ammonium hydroxide of filter residue quality 13% is added, stirs evenly, is put into reaction kettle, nitrogen
Protection, is warming up to 93 DEG C, boosts to 1.4MPa, stirs 7h, is cooled to room temperature, and discharges, collects out material, filters, uses washing
It washs, is freeze-dried, collect dried object；
(3) dried object, modifying agent and extract 8:2:9 in mass ratio are mixed, collects mixture, mixture is put into instead
It answers in device, adds 8 times of dried object quality of toluene, stir evenly, in 60 DEG C of preheating 40min；
(4) after wait preheat, the formaldehyde of dried object quality 12%, the morpholine of dried object quality 5% is added, is warming up to 150 DEG C,
Stirring heat preservation 8h, cooling discharging, evaporative removal solvent, ethanol washing are dry to get rubber softener used additives.
Embodiment 3
Hybrid particles be blast furnace slag, kaolin and diatomite 1:7:2 in mass ratio mixing, with 800r/min mill 30min to get
Mixture.
Pretreating agent the preparation method comprises the following steps: sodium hexametaphosphate, triethylamine and water 1:1:16 in mass ratio are mixed.
Mixed molysite is that frerrous chloride, ferric nitrate and water 4:4:20 in mass ratio are mixed.
Modifying agent is according to parts by weight, to take 90 parts of tetrahydrofurans, 40 parts of adipic acids, 28 parts of hexamethylene diamines, 33 parts of acyls in oneself
Amine, 29 portions of activating agents, 17 parts of ethylene glycol, 8 parts of polyethylene glycol and 6 parts of catalyst, first by adipic acid, hexamethylene diamine, caprolactam,
Ethylene glycol and catalyst are put into reaction kettle, be heated to 220 DEG C, are kept the temperature 7h, are cooled to 40 DEG C, add tetrahydrofuran,
Activating agent, polyethylene glycol are stirred to react 8h, discharging, and rotary evaporation collects residue, and mixes with methanol 1:8 in mass ratio quiet
10h is set, is filtered, collects filter residue to get modifying agent.
The activating agent is glyoxaline cation glycol.
Catalyst be dibutyl tin dilaurate, butyl titanate by etc. mass ratioes mixed.
Mixing the preparation method comprises the following steps: raw material, mixed solvent 4:9 in mass ratio will be extracted for extract, shakes at 90 DEG C
2h is heated, is filtered while hot, filtrate is collected, rotary evaporation collects residue to get extract.
Mixed plant particle is citrus, Pericarpium Kaki 7:9 in mass ratio is mixed.
Mixed solvent is that 4:3 is mixed by volume for 1.1mol/L alcohol solvent and acetone.
A kind of preparation method of rubber softener used additives, the preparation method include the following steps:
(1) hybrid particles, pretreating agent 1:6 in mass ratio is taken to be uniformly mixed, filter residue is collected in ultrasonic vibration 20min, filtering, will
Filter residue, mixed molysite solution 7:18 in mass ratio are uniformly mixed, and are adjusted pH to 9.5 using sodium hydroxide solution, are stood 6h；
(2) after standing, the 0.6mol/L ammonium hydroxide of filter residue quality 15% is added, stirs evenly, is put into reaction kettle, nitrogen
Protection, is warming up to 95 DEG C, boosts to 1.5MPa, stirs 7h, is cooled to room temperature, and discharges, collects out material, filters, uses washing
It washs, is freeze-dried, collect dried object；
(3) dried object, modifying agent and extract 9:2:10 in mass ratio are mixed, collects mixture, mixture is put into
In reactor, 9 times of dried object quality of toluene is added, is stirred evenly, in 60 DEG C of preheating 40min；
(4) after wait preheat, the formaldehyde of dried object quality 15%, the morpholine of dried object quality 7% is added, is warming up to 150 DEG C,
Stirring heat preservation 8h, cooling discharging, evaporative removal solvent, ethanol washing are dry to get rubber softener used additives.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking pretreating agent.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking extract.
Comparative example 3: the rubber softener of Wuxi City company production.
Embodiment 1,2,3 and comparative example 1,2 gained rubber softener used additives are added to traditional rubber softening of comparative example 3
In agent, additional amount is 1% ~ 2%, is tested according still further to GB/T529-1999, GB/T528-2009, test result is as shown in table 1:
Table 1:
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Fracture tensile strength MPa | 9.37 | 9.25 | 8.96 | 8.51 | 7.92 | 7.35 |
| Elongation at break % | 327 | 312 | 310 | 305 | 302 | 295 |
| Tearing strength MPa | 315 | 356 | 398 | 426 | 495 | 540 |
| Viscosity mm2/s | 65 | 60 | 52 | 50 | 45 | 40 |
| It moves out situation | It is not easy to move out | It is not easy to move out | It is not easy to move out | It is not easy to move out | Easily move out | Easily move out |
| Density g/cm3 | 1.1035 | 1.0952 | 1.0826 | 0.9542 | 0.8236 | 0.7821 |
In summary, the bating effect of the resulting rubber softener used additives of the present invention is preferable, the rubber performance of production more preferably, rubber
Glue product quality is higher.It is more preferable compared to commercial product effect, it is worth promoting.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of rubber softener used additives, which is characterized in that the preparation method includes the following steps:
(1) hybrid particles, pretreating agent 1:4~6 in mass ratio are taken to be uniformly mixed, ultrasonic vibration, filtering is collected filter residue, will be filtered
Slag, mixed molysite solution 7:15~18 in mass ratio are uniformly mixed, and adjust pH to 9.0~9.5 using sodium hydroxide solution, quiet
It sets；
(2) after standing, the ammonium hydroxide of filter residue quality 10~15% is added, stirs evenly, is put into reaction kettle, nitrogen is protected
Shield, is warming up to 90~95 DEG C, boosts to 1.3~1.5MPa, stirs, is cooled to room temperature, and discharges, collects out material, filters, washes
It washs, is freeze-dried, collect dried object；
(3) dried object, modifying agent and extract 7~9:2:7~10 in mass ratio are mixed, collects mixture, will mixes
Object is put into reactor, is added 6~9 times of dried object quality of toluene, is stirred evenly, preheating；
(4) after wait preheat, the formaldehyde of dried object quality 10~15%, the morpholine of dried object quality 4~7% is added, heats up,
Stirring heat preservation, cooling discharging, evaporative removal solvent, washing are dry to get rubber softener used additives.
2. the preparation method of rubber softener used additives according to claim 1, which is characterized in that mixed in the step (1)
Conjunction particle is blast furnace slag, kaolin and diatomite 1:5~7:2 in mass ratio mixing, is milled to get mixture.
3. the preparation method of rubber softener used additives according to claim 1, which is characterized in that pre- in the step (1)
Inorganic agent the preparation method comprises the following steps: sodium hexametaphosphate, triethylamine and water 1:1:14~16 in mass ratio are mixed.
4. the preparation method of rubber softener used additives according to claim 1, which is characterized in that mixed in the step (1)
Conjunction molysite is that frerrous chloride, ferric nitrate and water 4:2~4:20 in mass ratio are mixed.
5. the preparation method of rubber softener used additives according to claim 1, which is characterized in that change in the step (3)
Property agent be according to parts by weight, take 80~90 parts of tetrahydrofurans, 30~40 parts of adipic acids, 25~28 parts of hexamethylene diamines, 18~33 parts
Caprolactam, 18~29 portions of activating agents, 15~17 parts of ethylene glycol, 4~8 parts of polyethylene glycol and 3~6 parts of catalyst, first by oneself
Diacid, hexamethylene diamine, caprolactam, ethylene glycol and catalyst are put into reaction kettle, are heated, cooling, add tetrahydrofuran,
Activating agent, polyethylene glycol, are stirred to react, and discharging, rotary evaporation is collected residue, and mixed with methanol 1:6~8 in mass ratio
It stands, filtering, collects filter residue to get modifying agent.
6. the preparation method of rubber softener used additives according to claim 5, which is characterized in that the activating agent is imidazoles
Cationic glycol.
7. the preparation method of rubber softener used additives according to claim 5, which is characterized in that the catalyst is February
Dilaurylate, butyl titanate by etc. mass ratioes mixed.
8. the preparation method of rubber softener used additives according to claim 1, which is characterized in that mentioned in the step (3)
Take object the preparation method comprises the following steps: raw material will be extracted, mixed solvent 4:7~9 in mass ratio mix, concussion heating is filtered while hot,
Filtrate is collected, rotary evaporation collects residue to get extract.
9. the preparation method of rubber softener used additives according to claim 8, which is characterized in that the mixed plant particle
It is mixed for citrus, Pericarpium Kaki 7:5~9 in mass ratio.
10. the preparation method of rubber softener used additives according to claim 8, which is characterized in that the mixed solvent is
4:1~3 mix by volume for alcohol solvent and acetone.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221006A (en) * | 1998-09-28 | 1999-06-30 | 何允吉 | Compound assistant for rubber |
| CN106279843A (en) * | 2016-08-29 | 2017-01-04 | 宁波江东甬风工业设计有限公司 | A kind of preparation method of the good RX of the compatibility |
| US20180298235A1 (en) * | 2017-04-18 | 2018-10-18 | Yuh-Jye Uang | Method For Bonding Rubber and Ethylene-Vinyl Acetate (EVA) Foam |
| CN109054406A (en) * | 2018-06-26 | 2018-12-21 | 常州市蓝勖化工有限公司 | A kind of rubber softener |
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2019
- 2019-06-21 CN CN201910539885.5A patent/CN110408082B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221006A (en) * | 1998-09-28 | 1999-06-30 | 何允吉 | Compound assistant for rubber |
| CN106279843A (en) * | 2016-08-29 | 2017-01-04 | 宁波江东甬风工业设计有限公司 | A kind of preparation method of the good RX of the compatibility |
| US20180298235A1 (en) * | 2017-04-18 | 2018-10-18 | Yuh-Jye Uang | Method For Bonding Rubber and Ethylene-Vinyl Acetate (EVA) Foam |
| CN109054406A (en) * | 2018-06-26 | 2018-12-21 | 常州市蓝勖化工有限公司 | A kind of rubber softener |
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