CN105754653B - A kind of preparation method of atoleine - Google Patents
A kind of preparation method of atoleine Download PDFInfo
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- CN105754653B CN105754653B CN201410786164.1A CN201410786164A CN105754653B CN 105754653 B CN105754653 B CN 105754653B CN 201410786164 A CN201410786164 A CN 201410786164A CN 105754653 B CN105754653 B CN 105754653B
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Abstract
The invention discloses a kind of preparation method of atoleine.This method uses sweatbox, cooling procedure on wax layer surface is uniformly paved with metallic particles after terminating, and force air flow through wax layer in the sweating effort that heats up, carry out the isoparaffin in liquid, the separating rate of n-alkane and isoparaffin is accelerated, and enhances the separating effect of n-alkane and isoparaffin.The present invention forces the process of n-alkane and isoparaffin separation using increasing in the sweating stage, improves the content of n-alkane in atoleine product, and can shorten the production cycle.Compared with existing production method, the inventive method has the advantages that plant investment is low, production process is simple, operating cost is low, non-environmental-pollution.
Description
Technical field
The invention belongs to pertroleum wax production technical field, more particularly to a kind of preparation method of atoleine.
Background technology
The general name of the pertroleum wax obtained all kinds of wax products that are crude oil after refining is processed from wax-containing distillate, including liquid
Body paraffin, paraffin and microwax.Atoleine, abbreviation liquid wax, including atoleine and Paraffin liquid heavy, typically with C9~C20
N-alkane be main component, be liquid under normal temperature.Atoleine is to be taken off by straight-runs such as kerosene or diesel oil through molecular sieve
What ceroplastic or urea dewaxing process obtained, also can be by solvent deoiling or squeezing dewaxing-sweating de-oiling technique productions.Molecular sieve takes off
Wax and urea dewaxing are the main flow production technologies of current large-scale production atoleine product.
Dewaxing by molecular sieve process is using molecular sieve as adsorbent, and the n-alkane in kerosene distillate is separated, obtained
Obtain the n-alkane of high-purity, as atoleine product.Dewaxing by molecular sieve investment of production equipment is big, production process high energy consumption.
Urea dewaxing process is in the solution by urea and diesel oil（Or kerosene）N-alkane reaction generation in cut is solid
Body complex compound, then decompose complex compound at a higher temperature, obtain n-alkane, as atoleine product.Urea dewaxing
Investment of production equipment is big, production process is complicated, high energy consumption, there is chemical substance consumption.
Solvent deoiling process is in selective solvent（Acetone, benzene and toluene mixture；Or acetone, toluene；Or MEK,
Toluene）Solution in freeze, according to the difference of n-alkane and isoparaffin solubility, by after n-alkane crystallization with isomeric alkane
The method production atoleine product of hydrocarbon separation.Solvent deoiling technique has that production process is continuous, wax high income, finished product wax oil-containing
The advantages that amount can be very low, production cost is relatively low, but solvent deoiling investment of production equipment is big；It is raw when producing atoleine product
Production process needs to carry out at quite low temperatures；Need largely to use solvent in production process, recycling design needs to consume largely
Energy；Contain benzene homologues in solvent, environment can be impacted；Solvent is inflammable, easily causes production accident.
Squeezing dewaxing-sweating degreasing process is will first to squeeze that slack wax is made after kerosene or diesel oil distillate freezing, then through sweating
De-oiling produces atoleine product.
Squeezing dewaxing is the solvent-free dewaxing technique of early-stage development, and press dewaxing process is intermittently operated, labor intensity is big,
Low production efficiency, work situation harsh conditions selective to feedstock oil.
Sweating de-oiling method is separated using the wax property different with oily fusing point.Point of various components in pertroleum wax
Son amount Bu Tong can all make its fusing point different with structure.When being all n-alkane structure, the larger n-alkane of molecular weight melts
Point is higher, and the fusing point of the less n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will
Less than n-alkane, and isomery degree more high-melting-point is lower.So sweating de-oiling can improve normal paraffin content.Sweating de-oiling
Method only needs for raw material to be heated to temperature more than fusing point in process of production without using solvent, and in production process.
Common sweating degreasing process mainly includes the following steps that：（1）Preparation：Water is padded, is full of sweatbox with water
Ware plate lower space；（2）Charging：Load sweatbox when raw material is heated to more than fusing point being in a liquid state；（3）Decrease temperature crystalline：By original
Material progressively cools to below its fusing point 10~20 DEG C with the rate of temperature fall no more than 4 DEG C/h.In cooling procedure, various components are pressed
The order of fusing point from high to low crystallizes to form solid successively；（4）Heat up sweating：Temperature is terminated when wax layer temperature reaches default cooling
After degree, pad water is bled off；Raw material is slowly heated to default sweating final temperature again.It is various in the sweating effort that heats up
Component is successively fused into liquid by the order of fusing point from low to high and flowed out（Under wax）, the wax layer residue that finally obtains（On wax）
It is exactly high-melting-point, the wax of high normal paraffin content；（5）Crude product is collected：Heating sweating effort terminates follow-up high-temperature of continuing rising, with
Fusing is taken out on wax, as paraffin crude product；（6）Product purification, shaping, packaging：Subtractive process generally use is clay-filtered：Will
Predetermined temperature is warming up to after crude product fusing, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the scheduled time；Again through being molded, packing i.e.
For paraffin wax product.
To common sweating de-oiling method, dystectic n-alkane and the isoparaffin of low melting point in the sweating effort that heats up
Although two class components are respectively at solid and liquid condition, but also be difficult to be kept completely separate.To make the n-alkane of final products
Content meets the requirements, and generally use extends sweating sessions, and the method for improving sweating final temperature.Extending sweating sessions can cause
Production cycle is grown；Improving sweating final temperature can be such that part n-alkane is removed with isoparaffin, cause yield to decline.
Common sweating de-oiling method can produce the soap wax and low melting point stone of atoleine and fusing point at 40 DEG C~60 DEG C
Wax.Compared with the technique of the production atoleine such as dewaxing by molecular sieve, urea dewaxing, solvent deoiling, sweating de-oiling is intermittently operated,
And product yield is relatively low, the production cycle is longer, but sweating de-oiling method has that small investment, production process be simple, operating cost
Low advantage, still there is part producer at present using this method production soap wax and low melt point paraffin product.
For many years, sweating de-oiling method has obtained some development, such as CN89214332 in production equipment and process aspect（It is vertical
Formula square multipul sections spacer diaphoresis tank）、CN98233254.8（Paraffin sweating pot）、CN201320127680.4（Tubular type paraffin de-oiling
Device）Deng being improved in sweating de-oiling production equipment；CN91206202（A kind of high-efficient sweat pot for paraffin wax）In sweating de-oiling
Improved in technique；And CN201210415023.X（A kind of method for producing liquid wax）The methods of, but these methods are still deposited
The production cycle is long the shortcomings of.
Sweating de-oiling method is to be currently known unique solvent-free de-oiling technique for commercial scale petroleum paraffin product,
Advocating green, low-carbon energy-saving the concern for being increasingly subject to people today.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation method of atoleine, specifically with straight run
Kerosene distillate or straight(-run) diesel distillate are raw material, and Suitable ingredients are prepared through distillation；Using sweatbox, in common sweating de-oiling side
On the basis of method, the process of cooling terminate and constant temperature for a period of time after, be uniformly paved with metallic particles on wax layer surface, and
Heating and the sweating of constant temperature force air flow through wax layer during taking off isoparaffin, carry out the isoparaffin in liquid,
So as to accelerate the separating rate of solid-state n-alkane and liquid isoparaffin, and enhance solid-state n-alkane and liquid isomery
The separating effect of alkane, so improving the content of n-alkane in atoleine product and shortening the production cycle.
A kind of preparation method of atoleine of the present invention, including herein below：
（1）Load low-freezing liquid in sweatbox as hearth layer；
（2）Obtained kerosene or diesel oil distillate are distilled as raw material using paraffinic base crude oil, load sweatbox after fusing；
（3）Crystallized with 1.0 DEG C/h~4.0 DEG C/h speed cooling, when material temperature is down to predetermined temperature（Less than original
Expect 10 DEG C~20 DEG C of freezing point）Afterwards, constant temperature is for a period of time；
（4）Discharge the hearth layer in sweatbox（That is step（1）The low-freezing liquid of loading）, then with 0.5 DEG C/h
~3.0 DEG C/h speed be warming up to after predetermined temperature and constant temperature for a period of time after, stop sweating；Air-flow is forced in sweating effort
Pass through wax layer；
（5）Collect on wax；
（6）After refined, packaging it is atoleine product on wax.
In the atoleine production method of the present invention, step（1）The freezing point of the hearth layer of loading will be less than raw material and cool
The predetermined temperature of cooling.Described low-freezing liquid hearth layer can select the methanol and its aqueous solution, the ethanol and its aqueous solution,
The suitable liquid of glycol water, anti-icing fluid or other meet demands, preferably water-based liquid.
In the atoleine production method of the present invention, described paraffinic base crude oil distills obtained kerosene or diesel oil distillate
Initial boiling point is generally 170 DEG C~240 DEG C, and the end point of distillation is generally 250 DEG C~310 DEG C, normal paraffin content be generally 35wt%~
85wt%。
In the atoleine preparation method of the present invention, preferably after raw material decrease temperature crystalline and before the sweating effort that heats up,
The solid particle of 10~100 mesh, preferably 20~50 mesh is uniformly paved with the surface of wax layer.The density of solid particle is more than 4 g/
cm3, can be the materials such as nonmetallic, metal and alloy, preferred specific gravity is 6~12 g/cm3Metal and alloying pellet, as zinc,
The more stable low price metal material of the chemical property such as iron, copper, lead and its alloy.Two or more difference can be selected
The solid particle of proportion, various solid particles can similar ratio mixing in parts by weight, two kinds of adjacent solid particles of density
The density contrast of material is 1~5 g/cm3.Density described herein refers to the density for forming the material of solid particle, and non-solid
The heap density of particle.Sweating effort can reclaim solid particle and clean to reuse after terminating.
The atoleine preparation method of the present invention, described sweatbox are generally sweating ware, and added above in wax layer
Dismountable sealing system and pressue device and/or increase vacuum plant below wax layer.Described forces air flow through wax layer
It is utilized in increase pressure above wax layer and/or pressure is reduced below wax layer, wax layer is formed what pressure differential was realized up and down.Institute
The pressure differential stated is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force air flow through wax layer.
The atoleine preparation method of the present invention, the described speed preferably 2.0 DEG C/h~3.0 DEG C/h that cools.
The atoleine preparation method of the present invention, step（3）Described in the final temperature that cools be preferably shorter than raw material condensation point
12 DEG C~15 DEG C.
The atoleine preparation method of the present invention, described heating rate preferably 1.0 DEG C/h~2.0 DEG C/h.Temperature-rise period
In predetermined temperature（That is final temperature）For 2 DEG C~10 DEG C of the fusing point less than purpose product.
The present invention method in, the heating rate and rate of temperature fall of said wax layer, can by air bath, ethanol bath or
Other feasible modes are controlled.When controlling heating rate and rate of temperature fall using ethanol bath mode, it can increase outside sweating ware
Add chuck, chuck is connected with removable coil pipe and the circulatory system, and the circulatory system has program cooling/heating function, the circulatory system
The materials such as ethanol are added as circulatory mediator；Coil pipe is immersed in wax layer after charging, can make wax layer lifting/lowering temperature process faster,
Wax layer more uniform temperature.
The atoleine preparation method of the present invention, the described wax layer that forces air flow through can be any in heating sweating effort
Stage implements, and preferably implements at the initial stage of heating sweating effort.
The atoleine preparation method of the present invention, the described wax layer that forces air flow through are utilized in increase gas above wax layer
What pressure was realized, the pressure preferably applied above wax layer（Air pressure）For 0.2~2.0 atmospheric pressure（Gauge pressure）, and kept below wax layer
For normal pressure.
The atoleine preparation method of the present invention, the described wax layer that forces air flow through are utilized in reduction gas below wax layer
What pressure was realized, preferably remain normal pressure above wax layer, and the pressure below wax layer（Air pressure）It is maintained -0.2~-1.0 big
Air pressure（Gauge pressure）.
The atoleine preparation method of the present invention, constant temperature is for a period of time after preset temperature is cooled to.Increase the constant temperature stage
N-alkane sufficient crystallising can be made, the time in constant temperature stage is 0~3.0 hour, preferably 1.0~3.0 hours.
The atoleine preparation method of the present invention, after described heating sweating to preset temperature, preferably constant temperature is for a period of time.
The increased constant temperature stage can be sufficiently separated n-alkane and isoparaffin, and the time in constant temperature stage is 0~5.0 hour,
Preferably 1.0~3.0 hours.
Sweating de-oiling method is to carry out separation production liquid stone using the n-alkane property different with isoparaffin fusing point
Wax product, but in the sweating effort that heats up, the n-alkane of solid-state and the isoparaffin of liquid are difficult to be kept completely separate, and this is
Because n-alkane and isoparaffin are all nonpolar hydrocarbon molecules, intermolecular force is larger；The N-alkanes of solid-state simultaneously
Hydrocarbon is crystallized to form capillary pipe structure, there is stronger coating function to isoparaffin, and this is resulted in only by the general of gravity natural separation
N-alkane and isoparaffin are difficult to be kept completely separate in logical sweating effort.Generally use extends sweating sessions, improves sweating termination
The methods of temperature, makes the normal paraffin content of final products meet the technical requirements of Related product.But this can cause the production cycle
Length, atoleine product yield are low, have impact on extensive use of the sweating de-oiling method in terms of atoleine product is produced.
The present invention is difficult to completely by the further investigation to common sweating degreasing process for n-alkane and isoparaffin
The reason for separation, the method by carrying out liquid isoparaffin by wax layer using air-flow in the sweating effort that heats up, force
N-alkane and isoparaffin separation, so as to enhance the separating effect of n-alkane and isoparaffin；Simultaneously further preferably cold
But after cooling-thermostatical crystallization process terminates（I.e. before heating sweating effort）, now wax layer be in solid state, on wax layer surface
The method for being uniformly paved with solid particle is improved.In the sweating effort that heats up, as wax layer temperature raises, wax layer softens, by
In solid particle than great, it by with slower velocity sedimentation, forms in wax layer under gravity and runs through tiny up and down
Passage, the isoparaffin for being advantageous to liquid are quickly discharged.Different densities are different with the sinking speed of the solid particle of particle diameter, such as adopt
With the solid particle of mixing can ensure in the overall process that sweating takes off isoparaffin wax layer different height have it is more
The passage of liquid isoparaffin is discharged, is more beneficial for the quick discharge of oil.
It is an advantage of the invention that：By carrying out liquid isomery using forcing air flow through wax layer in the sweating effort that heats up
The method of alkane, the separating rate of n-alkane and isoparaffin is accelerated, enhance the separation of n-alkane and isoparaffin
Effect；Formed simultaneously during solid particles sediment upper and lower through the tiny duct of wax layer, be more favorable to liquid isomeric alkane
Hydrocarbon is quickly discharged.So as to reach the content of n-alkane in raising atoleine product and shorten the atoleine production cycle
Purpose.The inventive method plant investment is low, production process is simple and operating cost is low, solvent-free pollution environment, makes sweating de-oiling
The method more highly effective of this solvent-free production atoleine.
Embodiment
Sweating ware top connects dismountable sealing device and is connected with surge tank and compressor, and/or under sweating ware
Portion connects surge tank and vavuum pump；Increase chuck outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system
With program refrigerating/heating function；The component of the suitable boiling range prepared with distillation（Belong to kerosene distillate or diesel oil distillate）For raw material,
（After fusing）Load sweating ware, coil pipe submergence is in the feed and fixed；Wax layer heating-cooling speed is controlled with ethanol bath；Wax layer
Temperature is down to preset temperature and constant temperature for a period of time；Before the sweating effort that heats up, the solid of mixing is uniformly paved with wax layer surface
Particle；Heating and constant temperature sweating effort in utilize above wax layer formed malleation and/or wax layer negative pressure formed below with
Force air flow through wax layer and carry out the isoparaffin in liquid.After wax layer temperature reaches preset temperature and constant temperature for a period of time
Stop sweating.
1-3 illustrates the preparation method of fluid present invention paraffin by the following examples.
Embodiment 1
The present embodiment includes：（1）Preparation,（2）Charging,（3）Cooling-thermostatical crystallization,（4）Heating-constant temperature sweating,
（5）Crude product collection,（6）The process such as product purification and packaging.
（1）Preparation
Daqing crude oil virgin kerosene and diesel oil distillate are distilled, prepares the cut of 200 DEG C~310 DEG C of boiling range（N-alkane contains
Measure as 42.6%, -8.6 DEG C of condensation point）Raw material as the present embodiment.
The sealing system on sweating ware top is connected with surge tank and compressor.
Pad anti-icing fluid below sweating ware ware plate（Freezing point is less than -30 DEG C）.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with second
Alcohol is medium；Start the circulatory system, ethanol medium is adjusted to 0 DEG C.
（2）Charging
Using 200 DEG C~310 DEG C cuts of foregoing distillation preparation as raw material,（After fusing）Add sweating ware.Coil pipe is submerged
It is in raw material wax layer and fixed.
（3）Cooling-thermostatical crystallization
Start the refrigerating function of the circulatory system, wax layer temperature is dropped to -20.0 DEG C and perseverance with 2.0 DEG C/h rate of temperature fall
Warm 2.0 hours so that wax layer sufficient crystallising；Close the refrigerating function of the circulatory system.
（4）Heating-constant temperature sweating
Discharge sweating ware " pad water "（That is anti-icing fluid）.
Connect sweating ware sealing device for upper portion of annular；The outlet of sweating ware connects intermediate storage tank to receive under wax；Start compressor simultaneously
Keep buffering pressure inside the tank stable in 1.2~1.4 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation
System heating function, wax layer temperature is set to be increased to 0.0 DEG C and constant temperature 2.0 hours so that in wax layer with 2.0 DEG C/h heating rate
Isoparaffin be sufficiently separated with n-alkane（Sweating degreasing process total time is 12 hours）.
Stop compressor, terminate sweating degreasing process.
（5）Crude product is collected
The outlet of sweating ware is changed to connect crude product storage tank；Continue to raise circulatory system temperature to 20 DEG C, to melt taking-up wax
On, as atoleine crude product.
（6）Product purification and packaging
Crude product is atoleine product after clay-filtered, packaging.
Atoleine product property：
Boiling range：Initial boiling point, 210 DEG C, 98% recovered (distilled) temperature, 310 DEG C；Normal paraffin content, 94.96%.Meet heavy liquid
The Specifications requirement of paraffin certified products.
Product fusing point：7.2℃.
Embodiment 2
The present embodiment includes：（1）Preparation,（2）Charging,（3）Cooling-thermostatical crystallization,（4）Heating-constant temperature sweating,
（5）Crude product is collected and mixed metal particles reclaim,（6）The process such as product purification and packaging.
（1）Preparation
Daqing crude oil virgin kerosene and diesel oil distillate are distilled, prepares the cut of 200 DEG C~310 DEG C of boiling range（Property is the same as implementation
Example 1）Raw material as the present embodiment.
The lead particle and zinc particle of the mesh of 30 mesh~50 are screened out, by weight being 1：1 is well mixed.
The sealing system on sweating ware top is connected with surge tank and compressor.
Pad anti-icing fluid below sweating ware ware plate（Freezing point is less than -30 DEG C）；In sweating ware ware plate upper berth bilayer Medium speed filter paper.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with second
Alcohol is medium；Start the circulatory system, ethanol medium is adjusted to 0 DEG C.
（2）Charging
Using 200 DEG C~310 DEG C cuts of foregoing distillation preparation as raw material,（After heating fusing）Add bottom and complete filter paper
Sweating ware.Coil pipe is immersed in raw material wax layer and fixed.
（3）Cooling-thermostatical crystallization
Start the refrigerating function of the circulatory system, wax layer temperature is dropped to -20.0 DEG C and perseverance with 2.0 DEG C/h rate of temperature fall
Warm 2.0 hours so that wax layer sufficient crystallising；Foregoing lead, zinc hybrid particles are uniformly paved with wax layer surface；Close the circulatory system
Refrigerating function.
（4）Heating-constant temperature sweating
Discharge sweating ware " pad water "（Anti-icing fluid）.
Connect sweating ware sealing device for upper portion of annular；The outlet of sweating ware connects intermediate storage tank to receive under wax；Start compressor simultaneously
Keep buffering pressure inside the tank stable in 1.2~1.4 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation
System heating function, wax layer temperature is set to be increased to 0.0 DEG C and constant temperature 2.0 hours so that in wax layer with 2.0 DEG C/h heating rate
Isoparaffin be sufficiently separated with n-alkane（Sweating degreasing process total time is 12 hours）.
Stop compressor, terminate sweating degreasing process.
（5）Crude product is collected and metallic particles recovery
The outlet of sweating ware is changed to connect crude product storage tank；Continue to raise circulatory system temperature to 20 DEG C, to melt taking-up wax
On, as atoleine crude product.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
（6）Product purification and packaging
Crude product is atoleine product after clay-filtered, packaging.
Atoleine product property：
Boiling range：Initial boiling point, 210 DEG C, 98% recovered (distilled) temperature, 310 DEG C；Normal paraffin content, 97.18%.Meet heavy liquid
The Specifications requirement of paraffin certified products.
Product fusing point：7.4℃.
Embodiment 3
The present embodiment includes：（1）Preparation,（2）Charging,（3）Cooling-thermostatical crystallization,（4）Heating-constant temperature sweating,
（5）Crude product is collected and mixed metal particles reclaim,（6）The process such as product purification and packaging.
（1）Preparation
Shen north crude oil straight run kerosene fraction is distilled, prepares 170 DEG C~250 DEG C cuts of boiling range（Normal paraffin content is
45.6%, -16.3 DEG C of condensation point）Raw material as the present embodiment.
The copper particle and iron particle of the mesh of 20 mesh~40 are screened out, by weight being 1：1 is well mixed.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with second
Alcohol is medium；Start the circulatory system, ethanol medium is adjusted to 0 DEG C；Surge tank is installed and connects vavuum pump in sweating ware bottom.
Pad industrial alcohol below sweating ware ware plate；In sweating ware ware plate upper berth bilayer Medium speed filter paper.
（2）Charging
Using 170 DEG C~250 DEG C cuts of foregoing distillation preparation as raw material,（After fusing）Add the sweating that filter paper is completed in bottom
Ware.Coil pipe is placed in raw material wax layer and fixed；Coil pipe, chuck and the circulatory system are connected.
（3）Cooling-thermostatical crystallization
Using ethanol as heat-conducting medium, start the refrigerating function of the circulatory system, wax layer temperature is made with 3.0 DEG C/h rate of temperature fall
- 30.0 DEG C and constant temperature 2.0 hours are dropped to so that wax layer sufficient crystallising；Foregoing copper, iron hybrid particles are paved with wax layer surface；
Close the refrigerating function of the circulatory system.
（4）Heating-constant temperature sweating
Discharge sweating ware " pad water "（Industrial alcohol）.
The outlet of sweating ware connects intermediate storage tank to receive under wax；Start vavuum pump and keeping buffer pressure inside the tank it is stable-
0.5~-0.7 atmospheric pressure（Gauge pressure）, wax layer top keeps normal pressure；Start circulation system function, with 1.5 DEG C/h heating speed
Rate makes wax layer temperature be increased to -4.0 DEG C and constant temperature 3.0 hours so that the isoparaffin in wax layer is sufficiently separated with n-alkane
（Sweating degreasing process total time is 20 hours）.
Stop vavuum pump, terminate sweating effort.
（5）Crude product is collected and metallic particles recovery
The outlet of sweating ware is changed to connect crude product storage tank to receive on wax；Continue to raise circulatory system temperature to 20 DEG C, with
Fusing is taken out on wax, as atoleine crude product.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
（6）Product purification and packaging
Crude product is atoleine product after clay-filtered, packaging.
Atoleine product property：
Boiling range：Initial boiling point, 190 DEG C, 98% recovered (distilled) temperature, 250 DEG C；Normal paraffin content, 96.87%.Meet atoleine 2
The Specifications requirement of number product.
Product fusing point：-2.6℃.
Comparative example 1
Patent CN201210415023.X（A kind of method for producing liquid wax）Embodiment 1：
With grand celebration straight-run diesel oil（Boiling range：Initial boiling point, 220 DEG C；98% recovered (distilled) temperature, 310 DEG C；Normal paraffin content,
42.6%）For raw material；Using sweat tank sweating；Heating-up time is 25 hours, constant temperature 2 hours（Total heating sweating sessions are 27 small
When）；Product property is：Boiling range：Initial boiling point, 220 DEG C；98% recovered (distilled) temperature, 310 DEG C；Normal paraffin content 92.85%.
Comparing embodiment 1-3 and comparative example 1, it can be seen that the production method of fluid present invention paraffin, by wax layer table
Face spreads metallic particles so that wax layer forms the duct run through up and down in sweating effort, and uses and force in the sweating effort that heats up
Air-flow accelerates the separating rate of n-alkane and isoparaffin, and enhance n-alkane and isomery by the method for wax layer
The separating effect of alkane, improve the content of n-alkane in atoleine product（Examples 1 and 2 increase than comparative example 1 respectively
2.11 and 4.33 percentage points）And substantially shorten the atoleine production cycle（The time in heating sweating stage, embodiment 1
56% is shortened with 2 than comparative example 1）.
Claims (27)
1. a kind of preparation method of atoleine, including herein below：
（1）Load low-freezing liquid in sweatbox as hearth layer；
（2）Obtained kerosene or diesel oil distillate are distilled as raw material using paraffinic base crude oil, load sweatbox after fusing；
（3）Crystallized with the cooling of 1.0 DEG C/h~4.0 DEG C/h speed, when material temperature is down to predetermined temperature, i.e., less than raw material
After 10 DEG C~20 DEG C of condensation point, constant temperature is for a period of time；
（4）The hearth layer in sweatbox is discharged, is then warming up to 0.5 DEG C/h~3.0 DEG C/h speed after predetermined temperature simultaneously
Constant temperature for a period of time after, stop sweating；Wax layer is forced air flow through in sweating effort；
（5）Collect on wax；
（6）After refined, packaging it is atoleine product on wax；
Wherein, in step（3）After middle raw material slack wax decrease temperature crystalline, and in step（4）Before middle heating sweating effort, in wax layer table
Face is uniformly paved with solid particle.
2. in accordance with the method for claim 1, it is characterised in that step（4）Described in the wax layer that forces air flow through be to adopt
Increase air pressure above wax layer and/or air pressure is reduced below wax layer, wax layer is formed what pressure differential was realized up and down, it is described
Pressure differential is 0.1~5.0 atmospheric pressure.
3. in accordance with the method for claim 1, it is characterised in that the mesh number of the solid particle is 10~100 mesh.
4. in accordance with the method for claim 3, it is characterised in that the density of the solid particle is more than 4 g/cm3。
5. in accordance with the method for claim 3, it is characterised in that methods described also includes herein below：Sweating effort terminates
Solid particle is reclaimed afterwards and is cleaned to reuse.
6. in accordance with the method for claim 3, it is characterised in that the material of the solid particle be zinc, iron, copper, lead and its
One or more in alloy.
7. in accordance with the method for claim 6, it is characterised in that described solid particle selects two or more unlike materials
The solid particle of density, the ratio mixing similar in parts by weight of two or more solid particles.
8. in accordance with the method for claim 7, it is characterised in that two kinds of adjacent solids of two or more solid particle Midst densities
The density contrast of particle is 1~5 g/cm3。
9. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
10. in accordance with the method for claim 1, it is characterised in that step（3）Described in predetermined temperature be less than raw material condensation point
12 DEG C~15 DEG C.
11. in accordance with the method for claim 1, it is characterised in that described forces air flow through wax layer in heating sweating
Journey any stage is implemented.
12. in accordance with the method for claim 1, it is characterised in that the speed of the cooling is 2.0 DEG C/h~3.0 DEG C/h.
13. in accordance with the method for claim 1, it is characterised in that described heating rate is 1.0 DEG C/h~2.0 DEG C/h.
14. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Top increase air pressure realizes that the gauge applied above wax layer is 0.2~2.0 atmospheric pressure, and is remained below wax layer
Normal pressure.
15. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Lower section reduces air pressure and realized, normal pressure is remained above wax layer, and the gauge below wax layer is maintained -0.2~-1.0
Atmospheric pressure.
16. in accordance with the method for claim 1, it is characterised in that step（3）Described in constant temperature time be 0~3.0 small
When.
17. in accordance with the method for claim 1, it is characterised in that step（4）Described in constant temperature time be 0~5.0 small
When.
18. in accordance with the method for claim 1, it is characterised in that step（4）The predetermined temperature of middle heating is to be produced less than purpose
2 DEG C~10 DEG C of the fusing point of product.
19. according to right will its seek method described in 1, it is characterised in that described paraffinic base crude oil distill obtained kerosene or
The initial boiling point of diesel oil distillate be 170 DEG C~240 DEG C, the end point of distillation be 250 DEG C~310 DEG C, normal paraffin content be 35wt%~
85wt%。
20. in accordance with the method for claim 1, it is characterised in that step（1）The freezing point of the hearth layer of loading is less than raw material
The predetermined temperature of cooling down.
21. in accordance with the method for claim 20, it is characterised in that described hearth layer selects methanol, methanol aqueous solution, second
Alcohol, ethanol water, glycol water or anti-icing fluid.
22. in accordance with the method for claim 2, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
23. in accordance with the method for claim 3, it is characterised in that the mesh number of the solid particle is 20~50 mesh.
24. in accordance with the method for claim 4, it is characterised in that the density of the solid particle is 6~12 g/cm3。
25. in accordance with the method for claim 11, it is characterised in that described forces air flow through wax layer in heating reality at initial stage
Apply.
26. in accordance with the method for claim 16, it is characterised in that step（3）Described in constant temperature time be 1.0~3.0
Hour.
27. in accordance with the method for claim 17, it is characterised in that step（4）Described in constant temperature time be 1.0~3.0
Hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410786164.1A CN105754653B (en) | 2014-12-18 | 2014-12-18 | A kind of preparation method of atoleine |
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|---|---|---|---|
| CN201410786164.1A CN105754653B (en) | 2014-12-18 | 2014-12-18 | A kind of preparation method of atoleine |
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| CN105754653A CN105754653A (en) | 2016-07-13 |
| CN105754653B true CN105754653B (en) | 2017-11-24 |
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| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1111566C (en) * | 2000-10-26 | 2003-06-18 | 中国石油化工股份有限公司 | Wax compositions for thermosensitive switch |
| CN1176191C (en) * | 2002-05-15 | 2004-11-17 | 中国石油化工股份有限公司 | Wax dielectric for heating temperature control valve and its preparing method |
| CN1183203C (en) * | 2002-05-15 | 2005-01-05 | 中国石油化工股份有限公司 | Wax dielectric for thermosensitive switch |
| CN1243073C (en) * | 2003-10-24 | 2006-02-22 | 中国石油化工股份有限公司 | Temerature sensitive medium for wax temperature controlling valve and its prepn process |
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