CN105754658A - Method for sweating and preparing wax product with high normal hydrocarbon content and narrow carbon number distribution - Google Patents
Method for sweating and preparing wax product with high normal hydrocarbon content and narrow carbon number distribution Download PDFInfo
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- CN105754658A CN105754658A CN201410786121.3A CN201410786121A CN105754658A CN 105754658 A CN105754658 A CN 105754658A CN 201410786121 A CN201410786121 A CN 201410786121A CN 105754658 A CN105754658 A CN 105754658A
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Abstract
The invention discloses a method for sweating and preparing a wax product with a high normal hydrocarbon content and narrow carbon number distribution. According to the method, a sweating device is adopted; a constant high-temperature process is added at a proper temperature during a cooling process; the surface of a wax layer is uniformly fully paved with mixed solid particles when a crystallization process is over; and an air-flow is forced to pass through the wax layer during a sweating process so as to carry liquid components out. The method has advantages of low equipment investment, simple production process, and low operation cost, and causes no solvent pollution. The product has characteristics of high normal hydrocarbon content and narrow carbon number distribution, and can be used as a wax medium or a phase-transition wax product for a thermostat.
Description
Technical field
The invention belongs to special wax production technical field, particularly relate to a kind of diaphoresis and the method preparing high normal hydrocarbon content wax product.
Background technology
Pertroleum wax is the general name of all kinds of wax products that crude oil prepares after refining processing from wax-containing distillate, including liquid paraffin, paraffin and microwax.Pertroleum wax generally produces through steps such as dewaxing, removing oil, refining and molding.Being liquid under liquid paraffin room temperature, usual melting point of paraffin wax is 52 DEG C～74 DEG C, and the melt drop temperature of microwax is 65 DEG C～92 DEG C.
Dewaxing is the process preparing the slack wax that oil content is about 10～30% with lube cut for raw material, and dewaxing technique mainly has squeezing dewaxing and solvent dewaxing.Removing oil is the process of the waxy stone preparing oil content less than 2% with slack wax for raw material, and removing oil technique mainly has diaphoresis removing oil and solvent deoiling.Waxy stone, then through clay-filtered or hydrofinishing and molding, packaging and other steps, can obtain petroleum paraffin product.
Thermostat is also known as thermoregulator, and its effect is the water yield that the temperature automatic adjustment according to engine cooling water enters radiator, changes the range of DO of water, to regulate the heat-sinking capability of cooling system, it is ensured that electromotor works in suitable temperature range.
Conventional thermostat is waxtype thermostat, and general temperature control scope 10～12 DEG C is divided into 70,72,76,80,82 equal-specifications by nominal temperature.To thermostat range demands it is generally: the stroke of room temperature～nominal temperature+2 DEG C is less than 1mm, and within the scope of temperature control, (nominal temperature～nominal temperature+10 DEG C or nominal temperature+12 DEG C) stroke is more than 8mm.Temperature control interval such as the thermostat that nominal temperature is 72 DEG C is 72 DEG C～82 DEG C, it is desirable to when 74 DEG C, stroke is less than 1mm, and 72 DEG C～82 DEG C strokes are more than 8mm.
Waxtype thermostat is dependent on its Wax dielectric used and varies with temperature the motive power producing change in volume as output action, and its character is the determiner of waxtype thermostat performance.When commodity oil wax is directly used as the Wax dielectric of thermostat, can cause that systemic circulation is opened too early (stroke of room temperature～nominal temperature+2 DEG C scope inner push-rod is more than 1mm), make engine prewarming time lengthening；Simultaneously because temperature control scope inner push-rod stroke less (stroke of nominal temperature～nominal temperature+10 DEG C or nominal temperature+12 DEG C is less than 8mm), the water shortage of systemic circulation during engine work can be caused, cause engine overheat.
Variations in temperature is little in fusing or process of setting for phase-change material (PhaseChangeMaterial is called for short PCM), but the latent heat absorbing in only small temperature range or discharging is quite big, and this characteristic makes it be widely used in constant temperature, energy storage etc..Generally require that phase-change material has suitable phase transition temperature and bigger latent heat of phase change.
Compared with isoparaffin and cycloalkane, the latent heat of phase change of n-alkane wants big.Along with the increase of n-alkane chain length, its fusing point increases, and the fusing point of common n-alkane is-20～100 DEG C.It is the concentrated expression of the various components of its composition due to the fusing point of pertroleum wax, thus it is believed that the fusing point of pertroleum wax is arbitrarily adjustable within the scope of-20～100 DEG C, this is the sharpest edges of wax class phase-change material.This temperature province is also the scope the most often contacted in people's daily life simultaneously, and the stable chemical nature of wax, non-corrosiveness, free from environmental pollution.But commodity oil wax contains the component such as isoparaffin and cycloalkane, and carbon number distribution is wider, being directly used as latent heat during phase-change material less, phase transformation interval is wider.
Commodity oil wax is the hydrocarbon mixture of the n-alkane of multiple carbon number, isoparaffin, cycloalkane etc., its carbon number distribution wider (in fusing point commodity oil wax more than 70 DEG C, the content of the carbon number that content is the highest is typically in less than 10%), normal paraffin content relatively low (the normal hydrocarbon content of fusing point commodity oil wax more than 70 DEG C is typically in less than 70%).To some specific uses, it is desirable to there is the stroke of more than 8mm in the temperature range of 10～12 DEG C, phase-change wax product requirement has the latent heat of more than 200J/g in the transition temperature range of 15 DEG C, and commodity oil wax can not meet instructions for use, it is necessary to through separating processing further.
In pertroleum wax production technology, conventional separation manufacturing process mainly has distillation, solvent separation, diaphoresis separation etc..
Distillation separation method is to utilize the boiling point difference of different hydrocarbons to reach the purpose separated, the boiling range reducing distillation can effectively reduce the width of product carbon distribution, but normal paraffin content impact is little on improving, simultaneously because still-process needs pertroleum wax is heated to more than boiling point, consume substantial amounts of energy.
Solvent fractionation method is to utilize n-alkane to reach the purpose separated with isoparaffin different solubility in a solvent, it is possible to being effectively improved the normal paraffin content in product, but affect little on the width of carbon distribution, solvent dewaxing investment of production equipment is big simultaneously；Needing in production process to use solvent in a large number, recycling design needs to consume substantial amounts of energy；Containing benzene homologues in solvent, environment can be impacted；Solvent is inflammable, it is easy to cause production accident.
Diaphoresis separation method is to utilize the character that in wax, various component fusing points are different to be easily separated.In pertroleum wax, the molecular weight of various components and structure difference all can make its fusing point different.When being all n-alkane, the fusing point of the n-alkane that molecular weight is bigger is higher, and the fusing point of the n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will lower than n-alkane, and isomery degree more high-melting-point is more low.So the width that diaphoresis separation method can reduce product carbon distribution can improve again normal paraffin content.Diaphoresis separation method does not use solvent in process of production, and has only to the temperature more than by heating raw materials to fusing point in production process.
Compared with distillation separation method, owing to the melting temperature of various hydro carbons is far below boiling temperature, so the energy consumption of diaphoresis separation method is far below distillation separation method；Compared with solvent fractionation method, diaphoresis separation method does not use solvent, so on environment without impact.And the width that diaphoresis method can reduce product carbon distribution can improve again normal paraffin content, so for the wax product preparing high normal hydrocarbon content, narrow carbon number distribution, diaphoresis separation method all has superiority in production process and properties of product two.
Common diaphoresis separation method mainly comprises the steps that (1) preparation: pad water, is full of sweatbox ware plate lower space with water；(2) charging: load sweatbox when heating raw materials is in a liquid state to fusing point；(3) decrease temperature crystalline: raw material is slow cooling to below its fusing point 10～20 DEG C with the speed being not more than 4 DEG C/h.In temperature-fall period, the component that fusing point is the highest is first with thick fibrous crystal morphological crystal out, and along with wax layer temperature continues to reduce, other component is pressed the fusing point crystallization successively of order from high to low and formed solid；(4) intensification diaphoresis: after wax layer temperature reaches the cooling final temperature preset, bleed off pad water；Raw material is heated to lentamente default diaphoresis final temperature again.In intensification sweating effort, various components are successively fused into liquid by fusing point order from low to high and flow out (under wax), and wax layer residue (on wax) finally obtained is exactly the wax of high-melting-point, low oil-containing；(5) thick product is collected: intensification sweating effort terminates follow-up high-temperature of continuing rising, to melt on taking-up wax, is thick product；(6) product purification, molding, packaging: subtractive process generally adopts clay-filtered: will thick product melt after be warming up to predetermined temperature, add hargil and constant temperature stirring filtered to the scheduled time；Then through molding, pack product for the purpose of namely.
To common diaphoresis separation method, in intensification sweating effort, solids fraction (wax of higher melt) and liquid composition (wax of oil and relatively low melting point) are although two class components are respectively at solid and two kinds of phases of liquid, but also are difficult to be kept completely separate.Generally adopt the method extending sweating sessions and improving diaphoresis final temperature, but so can cause that production cycle length and product yield decline.
Common diaphoresis separation method can produce fusing point at the soap wax of 40 DEG C～60 DEG C and low melt point paraffin, is not suitable for producing fusing point wax product more than 70 DEG C.Test is had to show, when common diaphoresis separation method produces fusing point product more than 70 DEG C, carbon distribution width and normal paraffin content on diaphoresis later stage wax are unrelated with yield, namely the carbon distribution width on wax does not decline with the decline of yield, normal paraffin content does not also improve with the decline of yield, so common diaphoresis separation method is not suitable for preparing the wax product of the fusing point high normal hydrocarbon content more than 70 DEG C, narrow carbon number distribution.Only having part producer at present uses sweating process to produce the mill run such as soap wax and low melt point paraffin.
For many years, sweating process obtains some development at production equipment and process aspect, such as CN89214332(vertical square multipul sections spacer diaphoresis tank), CN94223980.6(ware type sudorific device), CN98233254.8(Paraffin sweating pot), CN200920033500.X(Novel paraffin sweating tank), CN201210508905.0(Efficient paraffin sweatbox), CN201320127680.4(tubular type paraffin deoiler) etc., diaphoresis production equipment has done improvement；CN91206202(high-efficient sweat pot for paraffin wax) on sweating process, done improvement.But these methods still can not produce the wax product of high normal hydrocarbon content, narrow carbon number distribution.
Diaphoresis separation method has that plant investment is few, production process is simple and the advantage such as operating cost is low, the more important thing is, diaphoresis separation method is to be currently known the unique solvent-free separation method for industrial-scale production petroleum paraffin product, in the today advocating green low-carbon, environmental protection and energy saving, the demand of the wax product that employing sweating process prepares high normal hydrocarbon content, narrow carbon number distribution is more urgent.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of diaphoresis and the method preparing high normal hydrocarbon content wax, narrow carbon number distribution product.Specifically with paraffin grade wax for raw material, adopt sweatbox, and on the basis of common diaphoresis method, the proper temperature in temperature-fall period increases the high temperature constant temperature stage, and increases the constant temperature stage of the cryogenic thermostat stage after crystallization process terminates and intensification sweating effort；Uniformly it is paved with the metallic particles of mixing on wax layer surface after crystallization process terminates, and in intensification sweating effort, force air flow through wax layer, carry out liquid composition, thus enhancing the separating effect of solids fraction and liquid composition and accelerating separating rate, the content making the carbon number that this solvent-free separation method of diaphoresis can produce fusing point normal hydrocarbon content more than 80% more than 70 DEG C, content is the highest is typically in the wax product of more than 15%, these products have bigger volumetric expansion in the temperature range of 10～12 DEG C, can be used as thermostat Wax dielectric；In the transition temperature range of 15 DEG C, latent heat of phase change, at more than 200J/g, can be used as phase-change wax product simultaneously.
A kind of diaphoresis of the present invention and the method preparing high normal hydrocarbon content, narrow carbon number distribution wax product, including herein below:
(1) in sweatbox, water is padded；
(2) with paraffin grade wax for raw material, after adding heat fusing, sweatbox is loaded；
(3) with the speed of 1.0 DEG C/h～3.0 DEG C/h, wax layer is cooled to proper temperature, high temperature constant temperature a period of time；The cooling final temperature of below raw material fusing point 5 DEG C～20 DEG C cryogenic thermostat a period of time it is cooled to again with the speed of 0.5 DEG C/h～2.5 DEG C/h；
(4) the pad water in sweatbox is discharged；Then with the ramp of 0.5 DEG C/h～2.5 DEG C/h, wax layer reaches constant temperature a period of time after predetermined temperature, then turns off diaphoresis；In sweating effort, wherein force air flow through wax layer；
(5) collect on wax；
(6) namely wax obtain high normal hydrocarbon content, narrow carbon number distribution wax product after refining, molding, packaging.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, the melting range of described paraffin grade wax is generally 60～74 DEG C, it is preferable that melting range is 66～74 DEG C.
In the method for the present invention, described narrow carbon number distribution refers to that in product carbon number distribution, the content of the highest carbon number of content is more than 15%.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, preferably in after raw material decrease temperature crystalline before intensification sweating effort (now wax layer is in solid state), 10～100 orders uniformly it are paved with, it is preferable that the solid particle of 20～50 orders on the surface of wax layer.The density of solid particle is generally higher than 4g/cm3, it is possible to it is the materials such as nonmetal, metal and alloy, it is preferable that density is 6～12g/cm3Metal and alloying pellet, low price metal material as more stable in chemical property such as zinc, ferrum, copper, lead and alloys thereof.Can selecting the solid particle of two or more different densities, the density contrast of two kinds of solid particle materials that density is adjacent is 1～5g/cm3.Two or more solid particles can be close by weight ratio mixing.Density described herein refers to the density of material constituting solid particle, and the density such as metallic particles refers to the density of metal, and non-particulate bulk density.Sweating effort can reclaim solid particle and clean to reuse after terminating.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described sweatbox is generally diaphoresis ware.Angle between diaphoresis ware ware plate and baffle plate is 90 °～170 °, it is preferred to 120 °～150 °.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described sweatbox is generally diaphoresis ware, and at wax layer dismountable sealing system added above and pressue device and/or increase vacuum equipment below wax layer.The described wax layer that forces air flow through is utilized in above wax layer to increase reduction pressure (air pressure) below pressure (air pressure) or wax layer, makes wax layer form what pressure differential realized up and down.Described pressure differential is generally 0.1～5.0 atmospheric pressure, it is preferred to 0.2～2.0 atmospheric pressure, in order to force air flow through wax layer.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, rate of temperature fall preferably 1.5 DEG C/h～2.5 DEG C/h before high temperature constant temperature section in described temperature-fall period.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, the proper temperature of the high temperature constant temperature section of described temperature-fall period is raw material fusing point-1.0 DEG C～fusing point+2.0 DEG C, it is preferred to raw material fusing point～fusing point+1.0 DEG C.The time of the high temperature constant temperature section of temperature-fall period is 0～4.0 hour, it is preferred to 0.01～4.0 hour, it is most preferred that be 1.0～4.0 hours.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described temperature-fall period rate of temperature fall after high temperature constant temperature section preferably 1.0 DEG C/h～2.0 DEG C/h.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described cooling final temperature is preferably below raw material fusing point 8 DEG C～15 DEG C.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, after being cooled to preset temperature, increases the constant temperature stage so that solid crystal is more abundant.The time in the cryogenic thermostat stage of crystallization process is 0～3.0 hour, it is preferred to 0.01～3.0 hour, it is most preferred that be 1.0～3.0 hours.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, the heating rate of described sweating effort is 1.0 DEG C/h～2.0 DEG C/h preferably.The predetermined temperature (i.e. final temperature) of described intensification is the fusing point 1 DEG C～10 DEG C lower than purpose product.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described intensification diaphoresis is to after producing the preset temperature of product, increase the constant temperature stage so that solids fraction separates more abundant with liquid composition, the time in constant temperature stage is 0～5.0 hour, it is preferably 0.01～5.0 hour, it is most preferred that be 1.0～5.0 hours.
In the method for the present invention, the heating rate of said wax layer and rate of temperature fall, it is possible to be controlled by air bath, water-bath, oil bath or other feasible modes, it is preferred to use water-bath or oil bath are controlled.When the mode such as water-bath or oil bath of employing controls heating rate and rate of temperature fall, chuck can be increased outside diaphoresis ware, chuck is connected with removable coil pipe and blood circulation, and blood circulation has programmed cooling/heating function, and blood circulation adds water or wet goods material 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 diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, described force air flow through wax layer and can implement in sweating effort any stage, it is preferable that implement at the initial stage of intensification.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, the described wax layer that forces air flow through is utilized in above wax layer to increase what air pressure realized, as can be 0.2～1.5 atmospheric pressure (gauge pressure) at the pressure that wax layer is applied above, and remain normal pressure below wax layer.
The diaphoresis of the present invention and prepare the method for high normal hydrocarbon content, narrow carbon number distribution wax product, the described wax layer that forces air flow through can also adopt and reduces air pressure below wax layer and realize.As remained normal pressure above preferred wax layer, and the pressure below wax layer is maintained-0.2～-0.8 atmospheric pressure (gauge pressure).
Common diaphoresis separation method is that the character utilizing various component fusing point different is easily separated production petroleum paraffin product, but for the fusing point petroleum paraffin product at about 70 DEG C, owing in raw material, the material such as cycloalkane and isoparaffin increases, chemical composition is complicated, cause the more tiny densification of crystals upon crystallization structure, discharging of liquid composition is formed huge filter flow resistance, and this results in and only is difficult to be kept completely separate by solids fraction and liquid composition in the common sweating effort of gravity natural separation.Therefore common diaphoresis removing oil technique can not produce fusing point wax product more than 70 DEG C.
For some specialities, such as thermostat Wax dielectric and phase-change wax, from the relatedness research of serviceability and chemical composition, only normal hydrocarbon content more than 80%, the content of carbon number that content is the highest more than 15% time, instructions for use could be met: namely for thermostat Wax dielectric, in the temperature range of 10～12 DEG C, have the stroke of more than 8mm；For phase-change wax, in the transition temperature range of 15 DEG C, there is the latent heat of more than 200J/g.With oil or pertroleum wax for raw material, prepare higher normal hydrocarbon content (such as more than 90%) and the product of narrower carbon number distribution (content more than 25% of the carbon number that content is the highest), serviceability increases limited, but processing cost is greatly increased, economically improper.And the normal hydrocarbon content of the commodity oil wax that fusing point is more than 70 DEG C is typically in less than 70%, and the content of the wherein carbon number that content is the highest is typically in less than 10%, therefore can not meet the instructions for use of these specialities.
The method that the present invention separates this solvent-free production pertroleum wax to make diaphoresis can prepare high normal hydrocarbon content, narrow carbon number distribution wax product, and normal paraffin content wider for carbon number distribution in common petroleum wax product chemical composition is relatively low is cause common petroleum wax product can not meet the reason that some special wax product technology requires, adopts diaphoresis separation method to reduce carbon number distribution width and improves normal paraffin content simultaneously；It is difficult to separate reason with liquid composition for solids fraction in common sweating effort, the method that wax layer carries out liquid composition is forced air flow through by adopting in sweating effort, simultaneously it is also preferred that increase the high temperature constant temperature stage in the process of cooling, and the method being uniformly paved with solid particle after the process of cooling terminates (namely before intensification sweating effort) on wax layer surface improves；Increase cryogenic thermostat stage of temperature-fall period and intensification diaphoresis to processes such as the constant temperature stages after preset temperature simultaneously.These measures make diaphoresis separation method to prepare normal hydrocarbon content is more than 80%, the content of carbon number that content is the highest is more than 15% wax product.
Research for pertroleum wax sweating effort shows, in sweating effort, liquid composition is discharged gradually along crystalline portion, is similar to the situation that liquid flows in capillary tube.Owing to fusing point is in the crystalline texture of the tiny densification of pertroleum wax of about 70 DEG C, the filter flow resistance that liquid composition is formed can be made sharply to increase, and this results in the wax product that only can not prepare high normal hydrocarbon content, narrow carbon number distribution by the common diaphoresis method of gravity natural separation process.
Increasing the high temperature constant temperature stage in temperature-fall period can make the crystallization of pertroleum wax bigger, the discharge being beneficial in sweating effort liquid composition.Research for pertroleum wax crystallization process shows, its chemical composition is the main factor determining crystal habit, and the condition of cooling procedure also can affect crystal habit simultaneously, particularly in the cooling condition at the temperature near fusing point, the impact of crystal habit is the most obvious.Fusing point at the pertroleum wax of about 70 DEG C when being cooled near fusing point, the n-alkane of larger molecular weight has formed crystallization, this partially crystallizable body can as the nucleus being subsequently formed crystallization, now increase the high temperature constant temperature stage, nucleus can be enable fully to increase, forming larger sized crystal, although this larger sized crystal is thick like that not as the crystallization of low melt point paraffin, but diaphoresis stage discharge liquid composition is also highly beneficial by the crystal structure of this increase.
After crystallization process terminates, uniformly it is paved with solid particle on wax layer surface in sweating effort, forces air flow through the discharge that wax layer is also beneficial in sweating effort liquid composition simultaneously.After crystallization process terminates (namely before sweating effort), now wax layer is in solid state, is uniformly paved with solid particle (preferred metallic particles) on wax layer surface.In sweating effort, wax layer raises and deliquescing with temperature, and metallic particles is big due to density, with slower velocity sedimentation, will form the thin channel run through up and down in wax layer under gravity, reduces filter flow resistance, is conducive to the quick discharge of liquid composition.Different densities is different with the sedimentation velocity of the solid particle of particle diameter, adopts the solid particle of mixing to can ensure that the passage having more discharge liquid composition in diaphoresis overall process at the differing heights of wax layer.Forcing air flow through wax layer simultaneously, carrying out liquid composition thus enhancing the separating effect of solids fraction and liquid composition.The cryogenic thermostat stage being aided with cooling procedure again makes solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction separate the methods such as more abundant with liquid composition, makes diaphoresis separation method can prepare high normal hydrocarbon content, narrow carbon number distribution wax product.
Angle between common diaphoresis ware ware plate and baffle plate is 90 °, and in sweating effort, wax layer shrinks, when forcing air flow through wax layer, produce sometimes air-flow slit flow through between wax layer and ware plate cross and without the phenomenon of wax layer.In the inventive method, increase the angle between diaphoresis ware ware plate and baffle plate, increase effectively the resistance between wax layer and ware plate, it can be ensured that air-flow passes through wax layer to carry out liquid composition.
The invention have the advantage that employing forces air flow through the method that wax layer carries out liquid composition, enhance the separating effect of solids fraction and liquid composition；By making hybrid solid particles settling in sweating effort, the thin channel running through wax layer up and down of formation, it is more favorable to the quick discharge of liquid composition；The wax product that high normal hydrocarbon content is more than 80% so that diaphoresis separation method can be prepared, the content of carbon number that content is the highest is more than 15%, these products can serve as thermostat Wax dielectric or phase-change wax product.The inventive method plant investment is low, production process is simple and operating cost contaminated environment low, solvent-free.
Accompanying drawing explanation
Fig. 1-2 is the stroke performance curve of thermostat push rod prepared by the wax product (I) prepared by embodiment of the present invention 1-2, (II) respectively.In figure, abscissa is temperature, and vertical coordinate is stroke.
Detailed description of the invention
Increase the angle between diaphoresis ware ware plate and baffle plate；Diaphoresis ware top connects dismountable sealing device and is connected with surge tank and compressor, and/or connects surge tank and vacuum pump in diaphoresis ware bottom；Increasing chuck outside diaphoresis ware, chuck is connected with removable coil pipe and blood circulation, and blood circulation has programmed cooling/heating function；With the suitable paraffin of fusing point for raw material, after adding heat fusing, load diaphoresis ware；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature is reduced near raw material melting temperature and constant temperature a period of time；Hybrid solid granule uniformly it is paved with preferably in wax layer surface；Heat cycles water improves wax layer temperature；Wax layer temperature reaches preset temperature and stops sweating effort after constant temperature a period of time.Sweating effort starts compressor with in wax layer malleation formed above, and/or start vacuum pump with in wax layer negative pressure formed below, in order to force air flow through wax layer；Wax is the wax product that normal hydrocarbon content is more than 80%, the content of carbon number that content is the highest is more than 15% after refining, molding, packaging.
1-2 illustrates diaphoresis of the present invention and the method preparing high normal hydrocarbon content, narrow carbon number distribution wax product by the following examples.
Embodiment 1
The present embodiment includes: (1) preparation, (2) charging, (3) cooling high temperature constant temperature cooling cryogenic thermostat crystallization, (4) intensification constant temperature diaphoresis, (5) thick product collection, (6) product purification and the process such as molding, packaging.
(1) preparation
The sealing system on diaphoresis ware (angle between diaphoresis ware ware plate and baffle plate is 120 °) top is connected with surge tank and compressor.Surge tank is installed in diaphoresis ware bottom and connects vacuum pump.
Diaphoresis ware ware plate bottom pad water.
By the chuck of diaphoresis ware and removable coil pipe with there is the blood circulation of program refrigerating/heating function be connected, with water for heat-conducting medium.
Start the heating function of blood circulation, make water-cycling-media be warming up to 78 DEG C.
(2) charging
With No. 72 semi-refined waxs, (Dalian Petrochemical Industry Company produces, and its character is: fusing point 72.5 DEG C；Normal paraffin content 68.25%；Maximum carbon number (C43) content 8.92%；DSC fusion range 22.67 DEG C, latent heat 182.36J/g) for raw material, after adding heat fusing, add diaphoresis ware.Coil pipe it is immersed in paraffin layer and fixes.
(3) cooling high temperature constant temperature cooling cryogenic thermostat crystallization
Start the refrigerating function of blood circulation, make wax layer temperature drop to 73.0 DEG C with the rate of temperature fall of 2.0 DEG C/h and constant temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Make wax layer temperature drop to 62.0 DEG C with the rate of temperature fall of 1.5 DEG C/h again and constant temperature carries out cryogenic thermostat in 2.0 hours, so that crystallization is more abundant.
Close the refrigerating function of closed loop system.
(4) intensification constant temperature diaphoresis
Discharge diaphoresis ware pad water.
The outlet of diaphoresis ware connects storage tank under wax；Connect diaphoresis ware sealing device for upper portion of annular；Start compressor and keep the stable maintenance normal pressure below 1.0～1.2 atmospheric pressure (gauge pressure), diaphoresis ware ware plate of buffering pressure inside the tank；Start circulation system function, make wax layer temperature be increased to 72.0 DEG C with the heating rate of 1.5 DEG C/h.
Stop compressor.Remove sealing device.
Open vacuum pump and keep buffering pressure inside the tank stable-0.4～-0.6 atmospheric pressure (gauge pressure), above wax layer, keeping normal pressure；Wax layer temperature is made to be increased to 75.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.5 DEG C/h so that the solids fraction in wax layer is sufficiently separated with liquid composition.
Stop vacuum pump, terminate diaphoresis degreasing process.
(5) thick product is collected
The diaphoresis ware outlet thick product storage tank of changing-over (I) is to receive on wax；Continue to raise the temperature to 90 DEG C of recirculated water, to melt on taking-up wax, be thick product (I).
(6) product purification and molding, packaging
Thick product is high normal hydrocarbon content, narrow carbon number distribution wax product (I) after clay-filtered, molding and packaging.
High normal hydrocarbon content, narrow carbon number distribution wax product (I) yield be that 14.6%(is relative to raw material 72# semi-refined wax).
High normal hydrocarbon content, narrow carbon number distribution wax product (I) character:
Fusing point 76.2 DEG C；Normal paraffin content 83.56%；Maximum carbon number (C44) content 16.27%.
The stroke temperature relation of the thermostat product push rod prepared by high normal hydrocarbon content, narrow carbon number distribution wax product (I) is as shown in Figure 1.It will be seen from figure 1 that thermostat push rod stroke when 74 DEG C, stroke is less than 1mm, between 72 DEG C～82 DEG C, stroke is more than 8mm, meets the technology requirement that nominal temperature is 72 DEG C of thermostats.
High normal hydrocarbon content, narrow carbon number distribution wax product (I) fusing point (DSC method): 77.51 DEG C；Latent heat of phase change: 218.52J/g；DSC fusion range: 12.38 DEG C.
Embodiment 2
The present embodiment includes: cryogenic thermostat crystallization that (1) preparation, (2) feed, (3) cooling high temperature constant temperature is lowered the temperature, (4) intensification constant temperature diaphoresis, (5) thick product are collected and metallic particles recovery, (6) product purification and the process such as molding, packaging.
(1) preparation
Screen out plumbous granule and the zinc granule of 20 order～40 orders, by weight for 1:1 mix homogeneously.
The sealing system on diaphoresis ware (angle between diaphoresis ware ware plate and baffle plate is 150 °) top is connected with surge tank and compressor.Surge tank is installed in diaphoresis ware bottom and connects vacuum pump.
Diaphoresis ware ware plate bottom pad water；The double-deck Medium speed filter paper of paving bottom diaphoresis ware；
By the diaphoresis ware of chuck and removable coil pipe with there is the blood circulation of program refrigerating/heating function be connected, with water for heat-conducting medium；
Start the heating function of blood circulation, make water-cycling-media be warming up to 78 DEG C.
(2) charging
With No. 72 semi-refined waxs (character is with embodiment 1) for raw material, add bottom after adding heat fusing and complete the diaphoresis ware of filter paper.Coil pipe it is immersed in paraffin layer and fixes.
(3) cooling high temperature constant temperature cooling cryogenic thermostat crystallization
Start the refrigerating function of blood circulation, make wax layer temperature drop to 73.0 DEG C with the rate of temperature fall of 2.0 DEG C/h and constant temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Make wax layer temperature drop to 62.0 DEG C with the rate of temperature fall of 1.5 DEG C/h again and constant temperature carries out cryogenic thermostat in 2.0 hours, so that crystallization is more abundant.
Close the refrigerating function of closed loop system.
(4) intensification constant temperature diaphoresis
Aforesaid lead, zinc hybrid particles uniformly it is paved with on wax layer surface.
Discharge diaphoresis ware pad water.
The outlet of diaphoresis ware connects storage tank under wax；Connect diaphoresis ware sealing device for upper portion of annular；Start compressor and keep the stable maintenance normal pressure below 1.0～1.2 atmospheric pressure (gauge pressure), diaphoresis ware ware plate of buffering pressure inside the tank；Start circulation system function, make wax layer temperature be increased to 72.0 DEG C with the heating rate of 1.5 DEG C/h；
Stop compressor.Remove sealing device.
Open vacuum pump and keep buffering pressure inside the tank stable in-0.4～-0.6 atmospheric pressure (gauge pressure), above wax layer, keeping normal pressure；Wax layer temperature is made to be increased to 75.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.5 DEG C/h so that the solids fraction in wax layer is sufficiently separated with liquid composition.
Stop vacuum pump, terminate diaphoresis degreasing process.
(5) thick product is collected and metallic particles recovery
The diaphoresis ware outlet thick product storage tank of changing-over (II) is to receive on wax；Continue to raise the temperature to 90 DEG C of recirculated water, to melt on taking-up wax, be thick product (II).
Collect the mixed metal particles on filter paper, clean, dry in order to reusing.
(6) product purification and molding, packaging
Thick product is high normal hydrocarbon content, narrow carbon number distribution wax product (II) after clay-filtered, molding and packaging.
High normal hydrocarbon content, narrow carbon number distribution wax product (II) yield be that 14.2%(is relative to raw material 72# semi-refined wax).
High normal hydrocarbon content, narrow carbon number distribution wax product (II) character:
Fusing point 76.5 DEG C；Normal paraffin content 86.35%；Maximum carbon number (C44) content 17.23%.
The stroke temperature relation of the thermostat product push rod prepared by high normal hydrocarbon content, narrow carbon number distribution wax product (II) is as shown in Figure 2.Figure it is seen that thermostat push rod stroke when 74 DEG C, stroke is less than 1mm, between 72 DEG C～82 DEG C, stroke is more than 8mm, meets the technology requirement that nominal temperature is 72 DEG C of thermostats.
High normal hydrocarbon content, narrow carbon number distribution wax product (II) fusing point (DSC method): 78.23 DEG C；Latent heat of phase change: 230.15J/g；DSC fusion range: 10.65 DEG C.
Be can be seen that by embodiment 1-2, diaphoresis of the present invention and the method preparing high normal hydrocarbon content, narrow carbon number distribution wax product, metallic particles is spread on wax layer surface to form the tiny duct running through wax layer up and down in sweating effort by adopting, and in sweating effort, force air flow through the methods such as wax layer, enhance the separating effect of solids fraction and liquid composition, the method that can use this solvent-free production paraffin of diaphoresis prepares the fusing point high normal hydrocarbon content more than 70 DEG C, narrow carbon number distribution wax product, and these can be used as thermostat Wax dielectric or phase-change wax product.
Claims (20)
1. diaphoresis and a method of preparing high normal hydrocarbon content, narrow carbon number distribution wax product, including herein below:
(1) in sweatbox, water is padded；
(2) with paraffin grade wax for raw material, after adding heat fusing, sweatbox is loaded；The fusing point of described paraffin grade wax is 60～74 DEG C；
(3) with the speed of 1.0 DEG C/h～3.0 DEG C/h, wax layer is cooled to proper temperature, high temperature constant temperature a period of time；It is cooled to final temperature again with the speed of 0.5 DEG C/h～2.5 DEG C/h, namely below raw material fusing point 5 DEG C～20 DEG C, and cryogenic thermostat a period of time；
(4) the pad water in sweatbox is discharged；Then with the ramp of 0.5 DEG C/h～2.5 DEG C/h, wax layer reaches constant temperature a period of time after predetermined temperature, then turns off diaphoresis；In sweating effort, wherein force air flow through wax layer；
(5) collect on wax；
(6) namely wax obtain high normal hydrocarbon content, narrow carbon number distribution wax product after refining, molding, packaging.
2. in accordance with the method for claim 1, it is characterised in that the fusing point of described paraffin grade wax is 66～74 DEG C.
3. in accordance with the method for claim 1, it is characterised in that in step (3) after raw material decrease temperature crystalline before step (4) intensification sweating effort, be uniformly paved with 10～100 orders on the surface of wax layer, it is preferable that the solid particle of 20～50 orders.
4. in accordance with the method for claim 3, it is characterised in that the density of described solid particle is more than 4g/cm3, it is preferred to 6～12g/cm3。
5. in accordance with the method for claim 4, it is characterised in that one or more in zinc, ferrum, copper, lead and alloy thereof of described solid particle.
6. in accordance with the method for claim 5, it is characterised in that described solid particle selects the solid particle of two or more different densities, and the density contrast of two kinds of solid particle materials that density is adjacent is 1～5g/cm3, the ratio that two or more solid particles are close by weight mixes.
7. in accordance with the method for claim 3, it is characterised in that described method also includes: sweating effort reclaims solid particle and cleans to reuse after terminating.
8. in accordance with the method for claim 1, it is characterized in that, the described wax layer that forces air flow through is utilized in above wax layer to increase reduction air pressure below air pressure and/or wax layer, wax layer is made to form what pressure differential realized up and down, described pressure differential is 0.1～5.0 atmospheric pressure, it is preferred to 0.2～2.0 atmospheric pressure.
9. in accordance with the method for claim 1, it is characterised in that the rate of temperature fall before high temperature constant temperature section of the temperature-fall period described in step (3) is 1.5 DEG C/h～2.5 DEG C/h, and the rate of temperature fall after high temperature constant temperature section is 1.0 DEG C/h～2.0 DEG C/h.
10. in accordance with the method for claim 1, it is characterised in that the proper temperature described in step (3) is raw material fusing point-1.0 DEG C～fusing point+2.0 DEG C, it is preferred to raw material fusing point～fusing point+1.0 DEG C.
11. in accordance with the method for claim 1, it is characterised in that the time of the high temperature constant temperature section described in step (3) is 0～4.0 hour, it is preferred to 0.01～4.0 hour, it is most preferred that be 1.0～4.0 hours.
12. in accordance with the method for claim 1, it is characterised in that the cooling final temperature described in step (3) is below raw material fusing point 8 DEG C～15 DEG C.
13. in accordance with the method for claim 1, it is characterised in that the time in step (3) described cryogenic thermostat stage is 0～3.0 hour, it is preferred to 0.01～3.0 hour, it is most preferred that be 1.0～3.0 hours.
14. in accordance with the method for claim 1, it is characterised in that the heating rate described in step (4) is 1.0 DEG C/h～2.0 DEG C/h.
15. in accordance with the method for claim 1, it is characterised in that the predetermined temperature heated up in step (4) is the fusing point 1 DEG C～10 DEG C lower than purpose product.
16. in accordance with the method for claim 1, it is characterised in that the time in the constant temperature stage described in step (4) is 0～5.0 hour, it is preferred to 0.01～5.0 hour, it is most preferred that be 1.0～5.0 hours.
17. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is implemented in sweating effort any stage, it is preferable that implement at the initial stage of intensification.
18. in accordance with the method for claim 8, it is characterised in that the described wax layer that forces air flow through is utilized in above wax layer to increase what air pressure realized: at wax layer 0.2～1.5 atmospheric gauge applied above, and remain normal pressure below wax layer.
19. in accordance with the method for claim 8, it is characterised in that the described wax layer that forces air flow through is utilized in below wax layer to reduce what pressure realized: keep normal pressure above wax layer, and the gauge below wax layer is maintained-0.2～-0.8 atmospheric pressure.
20. in accordance with the method for claim 1, it is characterised in that described sweatbox is diaphoresis ware, the angle between diaphoresis ware ware plate and baffle plate is 90 °～170 °, it is preferred to 120 °～150 °.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810725A (en) * | 2019-03-15 | 2019-05-28 | 上海焦耳蜡业有限公司 | A kind of wax sweating method based on particle |
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| CN1335372A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Production process of high-smelting point petroleum wax |
| CN1458242A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Waxy temperature sensing medium for automatic temperature regulating valve of showering |
| CN1458188A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Wax dielectric for thermosensitive switch |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1335372A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Production process of high-smelting point petroleum wax |
| CN1458242A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Waxy temperature sensing medium for automatic temperature regulating valve of showering |
| CN1458188A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Wax dielectric for thermosensitive switch |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109810725A (en) * | 2019-03-15 | 2019-05-28 | 上海焦耳蜡业有限公司 | A kind of wax sweating method based on particle |
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