CN108485706A - A kind of preparation method of oxidation inert type paraffin - Google Patents
A kind of preparation method of oxidation inert type paraffin Download PDFInfo
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- CN108485706A CN108485706A CN201810290327.5A CN201810290327A CN108485706A CN 108485706 A CN108485706 A CN 108485706A CN 201810290327 A CN201810290327 A CN 201810290327A CN 108485706 A CN108485706 A CN 108485706A
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- 239000012188 paraffin wax Substances 0.000 title claims abstract description 59
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 32
- 230000003647 oxidation Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003921 oil Substances 0.000 claims abstract description 43
- 235000019198 oils Nutrition 0.000 claims abstract description 43
- 230000004913 activation Effects 0.000 claims abstract description 15
- 235000019271 petrolatum Nutrition 0.000 claims abstract description 14
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 12
- 239000003549 soybean oil Substances 0.000 claims abstract description 12
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 239000000843 powder Substances 0.000 claims description 47
- 239000001993 wax Substances 0.000 claims description 38
- 238000000855 fermentation Methods 0.000 claims description 35
- 230000004151 fermentation Effects 0.000 claims description 35
- 239000007795 chemical reaction product Substances 0.000 claims description 29
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 235000019441 ethanol Nutrition 0.000 claims description 20
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000005642 Oleic acid Substances 0.000 claims description 15
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical class CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 11
- 235000007164 Oryza sativa Nutrition 0.000 claims description 10
- 235000009566 rice Nutrition 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 235000012255 calcium oxide Nutrition 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 9
- 240000008042 Zea mays Species 0.000 claims description 8
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 235000009973 maize Nutrition 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 239000010902 straw Substances 0.000 claims description 8
- 230000032050 esterification Effects 0.000 claims description 7
- 238000005886 esterification reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- SZINCDDYCOIOJQ-UHFFFAOYSA-L manganese(2+);octadecanoate Chemical class [Mn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O SZINCDDYCOIOJQ-UHFFFAOYSA-L 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 241000196324 Embryophyta Species 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical class CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- -1 Anilino- Chemical class 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 2
- 150000003254 radicals Chemical class 0.000 abstract description 6
- 230000003078 antioxidant effect Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 150000002148 esters Chemical class 0.000 abstract description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 4
- 230000021615 conjugation Effects 0.000 abstract description 3
- 150000002831 nitrogen free-radicals Chemical class 0.000 abstract description 3
- 239000003963 antioxidant agent Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000004200 microcrystalline wax Substances 0.000 abstract description 2
- 238000007348 radical reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 241000209094 Oryza Species 0.000 description 8
- 238000010792 warming Methods 0.000 description 7
- 150000001335 aliphatic alkanes Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 235000019580 granularity Nutrition 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000035900 sweating Effects 0.000 description 2
- 230000009967 tasteless effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- DKCPKDPYUFEZCP-UHFFFAOYSA-N 2,6-di-tert-butylphenol Chemical class CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O DKCPKDPYUFEZCP-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 239000004169 Hydrogenated Poly-1-Decene Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000019383 crystalline wax Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000012777 electrically insulating material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000012184 mineral wax Substances 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/42—Refining of petroleum waxes
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P5/00—Preparation of hydrocarbons or halogenated hydrocarbons
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Zoology (AREA)
- Microbiology (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of oxidation inert type paraffin, belong to paraffin preparing technical field.The present invention increases the hardness and wear-resisting property of soft paraffin wax with a small amount of microwax, the present invention utilizes the oxidizable formation epoxidized soybean oil of soybean oil, it has excellent thermal stability and photostability, nitrogen free radical becomes highly stable under the influence of phenyl ring conjugation, not enough activity are reacted with esters oil molecule, it can only be with other radical reactions, they can and peroxy radical the reaction was continued generate NO free radical, the antioxidant intermediate of generation by phenyl ring conjugation, with very high stability, the chain termination reaction of free radical can only occur with other living radicals and peroxy radical, thermal stability is high, have with diphenylamines and cooperates with antioxidant effect well, to make the activation paraffin of preparation have good heat stable and Oxidation Stability, it has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of oxidation inert type paraffin, belong to paraffin preparing technical field.
Background technology
Paraffin is the popular name of solid-state higher alkane mixture, can be by natural or artificial petroleum waxy distillate cold press or molten
The methods of agent dewaxing, sweating are made, and for white, tasteless waxy solid, carbon atom number is about 18~30.It is generally divided into full refining
Three kinds of paraffin, semi-refined paraffin wax and scale wax.Paraffin is widely used, and good water resistance can have been produced after paper is immersed paraffin
Paraffin paper；After cotton yarn is added in paraffin, textile can be made soft, smooth and flexible.
Paraffin is one kind of refinery products.The mixture of solid alkane.Odorless, tasteless, white or faint yellow solid.
It is made by natural oil and artificial waxy distillate cold press or the methods of solvent dewaxing, sweating.For higher fatty acids processed, height
Grade alcohol, match, candle, waterproofing agent, ointment, electrically insulating material etc..
Paraffin is one kind of mineral wax and one kind of pertroleum wax；It is the lube cut warp obtained by the crude distillation
Slack wax is made through wax freezing and crystallizing, squeezing dewaxing in solvent refining, solvent dewaxing, then through solvent deoiling, it is refined obtained by sheet
Or acicular crystal.Also known as crystalline wax, the hydrocarbon mixture that carbon atom number is about 18~30, key component are linear paraffin（About
80%~95%）, the monocyclic naphthenes of alkane and belt length side chain also on a small quantity with individual branches（The two add up to content 20% with
Under）.Primary quality measure is fusing point and oil content, the former temperature resistant capability, the latter's expression purity.Wherein with the former two's purposes
It is relatively wide, it is mainly used as food and the component and packaging material of other commodity, painting dressing, the cosmetic material of baking container are used for
Fruit freshness preserving improves rubber ageing resistance and increases flexibility, electric elements insulation, hot investment casting etc., it can also be used to oxygen
Metaplasia is at synthetic fatty acid.
High added value paraffin wax product is developed, paraffin wax product can be further increased by improving the technology content of paraffin deep processed product
The market competitiveness.Paraffin can be widely applied to the industries such as chemicals, medicine, food, traffic.China is paraffin yield in the world
Maximum country, but high added value paraffin wax product is less, and the special special wax of most of purposes needs import.With science and technology
Development, the paraffin wax product of ordinary hard and fusing point cannot meet the needs of market.Paraffin oxidation inert type at present is poor,
Oxidizable to go bad, darken, or even stink, when use, can turn yellow in paraffin under illumination condition, paraffin brittleness itself
Greatly, by external impacts or friction fragmentation easy to wear.
Therefore, a kind of oxidation inert type paraffin of invention has positive effect to paraffin preparing technical field.
Invention content
Present invention mainly solves the technical issues of, poor for current paraffin oxidation inert type, oxidizable rotten, color becomes
Deep, or even stink, when use, can turn yellow in paraffin under illumination condition, and paraffin brittleness itself is big, by external impacts or rubs
The defect for wiping fragmentation easy to wear provides a kind of preparation method of oxidation inert type paraffin.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of oxidation inert type paraffin, it is characterised in that specifically preparation process is：
（1）By 3.4~3.8g2,6- DI-tert-butylphenol compounds, 3.6~4.0g diphenylamines are added in single-necked flask, continuously add
40~50ml n-decanes using magnetic stirrer, heat temperature raising, then are added under nitrogen protection into single-necked flask
8.5~10.0mL di-t-butyl peroxides, are stirred to react, and obtain reaction product；
（2）Above-mentioned single-necked flask is loaded onto into condensation reflux unit, heat temperature raising, after distillation, cooled to room temperature burns distillation
Bottle, which is placed in absolute ethyl alcohol, to be freezed, and is obtained the reaction product containing crystallization, is filtered to reaction product, and removal filtrate is filtered
Cake after filter cake is washed 3~5 times with n-decane, is placed in heat temperature raising in baking oven, dry, obtains 2,6 di-t-butyl -4-（Two
Anilino-）Phenol；
（3）Soybean oil, potassium hydroxide, ethanol solution are mixed, heat temperature raising is stirred to react, obtains mixed liquor, mixed liquor is set
In separatory funnel, hydrochloric acid is added into separatory funnel, adjusts mixed liquor PH, stands, liquid separation removal water layer obtains oil reservoir, with steaming
After distilled water water washed reservoir 3~5 times, it is to be esterified oleic acid to obtain purifying oil reservoir；
（4）Maize straw and rice bran are mixed, is put into pulverizer and crushes, sieving obtains mixing chaff powder, and 80~100g is mixed
Chaff powder, 20~30g oil plants waste oil, 40~50g esterification oleic acid are put into fermentation tank, then sequentially add 40~50g into crucible
Soft paraffin wax and 20~30g microwaxes, heat temperature raising make it melt completely, are then added dropwise in fermentation tank dropwise while hot, heat preservation
Fermentation, obtains tunning；
（5）By above-mentioned tunning heat temperature raising, filtering removal filter residue obtains filtrate, and liquid to be filtered is fermented after being cooled to room temperature
Wax powder, by fermentation wax powder and 2,6 di-t-butyl -4-（Hexichol amido）After phenol mixing 3 are washed with ethyl alcohol and deionized water successively
~5 times, standing and drying under room temperature obtains activation wax powder；
（6）The above-mentioned activation wax powders of 70~80g and 20~25g quick limes, 10 are sequentially added into the three-necked flask with blender
~15g diatomite heats up to three-necked flask oil bath, starts blender, is stirred, adds 0.10~0.15g manganese stearates,
Reaction product is obtained, then three-necked flask reaction product is poured into sheet frame mold, demoulds to obtain aoxidizing after being cooled to room temperature and stabilize
Type paraffin.
Step（1）The speed of agitator is 300~350r/min, and temperature is 140~160 DEG C after heat temperature raising, stirring
Reaction time is 3~4 h.
Step（2）Temperature is 140~150 DEG C after the heat temperature raising, and distillation time is 1~2h, absolute ethyl alcohol temperature
It it is -20~-15 DEG C, cooling time is 2~3h, and temperature is 90~100 DEG C after baking oven heat temperature raising, and drying time is 4~5h.
Step（3）The mass fraction of the ethanol solution is 75%, soybean oil, potassium hydroxide, ethanol solution mixing quality
Than for 5 ︰, 1 ︰ 8, temperature is 40~50 DEG C after heat temperature raising, it is 15~20min to be stirred to react the time, and the mass fraction of hydrochloric acid is
20%, it is 2~3 to adjust mixed liquor PH, and time of repose is 5~8min.
Step（4）The maize straw and rice bran mixing quality ratio is 4:1, it is 200 mesh that gained, which mixes chaff powder granularity, is added
Temperature is 60~80 DEG C after heat heating, and in fermentation tank, being heated to 40~50 DEG C, the heat-preservation fermentation time is 4~5 days.
Step（5）Temperature is 70~80 DEG C after the tunning heat temperature raising, fermentation wax powder and 2,6 di-t-butyls-
4-（Hexichol amido）Phenol mixing quality ratio is 5:1, the standing and drying time is 30~40min under room temperature, obtains activation wax powder.
Step（6）It is described heat up to three-necked flask oil bath after temperature be 120~150 DEG C, speed of agitator is 300~
350r/min, it is 10~15min to be stirred the time.
The beneficial effects of the invention are as follows：
（1）For the present invention with 2,6- DI-tert-butylphenol compounds, diphenylamines for major ingredient, oxidation reaction obtains oxidation product, by reflux, cold
Freeze, dry obtained 2,6 di-t-butyl -4-（Hexichol amido）Phenol is esterified using soybean oil, azelaic acid, neopentyl glycol as raw material
It to mixed ester, washes to obtain purifying oil reservoir by liquid separation and is esterified oleic acid, rice stalk and rice bran co-grinding are prepared mixed
Chaff powder is closed, by mixing chaff powder, oil plant waste oil, esterification oleic acid, soft paraffin wax, microwax mixed fermentation, heat-preservation fermentation is sent out
Ferment product obtains fermentation wax powder by cooling again after tunning heating and filtering, mixes 2,6 di-t-butyl -4-（Hexichol amido）Benzene
Phenol, standing and drying obtains activating wax powder after washing, finally mix activation wax powder, quick lime, diatomite etc. by certain mass ratio,
Mix a small amount of manganese stearate, in load plate frame mould, it is cooling after demoulding obtain oxidation inert type paraffin, the present invention is with a small amount of crystallite
Wax increases the hardness and wear-resisting property of soft paraffin wax, and the frictional behaviour of paraffin, diatomite are improved using fine-grained diatomite
Porosity characteristic paraffin can be protected not to be illuminated by the light influence and aoxidized, the calcium oxide in quick lime is conducive to resist paraffin solid
Absorb water dusting when chemical conversion type, improves the consistency of paraffin, and the calcium hydroxide of generation can increase the hardness of paraffin again, and it is anti-to improve it
Impact and wear-resisting property；
（2）The present invention utilizes the oxidizable formation epoxidized soybean oil of soybean oil, it has excellent thermal stability and photostability,
It can be esterified into esterification oleic acid under the action of alcohol and alkali, under the effect of the oxidative factors such as Esters oil molecule oxygen, oxidation reaction life occurs
At alkyl diradical and alkyl peroxy radical, these alkyl diradicals and alkyl peroxy radical and 2,6 di-t-butyl -4-
（Hexichol amido）Phenol reactant generates nitrogen free radical and the lower alcohol of activity and acid compounds, nitrogen free radical are conjugated in phenyl ring and imitate
What is become under the influence of answering is highly stable, and not enough activity are reacted with esters oil molecule, can only be with other radical reactions, they
Can and peroxy radical the reaction was continued generates NO free radical, such NO free radical is constantly lived again i.e. 2,6 di-t-butyl -4-
（Hexichol amido）The antioxidant effect of phenol is lived again so that antioxygen process is continued, the antioxidant intermediate of generation
By the conjugation of phenyl ring, there is very high stability, can only occur freely with other living radicals and peroxy radical
The chain termination reaction of base, thermal stability is high, with diphenylamines with antioxidant effect is cooperateed with well, to make the activation paraffin of preparation
With good hot stable and Oxidation Stability, have a extensive future.
Specific implementation mode
By 3.4~3.8g2,6- DI-tert-butylphenol compounds, 3.6~4.0g diphenylamines are added in single-necked flask, continuously add
40~50ml n-decanes stir 3~4h with the rotating speed of 300~350r/min using magnetic stirring apparatus, add under nitrogen protection
After heat is warming up to 140~160 DEG C, then 8.5~10.0mL di-t-butyl peroxides are added into single-necked flask, it is stirred to react 3~
4 h, obtain reaction product；Above-mentioned single-necked flask is loaded onto into condensation reflux unit, is heated to 140~150 DEG C, distillation 1~
After 2h, distilling flask is placed in 2~3h of freezing in -20~-15 DEG C of absolute ethyl alcohol, obtained containing crystallization by cooled to room temperature
Reaction product, reaction product is filtered, removal filtrate obtain filter cake, after filter cake is washed 3~5 times with n-decane, set
90~100 DEG C are heated in baking oven, dry 4~5h obtains 2,6 di-t-butyl -4-（Hexichol amido）Phenol；It will be big
The ethanol solution that soya-bean oil, potassium hydroxide, mass fraction are 75% is 5 ︰, 1 ︰ 8 mixing in mass ratio, is heated to 40~50 DEG C,
It is stirred to react 15~20min, obtains mixed liquor, mixed liquor is placed in separatory funnel, mass fraction is added into separatory funnel
For 20% hydrochloric acid, it is 2~3 to adjust mixed liquor PH, stands 5~8min, and liquid separation removal water layer obtains oil reservoir, washed with distilled water
After oil reservoir 3~5 times, it is to be esterified oleic acid to obtain purifying oil reservoir；It is 4 in mass ratio by maize straw and rice bran:1 mixing, is put into
Crushed in pulverizer, sieving obtain 200 mesh mixing chaff powder, by 80~100g mix chaff powder, 20~30g oil plants waste oil, 40~
50g esterification oleic acid is put into fermentation tank, then 40~50g soft paraffin wax and 20~30g microwaxes are sequentially added into crucible, is heated
60~80 DEG C are warming up to, it is made to melt completely, is then added dropwise in fermentation tank dropwise while hot, is heated to 40~50 DEG C, is protected
Temperature fermentation 4~5 days, obtains tunning；Above-mentioned tunning is heated to 70~80 DEG C, filtering removal filter residue is filtered
Liquid, liquid to be filtered obtain fermentation wax powder after being cooled to room temperature, by fermentation wax powder and 2,6 di-t-butyl -4-（Hexichol amido）Phenol is pressed
Mass ratio is 5:It is washed 3~5 times with ethyl alcohol and deionized water successively after 1 mixing, 30~40min of standing and drying under room temperature obtains work
Change wax powder；The above-mentioned activation wax powders of 70~80g and 20~25g quick limes, 10 are sequentially added into the three-necked flask with blender
~15g granularities are the diatomite of 300 mesh, are warming up to 120~150 DEG C to three-necked flask oil bath, start blender, with 300~
350r/min rotating speeds are stirred 10~15min, add 0.10~0.15g manganese stearates, obtain reaction product, then by three mouthfuls
Flask reaction product is poured into sheet frame mold, is demoulded after being cooled to room temperature and is obtained oxidation inert type paraffin.
By 3.4g2,6- DI-tert-butylphenol compounds, 3.6g diphenylamines are added in single-necked flask, continuously add the 40ml positive last of the ten Heavenly stems
Alkane stirs 3h using magnetic stirring apparatus with the rotating speed of 300r/min under nitrogen protection, after being heated to 140 DEG C, then to list
8.5mL di-t-butyl peroxides are added in mouth flask, is stirred to react 3 h, obtains reaction product；Above-mentioned single-necked flask is loaded onto cold
Solidifying reflux is heated to 140 DEG C, and after distilling 1h, distilling flask is placed in -20 DEG C anhydrous by cooled to room temperature
2h is freezed in ethyl alcohol, the reaction product containing crystallization is obtained, reaction product is filtered, and removal filtrate obtains filter cake, by filter cake
It after washing 3 times with n-decane, is placed in baking oven and is heated to 90 DEG C, dry 4h obtains 2,6 di-t-butyl -4-（Diphenylamines
Base）Phenol；It is that 5 ︰, 1 ︰ 8 are mixed in mass ratio by the ethanol solution that soybean oil, potassium hydroxide, mass fraction are 75%, heat temperature raising
To 40 DEG C, it is stirred to react 15min, obtains mixed liquor, mixed liquor is placed in separatory funnel, quality point is added into separatory funnel
Number is 20% hydrochloric acid, and it is 2 to adjust mixed liquor PH, stands 5min, liquid separation removal water layer obtains oil reservoir, with distilled water water washed reservoir 3
After secondary, it is to be esterified oleic acid to obtain purifying oil reservoir；It is 4 in mass ratio by maize straw and rice bran:1 mixing, is put into pulverizer
It crushes, sieving obtains 200 mesh mixing chaff powder, and 80g, which is mixed chaff powder, 20g oil plants waste oil, 40g esterification oleic acid, is put into fermentation tank
In, then 40g soft paraffin wax and 20g microwaxes are sequentially added into crucible, 60 DEG C are heated to, it is made to melt completely, then
It is added dropwise in fermentation tank dropwise while hot, is heated to 40 DEG C, heat-preservation fermentation 4 days obtains tunning；By above-mentioned tunning
70 DEG C are heated to, filtering removal filter residue obtains filtrate, and liquid to be filtered obtains fermentation wax powder after being cooled to room temperature, by wax powder of fermenting
With 2,6 di-t-butyl -4-（Hexichol amido）Phenol is 5 in mass ratio:After 1 mixing 3 are washed with ethyl alcohol and deionized water successively
Secondary, standing and drying 30min under room temperature obtains activation wax powder；The above-mentioned activation of 70g is sequentially added into the three-necked flask with blender
Wax powder and 20g quick limes, the diatomite that 10g granularities are 300 mesh, are warming up to 120 DEG C to three-necked flask oil bath, start blender,
It is stirred 10min with 300r/min rotating speeds, adds 0.10g manganese stearates, obtains reaction product, then three-necked flask is reacted
Product pours into sheet frame mold, is demoulded after being cooled to room temperature and obtains oxidation inert type paraffin.
By 3.6g2,6- DI-tert-butylphenol compounds, 3.8g diphenylamines are added in single-necked flask, continuously add the 45ml positive last of the ten Heavenly stems
Alkane stirs 3.5h using magnetic stirring apparatus with the rotating speed of 320r/min under nitrogen protection, after being heated to 150 DEG C, then
9.0mL di-t-butyl peroxides are added into single-necked flask, is stirred to react 3.5h, obtains reaction product；By above-mentioned single-necked flask
Condensation reflux unit is loaded onto, is heated to 145 DEG C, after distilling 1.5h, distilling flask is placed in -17 by cooled to room temperature
DEG C absolute ethyl alcohol in freeze 2.5h, obtain the reaction product containing crystallization, reaction product filtered, removal filtrate filtered
Cake after filter cake is washed 4 times with n-decane, is placed in baking oven and is heated to 95 DEG C, and dry 4.5h obtains 2,6 two tertiary fourths
Base -4-（Hexichol amido）Phenol；It is 5 ︰, 1 ︰ 8 in mass ratio by the ethanol solution that soybean oil, potassium hydroxide, mass fraction are 75%
Mixing, is heated to 45 DEG C, is stirred to react 17min, obtain mixed liquor, mixed liquor is placed in separatory funnel, is leaked to liquid separation
The hydrochloric acid that mass fraction is 20% is added in bucket, it is 2 to adjust mixed liquor PH, stands 7min, and liquid separation removal water layer obtains oil reservoir, uses
After distilled water water washed reservoir 4 times, it is to be esterified oleic acid to obtain purifying oil reservoir；It is 4 in mass ratio by maize straw and rice bran:1 is mixed
It closes, is put into pulverizer and crushes, sieving obtains 200 mesh mixing chaff powder, and 90g, which is mixed chaff powder, 25g oil plants waste oil, 45g, to be esterified
Oleic acid is put into fermentation tank, then 45g soft paraffin wax and 25g microwaxes are sequentially added into crucible, is heated to 70 DEG C, is made it
Melting completely, is then added dropwise in fermentation tank, is heated to 45 DEG C, heat-preservation fermentation 4 days obtains tunning dropwise while hot；
Above-mentioned tunning is heated to 75 DEG C, filtering removal filter residue obtains filtrate, and liquid to be filtered is fermented after being cooled to room temperature
Wax powder, by fermentation wax powder and 2,6 di-t-butyl -4-（Hexichol amido）Phenol is 5 in mass ratio:1 mixing after successively use ethyl alcohol and
Deionized water is washed 4 times, and standing and drying 35min under room temperature obtains activation wax powder；Add successively into the three-necked flask with blender
Enter the above-mentioned activation wax powders of 75g and 22g quick limes, the diatomite that 12g granularities are 300 mesh, 140 are warming up to three-necked flask oil bath
DEG C, start blender, 12min is stirred with 320r/min rotating speeds, adds 0.12g manganese stearates, obtains reaction product, then
Three-necked flask reaction product is poured into sheet frame mold, is demoulded after being cooled to room temperature and obtains oxidation inert type paraffin.
By 3.8g2,6- DI-tert-butylphenol compounds, 4.0g diphenylamines are added in single-necked flask, continuously add the 50ml positive last of the ten Heavenly stems
Alkane stirs 4h using magnetic stirring apparatus with the rotating speed of 350r/min under nitrogen protection, after being heated to 160 DEG C, then to
10.0mL di-t-butyl peroxides are added in single-necked flask, is stirred to react 4 h, obtains reaction product；Above-mentioned single-necked flask is filled
Upper condensation reflux unit is heated to 150 DEG C, and after distilling 2h, distilling flask is placed in -15 DEG C by cooled to room temperature
3h is freezed in absolute ethyl alcohol, the reaction product containing crystallization is obtained, reaction product is filtered, and removal filtrate obtains filter cake, will
It after filter cake washs 5 times with n-decane, is placed in baking oven and is heated to 100 DEG C, dry 5h obtains 2,6 di-t-butyl -4-（Two
Anilino-）Phenol；It is that 5 ︰, 1 ︰ 8 are mixed in mass ratio by the ethanol solution that soybean oil, potassium hydroxide, mass fraction are 75%, heating
50 DEG C are warming up to, 20min is stirred to react, obtains mixed liquor, mixed liquor is placed in separatory funnel, matter is added into separatory funnel
The hydrochloric acid that score is 20% is measured, it is 3 to adjust mixed liquor PH, stands 8min, and liquid separation removal water layer obtains oil reservoir, washed with distilled water
After oil reservoir 5 times, it is to be esterified oleic acid to obtain purifying oil reservoir；It is 4 in mass ratio by maize straw and rice bran:1 mixing, is put into crushing
It is crushed in machine, sieving obtains 200 mesh mixing chaff powder, and 100g, which is mixed chaff powder, 30g oil plants waste oil, 50g esterification oleic acid, is put into hair
In fermentation tank, then 50g soft paraffin wax and 30g microwaxes are sequentially added into crucible, be heated to 80 DEG C, it is made to melt completely,
It is then added dropwise in fermentation tank dropwise while hot, is heated to 50 DEG C, heat-preservation fermentation 5 days obtains tunning；By above-mentioned fermentation
Product is heated to 80 DEG C, and filtering removal filter residue obtains filtrate, and liquid to be filtered obtains fermentation wax powder, will ferment after being cooled to room temperature
Wax powder and 2,6 di-t-butyl -4-（Hexichol amido）Phenol is 5 in mass ratio:Ethyl alcohol and deionization is used to wash successively after 1 mixing
It washs 5 times, standing and drying 40min under room temperature obtains activation wax powder；It is above-mentioned that 80g is sequentially added into the three-necked flask with blender
Wax powder and 25g quick limes, the diatomite that 15g granularities are 300 mesh are activated, 150 DEG C are warming up to three-necked flask oil bath, starts stirring
Device is stirred 15min with 350r/min rotating speeds, adds 0.15g manganese stearates, obtains reaction product, then by three-necked flask
Reaction product is poured into sheet frame mold, is demoulded after being cooled to room temperature and is obtained oxidation inert type paraffin.
With the oxidation inert type paraffin of Guangzhou company production as a comparison case to oxidation inert type stone produced by the present invention
Oxidation inert type paraffin in wax and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Hardness test is detected using hardness-testing device；
Antioxygenic property test method：Accelerated oxidation test is done using Schaal Oven Methods, it will be in example 1~3 and comparative example
Paraffin is respectively placed in the relatively good insulating box of air and stores 4d, is sampled every for 24 hours, according to national regulation GB/T5009.37-
2003 method measures peroxide value, and observes surface situation of change.
1 paraffin performance measurement result of table
It is small according to the oxidation inert type paraffin peroxide value produced by the present invention of data among the above, slow down oxidation rate, aoxidizes
Stability is greatly improved, and antioxygenic property is greatly improved, and color does not change, and free from extraneous odour generates, hardness
Height, good impact resistance is not easy to wear, has broad application prospects.
Claims (7)
1. a kind of preparation method of oxidation inert type paraffin, it is characterised in that specifically preparation process is：
（1）By 3.4~3.8g2,6- DI-tert-butylphenol compounds, 3.6~4.0g diphenylamines are added in single-necked flask, continuously add
40~50ml n-decanes using magnetic stirrer, heat temperature raising, then are added under nitrogen protection into single-necked flask
8.5~10.0mL di-t-butyl peroxides, are stirred to react, and obtain reaction product；
（2）Above-mentioned single-necked flask is loaded onto into condensation reflux unit, heat temperature raising, after distillation, cooled to room temperature burns distillation
Bottle, which is placed in absolute ethyl alcohol, to be freezed, and is obtained the reaction product containing crystallization, is filtered to reaction product, and removal filtrate is filtered
Cake after filter cake is washed 3~5 times with n-decane, is placed in heat temperature raising in baking oven, dry, obtains 2,6 di-t-butyl -4-（Two
Anilino-）Phenol；
（3）Soybean oil, potassium hydroxide, ethanol solution are mixed, heat temperature raising is stirred to react, obtains mixed liquor, mixed liquor is set
In separatory funnel, hydrochloric acid is added into separatory funnel, adjusts mixed liquor PH, stands, liquid separation removal water layer obtains oil reservoir, with steaming
After distilled water water washed reservoir 3~5 times, it is to be esterified oleic acid to obtain purifying oil reservoir；
（4）Maize straw and rice bran are mixed, is put into pulverizer and crushes, sieving obtains mixing chaff powder, and 80~100g is mixed
Chaff powder, 20~30g oil plants waste oil, 40~50g esterification oleic acid are put into fermentation tank, then sequentially add 40~50g into crucible
Soft paraffin wax and 20~30g microwaxes, heat temperature raising make it melt completely, are then added dropwise in fermentation tank dropwise while hot, heat preservation
Fermentation, obtains tunning；
（5）By above-mentioned tunning heat temperature raising, filtering removal filter residue obtains filtrate, and liquid to be filtered is fermented after being cooled to room temperature
Wax powder, by fermentation wax powder and 2,6 di-t-butyl -4-（Hexichol amido）After phenol mixing 3 are washed with ethyl alcohol and deionized water successively
~5 times, standing and drying under room temperature obtains activation wax powder；
（6）The above-mentioned activation wax powders of 70~80g and 20~25g quick limes, 10 are sequentially added into the three-necked flask with blender
~15g diatomite heats up to three-necked flask oil bath, starts blender, is stirred, adds 0.10~0.15g manganese stearates,
Reaction product is obtained, then three-necked flask reaction product is poured into sheet frame mold, demoulds to obtain aoxidizing after being cooled to room temperature and stabilize
Type paraffin.
2. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（1）It is described
Speed of agitator be 300~350r/min, temperature is 140~160 DEG C after heat temperature raising, and it is 3~4 h to be stirred to react the time.
3. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（2）It is described
Heat temperature raising after temperature be 140~150 DEG C, distillation time is 1~2h, and absolute ethyl alcohol temperature is -20~-15 DEG C, when freezing
Between be 2~3h, temperature is 90~100 DEG C after baking oven heat temperature raising, and drying time is 4~5h.
4. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（3）It is described
Ethanol solution mass fraction be 75%, soybean oil, potassium hydroxide, ethanol solution mixing quality ratio be 5 ︰, 1 ︰ 8, heat temperature raising
Temperature is 40~50 DEG C afterwards, and it is 15~20min to be stirred to react the time, and the mass fraction of hydrochloric acid is 20%, and it is 2 to adjust mixed liquor PH
~3, time of repose is 5~8min.
5. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（4）It is described
Maize straw and rice bran mixing quality ratio be 4:1, it is 200 mesh that gained, which mixes chaff powder granularity, after heat temperature raising temperature be 60~
80 DEG C, in fermentation tank, being heated to 40~50 DEG C, the heat-preservation fermentation time is 4~5 days.
6. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（5）It is described
Tunning heat temperature raising after temperature be 70~80 DEG C, fermentation wax powder and 2,6 di-t-butyl -4-（Hexichol amido）Phenol is mixed
It is 5 to close mass ratio:1, the standing and drying time is 30~40min under room temperature, obtains activation wax powder.
7. a kind of preparation method of oxidation inert type paraffin according to claim 1, it is characterised in that：Step（6）It is described
Heat up to three-necked flask oil bath after temperature be 120~150 DEG C, speed of agitator is 300~350r/min, is stirred the time and is
10~15min.
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| CN110511576A (en) * | 2019-07-23 | 2019-11-29 | 肥东县云武研发有限公司 | A kind of glass lost-wax process casting paraffin and preparation method thereof |
| CN113337243A (en) * | 2021-05-19 | 2021-09-03 | 张碧军 | Sealing silica gel and preparation method thereof |
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