CN110172109A - A kind of method of continuous synthesis oxidized polyethylene wax - Google Patents
A kind of method of continuous synthesis oxidized polyethylene wax Download PDFInfo
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- CN110172109A CN110172109A CN201910527722.5A CN201910527722A CN110172109A CN 110172109 A CN110172109 A CN 110172109A CN 201910527722 A CN201910527722 A CN 201910527722A CN 110172109 A CN110172109 A CN 110172109A
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- polyethylene wax
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- packed tower
- oxidized polyethylene
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- 239000004209 oxidized polyethylene wax Substances 0.000 title claims abstract description 30
- 235000013873 oxidized polyethylene wax Nutrition 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 239000004698 Polyethylene Substances 0.000 claims abstract description 44
- -1 polyethylene Polymers 0.000 claims abstract description 44
- 229920000573 polyethylene Polymers 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 35
- 239000003570 air Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 26
- 230000001590 oxidative effect Effects 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000001993 wax Substances 0.000 claims description 55
- 239000007788 liquid Substances 0.000 claims description 26
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000006057 Non-nutritive feed additive Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 claims description 2
- 239000003674 animal food additive Substances 0.000 claims description 2
- 239000013556 antirust agent Substances 0.000 claims description 2
- 239000002199 base oil Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000002537 cosmetic Substances 0.000 claims description 2
- 239000005548 dental material Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 claims description 2
- XMHIUKTWLZUKEX-UHFFFAOYSA-N hexacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O XMHIUKTWLZUKEX-UHFFFAOYSA-N 0.000 claims description 2
- 239000012943 hotmelt Substances 0.000 claims description 2
- 238000012432 intermediate storage Methods 0.000 claims description 2
- 238000005495 investment casting Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000003129 oil well Substances 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 239000006187 pill Substances 0.000 claims description 2
- 238000010057 rubber processing Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 239000006224 matting agent Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000009941 weaving Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000002253 acid Substances 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000002904 solvent Substances 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 20
- 239000007791 liquid phase Substances 0.000 description 15
- 239000012071 phase Substances 0.000 description 13
- 238000007254 oxidation reaction Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 8
- 238000012546 transfer Methods 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000007792 gaseous phase Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000010960 commercial process Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/06—Oxidation
Abstract
The present invention relates to a kind of methods of continuous synthesis oxidized polyethylene wax, and using micro passage reaction or packed tower as reactor, oxidizing gas and polyethylene wax obtain oxidized polyethylene wax in filler surface haptoreaction.Production process is carried out continuously, and high degree of automation, labor intensity is small, stable product quality, and acid value is adjustable.The oxidizing gas is air, oxygen or oxygen-enriched air, and the polyethylene wax is soluble in solvent, or is added in micro passage reaction or packed tower in the molten state.By the production technology, the oxidized polyethylene wax that acid value is 5-40mgKOH/g, paler colour can be obtained.
Description
Technical field
The invention belongs to technical field of fine, and in particular to a kind of continuity method oxidation reaction process.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
Oxidized polyethylene wax is excellent novel polar waxes, since oxidized polyethylene wax strand has a certain amount of carbonyl
And hydroxyl, so just significantly improving with the intermiscibility of filler, pigment, polar resin.Wetability in polar system, point
It dissipates property and is better than polyethylene wax, while also having both coupled.It can be used for fruit coating guarantee the quality, prepare various pipelines, mechanical fitting,
Hardware tool preservative and the moisture-proof important source material of polyethylene board, corrugation case, it may also be used for advanced papermaking, liquid leather shoes
Oil, floor wax, furniture cream, car detailing wax etc..Existing oxidized polyethylene wax production technology is intermittent autoclave production work
Skill.Patent 200810223933.1 proposes and is passed through oxidizing gas in water and polyethylene wax system, and heating crack anti-
It answers, prepares oxidized polyethylene wax.Patent 201720015346.8 proposes a kind of process units of oxidized polyethylene wax, passes through
The setting of filter chamber improves purity；The water in reaction warehouse pedestal is heated by electric heating tube, heating temperature is stablized；Pass through preheating
The setting of pipe, capacity usage ratio are high.Patent 201710765211.8 carries out oxidation reaction in high-pressure bottle, and preparation aoxidizes poly- second
Alkene wax.As it can be seen that be batch production technique now with technology, and oxygen concentration of gas phase is higher in reaction process, it is easy to form
Explosive mixture brings the risk of safety and environmental protection.Meanwhile if wanting to obtain the higher product of quality, longer oxidation is needed
Reaction time, therefore, mature commercial process are batch tank production technology.According to the production work of serialization
Skill, residence time of material is long, and the equipment size needed is very big, and safety coefficient is low, and industrialization is difficult.
Summary of the invention
In order to overcome the above problem, the present invention provides a kind of continuous oxidation reaction processes, and reaction speed is fast, by-product
Few and highly-safe, product yield is high, can get the oxidic polyethylene wax product of high quality.
To realize the above-mentioned technical purpose, The technical solution adopted by the invention is as follows:
A kind of method of continuous synthesis oxidized polyethylene wax, polyethylene wax solution and oxidizing gas are in micro passage reaction
Or reaction in packed tower, oxidized polyethylene wax is made.
The hair that the above-mentioned design of the application improves oxidation reaction speed under the premise of guaranteeing product quality, inhibits side reaction
It raw, the reduction residence time, realizes the miniaturization of equipment, breaches the technology barrier of current oxidic polyethylene wax product continuous production
Hinder.
In the micron-scale, the ratio of surface area and volume is long-range for the characteristic dimension of all kinds of basic units in micro passage reaction
In conventional system, so that heat transfer, mass transport process be made to be strengthened, Temperature Distribution is set to realize in a short period of time uniform
Change.Therefore, in the one aspect of the application, oxidized polyethylene wax is continuously synthesized using micro passage reaction.
The micro passage reaction is made of multiple flechette-type modules and straight runner, wherein the entrance of flechette-type module is set
It is equipped with arrow-shaped protrusion, the exit of the flechette-type module is provided with cylindrical protrusions, so that fluid be made to be formed in flechette-type module
Interaction reflux, greatly improved the mixing efficiency and reaction efficiency of fluid, and then the yield of product, purity is made to increase.
After polyethylene wax solution and oxidizing gas react in micro passage reaction, in order to which the oxidation for obtaining high-purity is poly-
Ethylene waxes, in some embodiments, the micro passage reaction are also connected with gas-liquid separator, to remove solvent by distillation,
Improve the purity of oxidized polyethylene wax.
Research is found: as microreactor temperature increases, pressure increase, oxidized polyethylene wax yield increases.If but reacting
Temperature is excessively high to will lead to side reaction increase, and product purity declines, and after pressure reaches 1.2MPa, pressure is continued growing, to oxidation
Polyethylene wax yield is promoted less, and therefore, in some embodiments, the temperature of the micro passage reaction is 80-240 DEG C, presses
Power is 0-1.2MPa.
Packed tower is contacted and the basic building block of mass transfer using filler as air-liquid, liquid filler surface in it is membranaceous from upper and
Lower flowing, gas is presented to flow with liquid from bottom to top in continuous phase, and carries out mass transfer and heat transfer between gas and liquid two phases, has
Have that production capacity is big, separative efficiency is high, and pressure drop is small, and liquid holdup is small, the big advantage of operating flexibility, therefore, at of the invention one
Aspect synthesizes oxidized polyethylene wax as reactor using packed tower.
In some embodiments, the packed tower is also sequentially connected with intermediate storage tank, distillation still, effectively to elimination reaction
Solvent afterwards obtains high-purity mangesium oxide polyethylene wax.
In some embodiments, the polyethylene wax solution and oxidizing gas the hybrid mode of packed tower be cocurrent or
Countercurrently.In cocurrent and counter-current process, polyethylene wax solution flows to form liquid film along filler surface, is dispersed in the oxygen continuously flowed
Among the property changed gas, for gas-liquid two-phase contact surface on the liquid film surface of filler, reaction efficiency is high.
Research is found: if reaction temperature is lower than 100 DEG C, the gas liquid reaction efficiency on liquid film is lower, oxidized polyethylene wax
Yield is low, if temperature is greater than 200 DEG C, continues to improve reaction temperature, be promoted less to the yield of oxidized polyethylene wax, therefore,
In some embodiments, the reaction temperature of the packed tower is 100-200 DEG C, pressure 0-1.0MPa, to effectively improve oxidation
The yield and purity of polyethylene wax.
In order to obtain higher reaction efficiency, the application selects mass-transfer efficiency is high, flood point is high and pressure drop is low to fill out
Material, in some embodiments, the filler of the packed tower are that filler can be spherical, Pall ring or Raschig ring filler.
The solution that this field routine can be used in the polyethylene wax solution of the application is prepared, as long as can guarantee and oxidisability gas
The reaction efficiency of body, in this regard, the application does not make special restriction, in some embodiments, the polyethylene wax solution
For the polyethylene wax or polyethylene wax toluene, xylene solution of melting.
The application considers that in some embodiments, the oxidizing gas is for of both cost and oxidation efficiency
Air, oxygen or oxygen-enriched air.
The present invention also provides the oxidized polyethylene wax of any above-mentioned method preparation.
The present invention also provides above-mentioned oxidized polyethylene wax as shoe polish, floor wax, wax polish, car wax, cosmetics,
Match candlestick, ink anti-wear agent, ceramics, hot investment casting agent, oil absorbent, lute in, Chinese medicine wax-wrapped pill, hotmelt, paint
With powdery paints delustering agent, cable feed additives, oil well inhale cerate, wax crayon, carbon paper, paraffin paper, ink paste, photosensitive material matrix,
Textile softener, electronic component encapsulation agent, the agent of transistor package, rubber processing aids, automobile base oil, dental material processing help
Agent, the application of steel antirust agent.
The beneficial effects of the present invention are:
(1) production technology is continuous production technology, and process regulation is simple, accurate, high degree of automation, product matter
Amount is stablized.The product of different acid values can be obtained by the adjustment of technological parameter.
(2) operating method of the application it is simple, it is at low cost, have universality, be easy to large-scale production.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the process flow chart of the invention patent of embodiment 1；
Fig. 2 is the flow diagram of the micro passage reaction of embodiment 1；
Fig. 3 is the flechette-type module map of the micro passage reaction of embodiment 1；
Fig. 4 is the overall structure figure of the micro passage reaction of embodiment 1；
Fig. 5 is the process flow chart of the invention patent of embodiment 4.
Wherein, 1 be flechette-type module, 2 be cylindrical protrusions, 3 be arrow-shaped protrusion.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used in this application have logical with the application person of an ordinary skill in the technical field
The identical meanings understood.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
In the examples where no specific technique or condition is specified, according to the literature in the art described technology or conditions or
Person carries out according to product description.Reagents or instruments used without specified manufacturer, being can be by the normal of commercially available acquisition
Advise product.
As background technique is introduced, easy to form explosion higher for oxygen concentration of gas phase during batch production
Property mixture, bring safety and environmental protection risk the problem of.Therefore, the present invention proposes a kind of continuous metaplasia of oxidized polyethylene wax
Production. art, respectively using micro passage reaction, packed tower as reactor, oxidizing gas and polyethylene wax are anti-in filler surface contact
It answers, obtains oxidized polyethylene wax.Production process is carried out continuously, and high degree of automation, labor intensity is small, stable product quality, acid
Value is adjustable.The oxidizing gas is air, oxygen or oxygen-enriched air, and the polyethylene wax is soluble in solvent
In, or be added in packed tower in the molten state.By the production technology, can obtain acid value is 5-40mgKOH/g, color
Thin oxidized polyethylene wax.
It is specifically divided into following two situation:
One aspect of the present invention provides a kind of method that micro passage reaction continuously synthesizes oxidized polyethylene wax, packet
It includes following steps: by polyethylene wax wiring solution-forming, and heating；Oxidizing gas is preheated using preheater；Above-mentioned two strands of materials are logical
Enter micro passage reaction, carries out hybrid reaction；The material of reactor is molten through distillation removing after gas-liquid separator separates gas phase out
Agent obtains oxidic polyethylene wax product.
In some embodiments, polyethylene wax can be by high temperature melt, or is made into using toluene, dimethylbenzene equal solvent molten
Liquid.
In some embodiments, oxidizing gas is air, oxygen or oxygen-enriched air.
In some embodiments, oxidized polyethylene wax and the preheated device of oxidizing gas are preheated to 80-240 DEG C.
In some embodiments, the mass ratio of polyethylene wax solution and oxidizing gas is 1000:1-1000:10.
In some embodiments, micro passage reaction temperature is 80-240 DEG C.
In some embodiments, micro passage reaction pressure is 0-1.2MPa.
One aspect of the present invention provides a kind of oxidized polyethylene wax production technology of packed tower serialization, comprising: oxygen
The property changed gas and polyethylene wax carry out two interphase mass transfers, heat transfer in packed tower, and catalytic oxidation occurs, and production process connects
Continuousization operation
In some embodiments, oxidizing gas first passes through preheating, enters back into packed tower, under certain temperature and pressure into
Row oxidation reaction；
In some embodiments, packed tower can be operated using modes such as cocurrent or countercurrents；
In some embodiments, by the operation such as gas phase flow velocity, liquid phase flow rate and liquid phase circulation, the controllable reaction time is
1-8 hours；
In some embodiments, oxidizing gas can be air, oxygen or oxygen-enriched air；
In some embodiments, packed tower reaction temperature is 100-200 DEG C；
In some embodiments, packed tower reaction pressure is 0-1.0MPa；
In some embodiments, the filler that packed tower uses can be the forms such as spherical shape, Pall ring, Raschig ring.
It is described below by way of scheme of the specific embodiment to the application.
Embodiment 1:
1.100g polyethylene wax wiring solution-forming in dissolving tank 1 with 200g toluene, 110 DEG C are heated in preheater 2, is
3 liquid phase feeding of micro passage reaction enters reactor with the flow velocity of 10g/min.
It is 3 gas-phase feed of micro passage reaction 2. air is heated to 110 DEG C with the preheated device 4 of the speed of 0.1g/min.
3. liquid phase material and the gaseous phase materials hybrid reaction in micro passage reaction 3, residence time 90s, temperature control
At 110 DEG C.
4. the material come out from micro passage reaction 3 through gas-liquid separator 5, separates gas phase, liquid phase go out distillation still 6 steam it is molten
Agent obtains oxidic polyethylene wax product, the micro- Huang of appearance, acid value 19.3mgKOH/g.
Embodiment 2:
1.100g polyethylene wax wiring solution-forming in dissolving tank 1 with 200g dimethylbenzene, is heated to 130 DEG C in preheater 2,
For 3 liquid phase feeding of micro passage reaction, reactor is entered with the flow velocity of 10g/min.
It is 3 gas-phase feed of micro passage reaction 2. air is heated to 130 DEG C with the preheated device 4 of the speed of 0.1g/min.
3. liquid phase material and the gaseous phase materials hybrid reaction in micro passage reaction 3, residence time 100s, temperature control
At 130 DEG C.
4. the material come out from micro passage reaction 2 through gas-liquid separator 5, separates gas phase, liquid phase go out distillation still 6 steam it is molten
Agent obtains oxidic polyethylene wax product, the micro- Huang of appearance, acid value 15.9mgKOH/g.
Embodiment 3
1.100g polyethylene wax is heated to 100 DEG C in dissolving tank 1, and 120 DEG C are heated in preheater 2, is microchannel
3 liquid phase feeding of reactor enters reactor with the flow velocity of 50g/min.
It is 2 gas-phase feed of micro passage reaction 2. air is heated to 120 DEG C with the preheated device 4 of the speed of 0.2g/min.
3. liquid phase material and the gaseous phase materials hybrid reaction in micro passage reaction 3, residence time 75s, temperature control
At 120 DEG C.
4. the material come out from micro passage reaction 2 through gas-liquid separator 5, separates gas phase, liquid phase go out distillation still 6 steam it is molten
Agent obtains oxidic polyethylene wax product, the micro- Huang of appearance, acid value 28.7mgKOH/g.
Embodiment 4:
(1) Raschig ring of the filler using stainless steel material in packed tower, atmospheric operation, temperature are 120 DEG C；
(2) using air as oxidizing gas, preheated device is heated to 100 DEG C and enters filler tower bottom, and air mass flow is
1.2m3/h。
(3) the preheated device of the toluene solution of polyethylene wax is heated to 90 DEG C, is added from packed tower napex, in filler surface shape
At liquid film, and the oxygen in the air carried out with bottom is reacted.The liquid phase residence time is 3h.
(4) packed tower bottom liquid carries out relay reservoir, removes 150 DEG C of removing solvents of distillation still, is discharged and cooling, must aoxidize
Polyethylene wax product, acid value 14.3mgKOH/g.
Embodiment 5:
(1) Raschig ring of the filler using stainless steel material in packed tower, atmospheric operation, temperature are 135 DEG C；
(2) using air as oxidizing gas, preheated device is heated to 100 DEG C and enters filler tower bottom, and air mass flow is
1.5m3/h。
(3) the preheated device of the toluene solution of polyethylene wax is heated to 100 DEG C, is added from packed tower napex, in filler surface
Liquid film is formed, and the oxygen in the air carried out with bottom is reacted.The liquid phase residence time is 3.5h.
(4) packed tower bottom liquid carries out relay reservoir, removes 150 DEG C of removing solvents of distillation still, is discharged and cooling, must aoxidize
Polyethylene wax product, acid value 26.3mgKOH/g.
Embodiment 6:
(1) Pall ring of the filler using stainless steel material in packed tower, atmospheric operation, temperature are 135 DEG C；
(2) using air as oxidizing gas, preheated device is heated to 100 DEG C and enters filler tower bottom, and air mass flow is
1.5m3/h。
(3) the preheated device of the toluene solution of polyethylene wax is heated to 100 DEG C, is added from packed tower napex, in filler surface
Liquid film is formed, and the oxygen in the air carried out with bottom is reacted.The liquid phase residence time is 4.5h.
(4) packed tower bottom liquid carries out relay reservoir, removes 150 DEG C of removing solvents of distillation still, is discharged and cooling, must aoxidize
Polyethylene wax product, acid value 38.2mgKOH/g.
Embodiment 7:
(1) Pall ring of the filler using stainless steel material in packed tower, atmospheric operation, temperature are 145 DEG C；
(2) using air as oxidizing gas, preheated device is heated to 100 DEG C and enters filler tower bottom, and air mass flow is
1.0m3/h。
(3) the preheated device of polyethylene wax is heated to 140 DEG C, is added from packed tower napex, forms liquid film in filler surface, and
The oxygen in air carried out with bottom is reacted.The liquid phase residence time is 5.5h.
(4) packed tower bottom liquid carries out relay reservoir, is discharged and cooling, obtains oxidic polyethylene wax product, acid value is
28.9mgKOH/g。
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to technical solution documented by previous embodiment, or part is equivalently replaced.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (10)
1. a kind of method of continuous synthesis oxidized polyethylene wax, which is characterized in that polyethylene wax solution and oxidizing gas are micro-
Reaction in channel reactor or packed tower, is made oxidized polyethylene wax.
2. the method as described in claim 1, which is characterized in that the micro passage reaction is also connected with gas-liquid separator.
3. the method as described in claim 1, which is characterized in that the temperature of the micro passage reaction is 80-240 DEG C, pressure
For 0-1.2MPa.
4. the method as described in claim 1, which is characterized in that the packed tower is also sequentially connected with intermediate storage tank, distillation still.
5. the method as described in claim 1, which is characterized in that the polyethylene wax solution and oxidizing gas are in packed tower
Hybrid mode is cocurrent or countercurrent.
6. the method as described in claim 1, which is characterized in that the reaction temperature of the packed tower is 100-200 DEG C, and pressure is
0-1.0MPa；
Or it can be spherical, Pall ring or Raschig ring filler that the filler of the packed tower, which is filler,.
7. the method as described in claim 1, which is characterized in that the polyethylene wax solution is the polyethylene wax or poly- of melting
Ethylene waxes toluene, xylene solution.
8. the method as described in claim 1, which is characterized in that the oxidizing gas is air, oxygen or oxygen-enriched air.
9. the oxidized polyethylene wax of the described in any item method preparations of claim 1-8.
10. oxidized polyethylene wax as claimed in claim 9 is as shoe polish, floor wax, wax polish, car wax, cosmetics, match wax
Bar, ink anti-wear agent, ceramics, hot investment casting agent, oil absorbent, lute in, Chinese medicine wax-wrapped pill, hotmelt, paint and powder
Coating Matting agent, cable feed additives, oil well suction cerate, wax crayon, carbon paper, paraffin paper, ink paste, photosensitive material matrix, weaving are soft
Soft dose, electronic component encapsulation agent, the agent of transistor package, rubber processing aids, automobile base oil, dental material processing aid, steel
The application of antirust agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910527722.5A CN110172109A (en) | 2019-06-18 | 2019-06-18 | A kind of method of continuous synthesis oxidized polyethylene wax |
Applications Claiming Priority (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797867A (en) * | 2021-09-30 | 2021-12-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Preparation method of continuous micro-channel of oxidized wax |
| CN114345255A (en) * | 2021-12-27 | 2022-04-15 | 沈阳化工研究院有限公司 | Device for continuously preparing 3,3, 3-trifluoro-2, 2-dichloropropanal |
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|---|---|---|---|---|
| CN113797867A (en) * | 2021-09-30 | 2021-12-17 | 内蒙古伊泰煤基新材料研究院有限公司 | Preparation method of continuous micro-channel of oxidized wax |
| CN114345255A (en) * | 2021-12-27 | 2022-04-15 | 沈阳化工研究院有限公司 | Device for continuously preparing 3,3, 3-trifluoro-2, 2-dichloropropanal |
| CN114345255B (en) * | 2021-12-27 | 2023-09-12 | 沈阳化工研究院有限公司 | Device for continuously preparing 3, 3-trifluoro-2, 2-dichloropropionaldehyde |
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