CN106496717B - A kind of preparation method of uvioresistant rubber antioxidant - Google Patents
A kind of preparation method of uvioresistant rubber antioxidant Download PDFInfo
- Publication number
- CN106496717B CN106496717B CN201610946927.3A CN201610946927A CN106496717B CN 106496717 B CN106496717 B CN 106496717B CN 201610946927 A CN201610946927 A CN 201610946927A CN 106496717 B CN106496717 B CN 106496717B
- Authority
- CN
- China
- Prior art keywords
- rubber
- montmorillonite
- filter residue
- uvioresistant
- wide layer
- 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.)
- Active
Links
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 23
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 41
- 235000006708 antioxidants Nutrition 0.000 claims abstract description 22
- 235000009419 Fagopyrum esculentum Nutrition 0.000 claims abstract description 21
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 20
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 15
- 229930003944 flavone Natural products 0.000 claims abstract description 15
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 15
- 235000011949 flavones Nutrition 0.000 claims abstract description 15
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000005979 Citrus limon Nutrition 0.000 claims abstract description 14
- 244000131522 Citrus pyriformis Species 0.000 claims abstract description 14
- 244000215068 Acacia senegal Species 0.000 claims abstract description 8
- 229920000084 Gum arabic Polymers 0.000 claims abstract description 8
- 239000000205 acacia gum Substances 0.000 claims abstract description 8
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 8
- 240000008620 Fagopyrum esculentum Species 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000000855 fermentation Methods 0.000 claims description 30
- 230000004151 fermentation Effects 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 241000219051 Fagopyrum Species 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 230000010355 oscillation Effects 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 239000002054 inoculum Substances 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 238000000643 oven drying Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 244000063299 Bacillus subtilis Species 0.000 claims description 5
- 235000014469 Bacillus subtilis Nutrition 0.000 claims description 5
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical class C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 9
- 230000003712 anti-aging effect Effects 0.000 abstract description 6
- 230000002929 anti-fatigue Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 244000005700 microbiome Species 0.000 abstract description 3
- 239000007822 coupling agent Substances 0.000 abstract description 2
- 229930003935 flavonoid Natural products 0.000 abstract description 2
- 150000002215 flavonoids Chemical class 0.000 abstract description 2
- 235000017173 flavonoids Nutrition 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 23
- 230000032683 aging Effects 0.000 description 13
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 5
- 238000004108 freeze drying Methods 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000002688 persistence Effects 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000025 natural resin Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of preparation method of uvioresistant rubber antioxidant, belong to rubber antioxidant preparing technical field.The present invention handles montmorillonite by lemon juice, with gum arabic in the presence of microorganism to imvite modified after processing, wide layer montmorillonite must be modified, Flavonoid substances are extracted from bitter buckwheat again, after flavone extract and modified wide layer montmorillonite being reacted in the presence of coupling agent, be made uvioresistant rubber antioxidant.The beneficial effects of the invention are as follows：Preparation process of the present invention is simple, and gained rubber antioxidant has preferable heat endurance and enduring quality；It is good with rubber matrix compatibility after use, there is stronger antifatigue and anti-ultraviolet property, anti-aging efficiency improves 30~32% than traditional age resistor.
Description
Technical field
The present invention relates to a kind of preparation method of uvioresistant rubber antioxidant, belong to rubber antioxidant preparing technical field.
Background technology
Rubber in use, can be by extraneous factor（Such as ozone aging, thermo-oxidative ageing）Influence and aging, cause
Its physical and mechanical properties changes, and rubber is followed the string, and mechanical performance declines, and service life shortens.In order to solve rubber
Problem of aging, it is necessary to suitable adjuvants are added in rubber, to suppress or delaying aging process, are increased the service life, it is this
For preventing that the auxiliary agent of ageing of rubber from being age resistor.Rubber antioxidant be it is a kind of added during rubber production can prolong
Slow ageing of rubber, the chemicals for extending rubber service life.Age resistor yield and kind are occupied first of rubber chemicals.Amine is anti-old
Agent is one of kind of current production rate and dosage maximum because anti ageing property is good, but contains amino in its molecular structure, easily production
Raw carcinogen, and rubber discoloration can be made or occur bloom phenomenon on surface, therefore use and receive certain limitation, because
This investigated a kind of environmentally-frierubber rubber anti-ageing agent.
Environmentally-frierubber rubber anti-ageing agent has phenols, esters, Thiourea, composite environment-friendly age resistor, and phenol antiager is non-discolouring,
Do not pollute, no blooming, be a kind of pollution-free age resistor.Contain hydroxyl in phenol antiager, harmful thing will not be produced
Matter, it can suppress radical reaction, reach the purpose for preventing ageing of rubber.The use in vulcanizate of Phosphorus age resistor will not produce
Environmentally hazardous noxious material, it is a kind of green age resistor, can strengthen the stability of rubber.Rare earth age resistor
Substantial amounts of unoccupied orbital in rare earth element be present, can be combined with caused free radical in oxidizing process, terminate chain reaction, suppress oxidation
The continuation of reaction.Compound age resistor is to be compounded age resistor, using the synergy between component, is sent out to greatest extent
Wave the effect of each age resistor.But current age resistor also has that heat endurance is poor, and anti-aging efficiency is low, and persistence is poor, resist after use
Fatigue and anti-ultraviolet property it is poor, and with rubber matrix poor compatibility problem.
The content of the invention
The technical problems to be solved by the invention：It is poor for current traditional rubber antioxidant heat endurance and persistence, make
With rear antifatigue low with anti-ultraviolet property, and the drawbacks of with rubber matrix poor compatibility, there is provided one kind by lemon juice at
Manage montmorillonite, with gum arabic in the presence of microorganism to imvite modified after processing, wide layer montmorillonite must be modified, then
Flavonoid substances are extracted from bitter buckwheat, after flavone extract and modified wide layer montmorillonite are reacted in the presence of coupling agent,
Uvioresistant rubber antioxidant is made.Present invention utilizes the characteristic of montmorillonite shielding ultraviolet rays, first with citric acid by cheating engaging layer
Between metal cation be transformed into soluble-salt dissolution, so as to weaken its inter-layer bonding force, interlayer lattice is split, interlamellar spacing
Expand, then further increase interlamellar spacing through " ice is split " effect, increase the adsorption capacity and adsorptivity of montmorillonite, then through natural resin
It is modified, natural resin particle is grafted on montmorillonite surface in the presence of microorganism, so as to improve its knot with rubber matrix
Conjunction property, finally there is the bitter buckwheat flavone of inoxidizability using montmorillonite absorption, further increase the ageing resistace of age resistor,
And the age resistor heat endurance prepared by montmorillonite carrier is high, and persistence is strong, antifatigue uvioresistant, has wide application
Prospect.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）Take Fresh Lemon to be squeezed the juice after removing the peel, be filtrated to get lemon juice, lemon juice is centrifuged into 10~15min with centrifuge,
Isolated supernatant, after taking 20~30min of montmorillonite ball mill ball milling, 200 mesh sieves are crossed, sieving powder and supernatant are pressed
Mass ratio is 1:After 5 mixing, it is put into sonic oscillation instrument, 1~2h is impregnated with 200~300W oscillation of powers；
（2）After dipping terminates, filter residue is filtrated to get, handles 1~2min to gained filter residue surface spraying liquid nitrogen frozen immediately,
The filter residue after freezing processing is put into oven drying again, obtains wide layer montmorillonite powder；
（3）It is 1 in mass ratio by above-mentioned wide layer montmorillonite, gum arabic and distilled water:1:After 5 mixing, load fermentation
Fermentation substrate is used as in tank, then bacillus subtilis is accessed into fermentation substrate for 10% by inoculum concentration, is then put into fermentation tank
In 30~40 DEG C of insulating box, heat-preservation fermentation 7~9 days, take out fermentate and filter, filter residue is rinsed 3 repeatedly with deionized water
After~5 times, freeze-drying, wide layer montmorillonite powder must be modified, it is standby；
（4）800~900g bitter buckwheats are weighed, put it into 30~40min of crushing, the crushed material that will be obtained in tissue pulverizer
It is that 70% ethanol solution by quality is 1 with mass fraction:After 5 mixing, pour into reactor, be 0.15~0.25MPa in pressure,
Temperature is at 70~75 DEG C, and 3~5h of stirring reaction, reaction is filtered after terminating, and obtains filtrate；
（5）Above-mentioned filtrate is transferred in cucurbit, ethanol is distilled to recover, obtains bitter buckwheat flavone extract solution, in parts by weight
Meter, weighs 50~60 parts of bitter buckwheat flavone extract solutions, 10~12 parts of dimethyldichlorosilanes, 30~40 parts of deionized waters, fills successively
Enter in reactor, in nitrogen atmosphere, 10~12h of stirring reaction, obtains mixed liquor at 40~50 DEG C；
（6）It is 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor, at 40~45 DEG C
Lower continuation 15~18h of stirring reaction, reaction are filtered after terminating, and obtain filter residue, after being freezed with vacuum freeze-drying machine, produce uvioresistant rubber
Glue age resistor.
The application process of the present invention：Uvioresistant rubber antioxidant produced by the present invention is added in rubber preparing raw material,
It is 0.3~0.8% to control addition, after being uniformly mixed under 200~300r/min, through being kneaded, rolling, being molded and vulcanizing
Rubber is made.Rubber antioxidant of the present invention is good with rubber matrix compatibility, and enduring quality is protected compared with traditional age resistor
50~60% are improved, the rubber as made from age resistor of the present invention has stronger to external interferences such as microwave irradiation, ozone and heat
Inhibitory action, ageing-resistant time extend 3~4 years than traditional rubber.
Compared with other method, advantageous effects are the present invention：
（1）Preparation process of the present invention is simple, and gained rubber antioxidant has preferable heat endurance and enduring quality；
（2）Rubber antioxidant of the present invention is good with rubber matrix compatibility, has stronger antifatigue and uvioresistant after use
Linearly energy, anti-aging efficiency improve 30~32% than traditional age resistor.
Embodiment
Take first Fresh Lemon remove the peel after squeeze the juice, be filtrated to get lemon juice, with centrifuge by lemon juice centrifuge 10~
15min, isolated supernatant, after taking 20~30min of montmorillonite ball mill ball milling, 200 mesh sieves are crossed, will sieving powder and upper
Clear liquid is 1 in mass ratio:After 5 mixing, it is put into sonic oscillation instrument, 1~2h is impregnated with 200~300W oscillation of powers；Dipping knot
Shu Hou, filter residue is filtrated to get, handles 1~2min to gained filter residue surface spraying liquid nitrogen frozen immediately, then by after freezing processing
Filter residue is put into oven drying, obtains wide layer montmorillonite powder；Above-mentioned wide layer montmorillonite, gum arabic and distilled water are pressed into quality
Than for 1:1:After 5 mixing, it is fitted into fermentation tank and is used as fermentation substrate, then withered grass is accessed into fermentation substrate for 10% by inoculum concentration
Bacillus, then fermentation tank is put into 30~40 DEG C of insulating box, heat-preservation fermentation 7~9 days, takes out fermentate and filter,
After filter residue is rinsed into 3~5 times repeatedly with deionized water, freeze-drying, wide layer montmorillonite powder must be modified, it is standby；Then weigh
800~900g bitter buckwheats, 30~40min of crushing in tissue pulverizer is put it into, be 70% by obtained crushed material and mass fraction
Ethanol solution is 1 by quality:After 5 mixing, pour into reactor, be 0.15~0.25MPa in pressure, temperature is 70~75 DEG C
Under, 3~5h of stirring reaction, reaction is filtered after terminating, and obtains filtrate；Above-mentioned filtrate is transferred in cucurbit, is distilled to recover ethanol,
Bitter buckwheat flavone extract solution is obtained, is counted in parts by weight, weighs 50~60 parts of bitter buckwheat flavone extract solutions, 10~12 parts of dimethyl dichloros
Silane, 30~40 parts of deionized waters, are sequentially loaded into reactor, in nitrogen atmosphere, at 40~50 DEG C stirring reaction 10~
12h, obtain mixed liquor；It is finally 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor,
Continue 15~18h of stirring reaction at 40~45 DEG C, reaction is filtered after terminating, and obtains filter residue, after being freezed with vacuum freeze-drying machine, is produced
Uvioresistant rubber antioxidant.
Example 1
Take Fresh Lemon to be squeezed the juice after removing the peel first, be filtrated to get lemon juice, lemon juice is centrifuged into 10min with centrifuge, point
From supernatant is obtained, after taking montmorillonite ball mill ball milling 20min, cross 200 mesh sieves, will sieving powder and supernatant in mass ratio
For 1:After 5 mixing, it is put into sonic oscillation instrument, 1h is impregnated with 200W oscillation of powers；After dipping terminates, filter residue is filtrated to get, is stood
1min is handled to gained filter residue surface spraying liquid nitrogen frozen, then the filter residue after freezing processing is put into oven drying, obtains width
Layer montmorillonite powder；It is 1 in mass ratio by above-mentioned wide layer montmorillonite, gum arabic and distilled water:1:After 5 mixing, load hair
Fermentation substrate is used as in fermentation tank, then bacillus subtilis is accessed into fermentation substrate for 10% by inoculum concentration, then puts fermentation tank
Enter in 30 DEG C of insulating box, heat-preservation fermentation 7 days, take out fermentate and filter, after filter residue is rinsed into 3 times repeatedly with deionized water,
Freeze-drying, must be modified wide layer montmorillonite powder, standby；Then 800g bitter buckwheats are weighed, puts it into tissue pulverizer and crushes
30min, it is that 70% ethanol solution by quality is 1 by obtained crushed material and mass fraction:After 5 mixing, pour into reactor,
Pressure is 0.15MPa, and temperature is at 70 DEG C, and stirring reaction 3h, reaction is filtered after terminating, and obtains filtrate；Above-mentioned filtrate is transferred to
In cucurbit, be distilled to recover ethanol, obtain bitter buckwheat flavone extract solution, count in parts by weight, weigh 50 parts of bitter buckwheat flavone extract solutions,
10 parts of dimethyldichlorosilanes, 30 parts of deionized waters, are sequentially loaded into reactor, in nitrogen atmosphere, are stirred at 40 DEG C anti-
10h is answered, obtains mixed liquor；It is finally 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor,
Continue stirring reaction 15h at 40 DEG C, reaction is filtered after terminating, and obtains filter residue, after being freezed with vacuum freeze-drying machine, produces uvioresistant
Rubber antioxidant.
Uvioresistant rubber antioxidant produced by the present invention is added in rubber preparing raw material, it is 0.3% to control addition,
After being uniformly mixed under 200r/min, rubber is made through being kneaded, rolling, being molded and vulcanizing.Rubber of the present invention is anti-old
Agent is good with rubber matrix compatibility, protects enduring quality to improve 50% compared with traditional age resistor, is made by age resistor of the present invention
Rubber have stronger inhibitory action to external interferences such as microwave irradiation, ozone and heat, the ageing-resistant time prolongs than traditional rubber
Grow 3 years.
Example 2
Take Fresh Lemon to be squeezed the juice after removing the peel first, be filtrated to get lemon juice, lemon juice is centrifuged into 13min with centrifuge, point
From supernatant is obtained, after taking montmorillonite ball mill ball milling 25min, cross 200 mesh sieves, will sieving powder and supernatant in mass ratio
For 1:After 5 mixing, it is put into sonic oscillation instrument, 2h is impregnated with 250W oscillation of powers；After dipping terminates, filter residue is filtrated to get, is stood
2min is handled to gained filter residue surface spraying liquid nitrogen frozen, then the filter residue after freezing processing is put into oven drying, obtains width
Layer montmorillonite powder；It is 1 in mass ratio by above-mentioned wide layer montmorillonite, gum arabic and distilled water:1:After 5 mixing, load hair
Fermentation substrate is used as in fermentation tank, then bacillus subtilis is accessed into fermentation substrate for 10% by inoculum concentration, then puts fermentation tank
Enter in 35 DEG C of insulating box, heat-preservation fermentation 8 days, take out fermentate and filter, after filter residue is rinsed into 4 times repeatedly with deionized water,
Freeze-drying, must be modified wide layer montmorillonite powder, standby；Then 850g bitter buckwheats are weighed, puts it into tissue pulverizer and crushes
35min, it is that 70% ethanol solution by quality is 1 by obtained crushed material and mass fraction:After 5 mixing, pour into reactor,
Pressure is 0.20MPa, and temperature is at 73 DEG C, and stirring reaction 4h, reaction is filtered after terminating, and obtains filtrate；Above-mentioned filtrate is transferred to
In cucurbit, be distilled to recover ethanol, obtain bitter buckwheat flavone extract solution, count in parts by weight, weigh 55 parts of bitter buckwheat flavone extract solutions,
11 parts of dimethyldichlorosilanes, 35 parts of deionized waters, are sequentially loaded into reactor, in nitrogen atmosphere, are stirred at 45 DEG C anti-
11h is answered, obtains mixed liquor；It is finally 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor,
Continue stirring reaction 17h at 43 DEG C, reaction is filtered after terminating, and obtains filter residue, after being freezed with vacuum freeze-drying machine, produces uvioresistant
Rubber antioxidant.
Uvioresistant rubber antioxidant produced by the present invention is added in rubber preparing raw material, it is 0.5% to control addition,
After being uniformly mixed under 250r/min, rubber is made through being kneaded, rolling, being molded and vulcanizing.Rubber of the present invention is anti-old
Agent is good with rubber matrix compatibility, protects enduring quality to improve 55% compared with traditional age resistor, is made by age resistor of the present invention
Rubber have stronger inhibitory action to external interferences such as microwave irradiation, ozone and heat, the ageing-resistant time prolongs than traditional rubber
Grow 4 years.
Example 3
Take Fresh Lemon to be squeezed the juice after removing the peel first, be filtrated to get lemon juice, lemon juice is centrifuged into 15min with centrifuge, point
From supernatant is obtained, after taking montmorillonite ball mill ball milling 30min, cross 200 mesh sieves, will sieving powder and supernatant in mass ratio
For 1:After 5 mixing, it is put into sonic oscillation instrument, 2h is impregnated with 300W oscillation of powers；After dipping terminates, filter residue is filtrated to get, is stood
2min is handled to gained filter residue surface spraying liquid nitrogen frozen, then the filter residue after freezing processing is put into oven drying, obtains width
Layer montmorillonite powder；It is 1 in mass ratio by above-mentioned wide layer montmorillonite, gum arabic and distilled water:1:After 5 mixing, load hair
Fermentation substrate is used as in fermentation tank, then bacillus subtilis is accessed into fermentation substrate for 10% by inoculum concentration, then puts fermentation tank
Enter in 40 DEG C of insulating box, heat-preservation fermentation 9 days, take out fermentate and filter, after filter residue is rinsed into 5 times repeatedly with deionized water,
Freeze-drying, must be modified wide layer montmorillonite powder, standby；Then 900g bitter buckwheats are weighed, puts it into tissue pulverizer and crushes
40min, it is that 70% ethanol solution by quality is 1 by obtained crushed material and mass fraction:After 5 mixing, pour into reactor,
Pressure is 0.25MPa, and temperature is at 75 DEG C, and stirring reaction 5h, reaction is filtered after terminating, and obtains filtrate；Above-mentioned filtrate is transferred to
In cucurbit, be distilled to recover ethanol, obtain bitter buckwheat flavone extract solution, count in parts by weight, weigh 60 parts of bitter buckwheat flavone extract solutions,
12 parts of dimethyldichlorosilanes, 40 parts of deionized waters, are sequentially loaded into reactor, in nitrogen atmosphere, are stirred at 50 DEG C anti-
12h is answered, obtains mixed liquor；It is finally 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor,
Continue stirring reaction 18h at 45 DEG C, reaction is filtered after terminating, and obtains filter residue, after being freezed with vacuum freeze-drying machine, produces uvioresistant
Rubber antioxidant.
Uvioresistant rubber antioxidant produced by the present invention is added in rubber preparing raw material, it is 0.8% to control addition,
After being uniformly mixed under 300r/min, rubber is made through being kneaded, rolling, being molded and vulcanizing.Rubber of the present invention is anti-old
Agent is good with rubber matrix compatibility, protects enduring quality to improve 60% compared with traditional age resistor, is made by age resistor of the present invention
Rubber have stronger inhibitory action to external interferences such as microwave irradiation, ozone and heat, the ageing-resistant time prolongs than traditional rubber
Grow 4 years.
Claims (1)
1. a kind of preparation method of uvioresistant rubber antioxidant, it is characterised in that specifically preparation process is：
（1）Take Fresh Lemon to be squeezed the juice after removing the peel, be filtrated to get lemon juice, lemon juice is centrifuged into 10~15min, separation with centrifuge
Supernatant is obtained, after taking 20~30min of montmorillonite ball mill ball milling, crosses 200 mesh sieves, sieving powder and supernatant are pressed into quality
Than for 1:After 5 mixing, it is put into sonic oscillation instrument, 1~2h is impregnated with 200~300W oscillation of powers；
（2）After dipping terminates, filter residue is filtrated to get, handles 1~2min to gained filter residue surface spraying liquid nitrogen frozen immediately, then will
Filter residue after freezing processing is put into oven drying, obtains wide layer montmorillonite powder；
（3）It is 1 in mass ratio by above-mentioned wide layer montmorillonite, gum arabic and distilled water:1:After 5 mixing, it is fitted into fermentation tank
It is 10% bacillus subtilis to be accessed into fermentation substrate as fermentation substrate, then by inoculum concentration, fermentation tank is then put into 30~
In 40 DEG C of insulating box, heat-preservation fermentation 7~9 days, take out fermentate and filter, filter residue is rinsed 3~5 times repeatedly with deionized water
Afterwards, it is freeze-dried, wide layer montmorillonite powder must be modified, it is standby；
（4）800~900g bitter buckwheats are weighed, 30~40min of crushing in tissue pulverizer are put it into, by obtained crushed material and matter
It is that 70% ethanol solution is 1 in mass ratio to measure fraction:After 5 mixing, pour into reactor, be 0.15~0.25MPa in pressure, temperature
Spend at 70~75 DEG C, 3~5h of stirring reaction, reaction is filtered after terminating, and obtains filtrate；
（5）Above-mentioned filtrate is transferred in cucurbit, ethanol is distilled to recover, obtains bitter buckwheat flavone extract solution, count in parts by weight, is claimed
50~60 parts of bitter buckwheat flavone extract solutions, 10~12 parts of dimethyldichlorosilanes, 30~40 parts of deionized waters are taken, are sequentially loaded into reaction
In kettle, in nitrogen atmosphere, 10~12h of stirring reaction, obtains mixed liquor at 40~50 DEG C；
（6）It is 3 in mass ratio:5, the standby wide layer montmorillonite of modification is added in above-mentioned mixed liquor, at 40~45 DEG C after
15~18h of continuous stirring reaction, reaction are filtered after terminating, and obtain filter residue, after being freezed with vacuum freeze-drying machine, are produced uvioresistant rubber and are prevented
Old agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610946927.3A CN106496717B (en) | 2016-11-02 | 2016-11-02 | A kind of preparation method of uvioresistant rubber antioxidant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610946927.3A CN106496717B (en) | 2016-11-02 | 2016-11-02 | A kind of preparation method of uvioresistant rubber antioxidant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106496717A CN106496717A (en) | 2017-03-15 |
| CN106496717B true CN106496717B (en) | 2017-12-29 |
Family
ID=58322098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610946927.3A Active CN106496717B (en) | 2016-11-02 | 2016-11-02 | A kind of preparation method of uvioresistant rubber antioxidant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106496717B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987027A (en) * | 2017-04-21 | 2017-07-28 | 周荣 | A kind of preparation method of rubber antioxidant |
| CN107459945A (en) * | 2017-07-31 | 2017-12-12 | 常州聚盛节能工程有限公司 | A kind of preparation method of high viscosity starch base paper tube adhesive |
| CN107473345A (en) * | 2017-07-31 | 2017-12-15 | 常州诺澜复合材料有限公司 | A kind of preparation method of composite algicide |
| CN108102074A (en) * | 2017-12-30 | 2018-06-01 | 常州文诺纺织品有限公司 | A kind of preparation method of heat radiating type slow-recovery sponge |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101449852A (en) * | 2007-12-01 | 2009-06-10 | 孙晓靖 | Tartary buckwheat husking and kernel-husk separation processing technique |
| CN105670160A (en) * | 2015-10-12 | 2016-06-15 | 陆思烨 | Anti-UV and anti-aging electric wire cable material and preparation method thereof |
| CN105906992A (en) * | 2016-06-24 | 2016-08-31 | 浙江英美达电缆科技有限公司 | Flame retardant long-term ultraviolet aging resistant steel-tape armoured aluminium alloy power cable |
| CN105924855A (en) * | 2016-06-24 | 2016-09-07 | 浙江英美达电缆科技有限公司 | Aluminum alloy electric wire resistant to ultraviolet aging |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140114231A1 (en) * | 2012-10-20 | 2014-04-24 | Bertha Rostro | Formulations and Compositions of Hydrophobic Extracts of Skin Tree |
-
2016
- 2016-11-02 CN CN201610946927.3A patent/CN106496717B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101449852A (en) * | 2007-12-01 | 2009-06-10 | 孙晓靖 | Tartary buckwheat husking and kernel-husk separation processing technique |
| CN105670160A (en) * | 2015-10-12 | 2016-06-15 | 陆思烨 | Anti-UV and anti-aging electric wire cable material and preparation method thereof |
| CN105906992A (en) * | 2016-06-24 | 2016-08-31 | 浙江英美达电缆科技有限公司 | Flame retardant long-term ultraviolet aging resistant steel-tape armoured aluminium alloy power cable |
| CN105924855A (en) * | 2016-06-24 | 2016-09-07 | 浙江英美达电缆科技有限公司 | Aluminum alloy electric wire resistant to ultraviolet aging |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106496717A (en) | 2017-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106496717B (en) | A kind of preparation method of uvioresistant rubber antioxidant | |
| CN104585563B (en) | It is a kind of to utilize the method for compounding heavy metal cadmium in lactobacillus-fermented removing rice | |
| CN102614834B (en) | Method for adsorbing and recovering heavy metals of lead and copper by persimmon tannin-containing metal adsorbent | |
| CN104987040A (en) | Ceramic vessel capable of activating water molecules and preparation method of ceramic vessel | |
| CN103920013A (en) | Preparation method of dendrobium officinale ultramicro wall-broken powder | |
| CN104305450A (en) | Polygonatum sibiricum beverage and novel method for producing same | |
| CN102115611A (en) | Method for performing steam explosion on chestnut hulls and coproducing pigment, tanning extract and active carbon | |
| CN107629537A (en) | A kind of processing method of pump paint filler | |
| KR101189482B1 (en) | Manufacturing method of soybean paste containing helianthus tuberosus | |
| CN109233285A (en) | A kind of waste silicone rubber cracking recycling and reusing method | |
| CN103462140B (en) | Low frequency ultrasonic-assisted desugaring and deacidification method for concentrated waxberry juice | |
| CN104944910A (en) | Ageing cracking resistant ceramic bowl and preparation method thereof | |
| CN102212219B (en) | Rice-husk-based carbon/silicon composite used as rubber filler and preparation method thereof | |
| CN106044980B (en) | A kind of compound water body fungicide | |
| JP2013118855A (en) | Crushed garlic, active oxygen scavenger and method for producing crushed garlic | |
| CN109880189A (en) | A kind of instrument and equipment rubber vibration isolation cushion material | |
| CN104172347A (en) | Processing method of dark grape juice | |
| CN104987051A (en) | Antibacterial and bactericidal ceramic bowl and preparation method thereof | |
| CN108553498A (en) | A kind of saussurea involucrata essence extraction process | |
| CN108912243B (en) | Process for extracting pectin from kiwi fruit peel residues | |
| CN107442107A (en) | A kind of manganese dioxide anionic clay composite and preparation method and application | |
| CN102599563B (en) | Walnut granule processing technology | |
| CN1245088C (en) | Gulfweed bag tea processing art | |
| CN101417002A (en) | Red clover fresh grass pre-processing method | |
| KR101185822B1 (en) | Method for preparing powder of wormwood |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Cong Guiyang Inventor before: Wu Rongrong Inventor before: Zou Yufan Inventor before: Zhang Jing |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20171123 Address after: 523872 Guangdong Province, Dongguan city Changan town Xiagang community Zhenxi No. 9 building ZC09 Applicant after: Top plastic industrial (Guangdong) Co., Ltd. Address before: 213164 Changzhou City, Jiangsu Province, Wujin, the Middle East Road, No. 801, Changzhou science and technology city church hall B block, 2519 Applicant before: TRUSYN CHEM-TECH CO., LTD. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180123 Address after: No. 10, Xi Yuan Road, Tianmu Lake Industrial Park, Liyang City, Changzhou, Jiangsu Patentee after: Jiangsu Top Polymer Enterprise Limited Address before: 523872 Guangdong Province, Dongguan city Changan town Xiagang community Zhenxi No. 9 building ZC09 Patentee before: Top plastic industrial (Guangdong) Co., Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190314 Address after: 523000 ZC09 Building, Zhenxi 9, Xiagang Community, Chang'an Town, Dongguan City, Guangdong Province Patentee after: Top plastic industrial (Guangdong) Co., Ltd. Address before: 213333 No. 10 Xiyuan Road, Tianmuhu Industrial Park, Liyang City, Changzhou City, Jiangsu Province Patentee before: Jiangsu Top Polymer Enterprise Limited |