CN105754658B - A kind of sweating and prepare high normal hydrocarbon content, the method for narrow carbon number distribution wax product - Google Patents
A kind of sweating and prepare high normal hydrocarbon content, the method for narrow carbon number distribution wax product Download PDFInfo
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- CN105754658B CN105754658B CN201410786121.3A CN201410786121A CN105754658B CN 105754658 B CN105754658 B CN 105754658B CN 201410786121 A CN201410786121 A CN 201410786121A CN 105754658 B CN105754658 B CN 105754658B
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Abstract
The invention discloses a kind of sweating and prepare high normal hydrocarbon content, the method for narrow carbon number distribution wax product.This method uses sweatbox, in the proper temperature increase high temperature constant temperature stage in temperature-fall period, is uniformly paved with the solid particle of mixing on wax layer surface after crystallization process terminates, and forces air flow through wax layer in sweating effort, carries out liquid composition.The inventive method has the advantages that plant investment is low, production process is simple and operating cost is low, solvent-free pollution；The characteristics of product has high normal hydrocarbon content, narrow carbon number distribution, can be used as thermostat Wax dielectric or phase transformation wax product.
Description
Technical field
The invention belongs to special wax production technical field, more particularly to a kind of sweating and the production of high normal hydrocarbon content wax is prepared
The method of product.
Background technology
The general name of the pertroleum wax obtained all kinds of wax products that are crude oil after refining processing from wax-containing distillate, including liquid
Body paraffin, paraffin and microwax.Pertroleum wax is general to be produced through steps such as dewaxing, de-oiling, refined and shapings.Under atoleine normal temperature
For liquid, 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 that the slack wax that oil content is 10~30% or so is prepared by raw material of lube cut, dewaxing technique
Mainly there is squeezing to dewax and solvent dewaxing.De-oiling is the process that waxy stone of the oil content below 2% is prepared by raw material of slack wax, de-oiling
Technique mainly has sweating de-oiling and solvent deoiling.Waxy stone is again through clay-filtered or hydrofinishing and shaping, packaging and other steps, you can
Obtain petroleum paraffin product.
Thermostat is also known as thermosistor, and it is the water for entering radiator according to the temperature automatic adjustment of engine cooling water that it, which is acted on,
Amount, changes the range of DO of water, to adjust the heat-sinking capability of cooling system, it is ensured that engine work within the scope of suitable temperature
Make.
Conventional thermostat is waxtype thermostat, general 10~12 DEG C of temperature control scope, be divided into 70 by nominal temperature, 72,76,
80th, 82 equal-specification.Typically it is to thermostat range demands：The stroke of normal temperature~+2 DEG C of nominal temperature is less than 1 mm, temperature control scope
It is interior（+ 12 DEG C of nominal temperature~+10 DEG C of nominal temperature or nominal temperature）Stroke is more than 8mm.Such as the section temperature that nominal temperature is 72 DEG C
The temperature control interval of device is 72 DEG C~82 DEG C, it is desirable to which stroke is less than 1 mm at 74 DEG C, and 72 DEG C~82 DEG C strokes are more than 8mm.
Waxtype thermostat is that the original for producing Volume Changes as output action is varied with temperature by the Wax dielectric used in it
Power, its property is the determinant of waxtype thermostat performance.When commodity oil wax is directly used as the Wax dielectric of thermostat, it can lead
Systemic circulation is caused to open too early（The stroke of normal temperature~+2 DEG C of nominal temperature scope inner push-rod is more than 1 mm）, make the engine prewarming time
Extension；Simultaneously because temperature control scope inner push-rod stroke is smaller（+ 12 DEG C of nominal temperature~+10 DEG C of nominal temperature or nominal temperature
Stroke is less than 8mm）, the water shortage of systemic circulation, causes engine overheat when can cause engine work.
Phase-change material（Phase Change Material, abbreviation PCM）Temperature change is not in fusing or process of setting
Greatly, but in the temperature range of very little the latent heat for absorbing or discharging is quite big, and this characteristic makes it in terms of constant temperature, energy storage
It is widely used.Typically require that phase-change material has appropriate phase transition temperature and larger latent heat of phase change.
Compared with isoparaffin and cycloalkane, the latent heat of phase change of n-alkane is big.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.Because the fusing point of pertroleum wax is the various components of its composition
Concentrated expression, thus can consider that the fusing point of pertroleum wax is any adjustable in the range of -20~100 DEG C, this is wax class phase transformation material
The sharpest edges of material.The temperature province is also the scope most often contacted in people's daily life simultaneously, and the chemical property of wax
It is stabilization, non-corrosiveness, free from environmental pollution.But commodity oil wax contains the components such as isoparaffin and cycloalkane, and carbon number distribution compared with
Width, it is smaller to be directly used as latent heat during phase-change material, and phase transformation is interval wider.
Commodity oil wax is the hydrocarbon mixture of the n-alkane, isoparaffin, cycloalkane of a variety of carbon numbers etc., its carbon number point
Cloth is wider（The content of content highest carbon number is general below 10% in commodity oil wax of the fusing point more than 70 DEG C）, N-alkanes
Hydrocarbon content is relatively low（The normal hydrocarbon content of commodity oil wax of the fusing point more than 70 DEG C is general below 70%）.To some special use
On the way, it is desirable to have more than 8mm stroke, phase transition temperature model of the phase-change wax product requirement at 15 DEG C within the temperature range of 10~12 DEG C
There is more than 200J/g latent heat in enclosing, commodity oil wax can not meet use requirement, it is necessary to through further separation processing.
In terms of pertroleum wax production technology, conventional separation manufacturing process mainly has distillation, solvent separation, sweating separation
Deng.
Distillation separation method is the purpose that separation is reached using the boiling point difference of different hydrocarbons, and the boiling range for reducing distillation can be with
The effectively width of reduction product carbon distribution, but little on improving normal paraffin content influence, simultaneously because still-process need by
Pertroleum wax is heated to more than boiling point, consumes substantial amounts of energy.
Solvent fractionation method is that the different solubility using n-alkane with isoparaffin in a solvent reaches the mesh separated
, the normal paraffin content in product can be effectively improved, but little is influenceed on the width that carbon is distributed, while solvent dewaxing is produced
Equipment investment is big；Need largely to use solvent in production process, recycling design needs to consume substantial amounts of energy；Contain benzene in solvent
It is thing, environment can be impacted；Solvent is inflammable, easily causes production accident.
Sweating separation method is separated using the different property of various component fusing points in wax.Various groups in pertroleum wax
The molecular weight divided Bu Tong can all make its fusing point different with structure.When being all n-alkane, the larger n-alkane of molecular weight
Fusing 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
To be less than n-alkane, and isomery degree more high-melting-point is lower.So sweating separation method can reduce the distribution of product carbon
Width can improve normal paraffin content again.Sweating separation method is in process of production without using in solvent, and production process
Need to be heated to raw material into temperature more than fusing point.
Compared with distillation separation method, because the melting temperature of various hydro carbons is far below boiling temperature, so sweating is separated
The energy consumption of method is far below distillation separation method；Compared with solvent fractionation method, sweating separation method is without using solvent, so right
Environment is without influence.And diaphoresis can reduce product carbon distribution width can improve normal paraffin content again, so to preparation
For high normal hydrocarbon content, the wax product of narrow carbon number distribution, sweating separation method at production process and the aspect of properties of product two all
It is advantageous.
Common sweating separation method is mainly included the following steps that：（1）Preparation：Water is padded, sweatbox is full of 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 is slow cooling to below its fusing point 10~20 DEG C to be not more than 4 DEG C/h speed.In temperature-fall period, fusing point highest component
First come out with thick fibrous crystal morphological crystal, as wax layer temperature continues to reduce, other components by fusing point from high to low
Crystallization forms solid to order successively；（4）Heat up sweating：After wax layer temperature reaches default cooling final temperature, pad is bled off
Water；Raw material is slowly heated to default sweating final temperature again.In heating sweating effort, various components are by fusing point by low
Successively liquid is fused into high order and is flowed out（Under wax）, the wax layer residue finally obtained（On wax）Be exactly high-melting-point, it is low
The wax of oil-containing；（5）Crude product is collected：Heating sweating effort terminates follow-up high-temperature of continuing rising, is taken out with melting on wax, is thick production
Product；（6）Product purification, shaping, packaging：Subtractive process is generally using clay-filtered：Pre- constant temperature is warming up to after crude product is melted
Degree, adds carclazyte and constant temperature stirs to the scheduled time filtering；It is again purpose product through shaping, packaging.
To common sweating separation method, the solids fraction in heating sweating effort（The wax of higher melt）And liquid composition
（Oil and compared with the wax of low melting point）Although two class components are respectively at two kinds of phases of solid and liquid, but also are difficult to be kept completely separate.
Generally using the method for extending sweating sessions and improving sweating final temperature, but it can so cause production cycle length and product yield
Decline.
Common sweating separation method can produce soap wax and low melt point paraffin of the fusing point at 40 DEG C~60 DEG C, be not suitable for production
Wax product of the fusing point more than 70 DEG C.There is experiment to show, when common sweating separation method produces product of the fusing point more than 70 DEG C,
The carbon dispersion of distribution and normal paraffin content on sweating later stage wax is unrelated with yield, i.e., the carbon dispersion of distribution on wax is not with yield
Decline and decline, normal paraffin content is not also improved with the decline of yield, so common sweating separation method is not suitable for preparing
High normal hydrocarbon content of the fusing point more than 70 DEG C, the wax product of narrow carbon number distribution.Only part producer uses sweating process at present
Produce the mill run such as soap wax and low melt point paraffin.
For many years, sweating process has obtained some development, such as CN89214332 in production equipment and process aspect（Vertical type square
Shape multipul sections spacer diaphoresis tank）、CN94223980.6（Ware type sudorific device）、CN98233254.8（Paraffin sweating pot）、
CN200920033500.X（Novel paraffin sweating tank）、CN201210508905.0（A kind of Efficient paraffin sweatbox）、
CN201320127680.4（Tubular type paraffin deoiler）Deng being improved in sweating production equipment；CN91206202（It is a kind of
High-efficient sweat pot for paraffin wax）Improved on sweating process.But these methods can not still produce high normal hydrocarbon content, narrow carbon number point
The wax product of cloth.
Sweating separation method has that plant investment is few, production process is simple and the low advantage of operating cost, it is often more important that,
Sweating separation method is to be currently known unique solvent-free separation method for commercial scale petroleum paraffin product, green advocating
Color low-carbon, today of environmental protection and energy saving, high normal hydrocarbon content, the demand of the wax product of narrow carbon number distribution are prepared more using sweating process
Plus it is urgent.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of sweating and prepares high normal hydrocarbon content wax, narrow carbon number distribution
The method of product.Specifically using paraffin grade wax as raw material, using sweatbox, and on the basis of common sweating method,
The proper temperature increase high temperature constant temperature stage in temperature-fall period, and increase cryogenic thermostat stage after crystallization process terminates and
The constant temperature stage of heating sweating effort；Uniformly it is paved with the metallic particles of mixing on wax layer surface after crystallization process terminates, and
Wax layer is forced air flow through in heating sweating effort, liquid composition is carried out, so as to enhance solids fraction and liquid composition
Separating effect simultaneously accelerates separating rate, this solvent-free separation method of sweating is produced fusing point more than 70 DEG C just
The general wax product more than 15% of content of structure hydrocarbon content more than 80%, content highest carbon number, these products are at 10~12 DEG C
Within the temperature range of have larger volumetric expansion, can be used as thermostat Wax dielectric；Simultaneously in 15 DEG C of transition temperature range
Latent heat of phase change can be used as phase transformation wax product in more than 200J/g.
A kind of sweating of the present invention and high normal hydrocarbon content, the method for narrow carbon number distribution wax product are prepared, it is including following interior
Hold：
（1）Water is padded in sweatbox；
（2）Using paraffin grade wax as raw material, load sweatbox after heating fusing；
（3）Wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h speed, high temperature constant temperature is for a period of time；Again with
0.5 DEG C/h~2.5 DEG C/h speed is cooled to 5 DEG C~20 DEG C below raw material fusing point of cooling final temperature, and cryogenic thermostat one
The section time；
（4）Discharge the pad water in sweatbox；Then heated up with 0.5 DEG C/h~2.5 DEG C/h speed, wax layer reaches predetermined
Constant temperature for a period of time, then stops sweating after temperature；Wax layer is wherein forced air flow through in sweating effort；
（5）Collect on wax；
（6）On wax high normal hydrocarbon content, narrow carbon number distribution wax product are obtained after refined, shaping, packaging.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, the paraffin grade wax
Melting range be generally 60~74 DEG C, preferably fusing point scope is 66~74 DEG C.
In the method for the present invention, described narrow carbon number distribution refers to that the content of content highest carbon number in product carbon number distribution is
More than 15%.
The present invention sweating and prepares in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, preferably raw material drop
After temperature crystallization and before heating sweating effort（Now wax layer is in solid state）, uniformly it is paved with 10 on the surface of wax layer~
The solid particle of 100 mesh, preferably 20~50 mesh.The density of solid particle is generally higher than 4 g/cm3, can be nonmetallic, metal
And the material such as alloy, preferred density is 6~12 g/cm3Metal and alloying pellet, such as zinc, iron, copper, lead and its alloy
Learn the more stable low price metal material of property.The solid particle of two or more different densities, density can be selected
The density contrast of two kinds of adjacent solid particle materials is 1~5 g/cm3.Two or more solid particles can be close by weight
Ratio mixing.Density described herein refers to the density for constituting the material of solid particle, and the density of such as metallic particles refers to gold
The density of category, and non-particulate heap density.Sweating effort can reclaim solid particle and clean to reuse after terminating.
The sweating of the present invention and prepares in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described sweating is filled
Put generally sweating ware.Angle between sweating ware ware plate and baffle plate is 90 °~170 °, preferably 120 °~150 °.
The sweating of the present invention and prepares in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described sweating is filled
Generally sweating ware is put, and is increased in wax layer dismountable sealing system added above and pressue device and/or below wax layer
Vacuum plant.The described wax layer that forces air flow through is utilized in increase pressure above wax layer（Air pressure）Or reduction pressure below wax layer
Power（Air pressure）, make to form what pressure differential was realized above and below wax layer.Described pressure differential is generally 0.1~5.0 atmospheric pressure, is preferably
0.2~2.0 atmospheric pressure, to force air flow through wax layer.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described cooling
Rate of temperature fall preferably 1.5 DEG C/h~2.5 DEG C/h in journey before high-temperature constant temperature section.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described cooling
The proper temperature of the high-temperature constant temperature section of journey is -1.0 DEG C of raw material fusing point~+2.0 DEG C of fusing point, preferably raw material fusing point~fusing point+1.0
℃.The time of the high-temperature constant temperature section of temperature-fall period be 0~4.0 hour, preferably 0.01~4.0 hour, most preferably 1.0~
4.0 hour.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described cooling
Rate of temperature fall of the journey after high-temperature constant temperature section preferably 1.0 DEG C/h~2.0 DEG C/h.
The sweating of the present invention and prepares in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described cooling end
Only temperature is preferably 8 DEG C~15 DEG C below raw material fusing point.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, it is default being cooled to
After temperature, the increase constant temperature stage is so that solid crystal is more abundant.The time in the cryogenic thermostat stage of crystallization process is 0~3.0 small
When, preferably 0.01~3.0 hour, most preferably 1.0~3.0 hours.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described sweating
The heating rate of journey preferably 1.0 DEG C/h~2.0 DEG C/h.The predetermined temperature of the heating（That is final temperature）For less than purpose product
1 DEG C~10 DEG C of fusing point.
The sweating of the present invention and prepares in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described heating is sent out
After sweat to the preset temperature for producing product, the increase constant temperature stage is so that solids fraction separates more abundant, constant temperature rank with liquid composition
The time of section is 0~5.0 hour, most preferably preferably 0.01~5.0 hour, 1.0~5.0 hours.
In the method for the present invention, the heating rate and rate of temperature fall of said wax layer can pass through air bath, water-bath, oil bath
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath are controlled.Using the mode control such as water-bath or oil bath
When heating rate processed and rate of temperature fall, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, followed
Loop system has program cooling/heating function, and the circulatory system adds the material such as water or oil and is used as circulatory mediator；By coil pipe after charging
Be immersed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described pressure gas
Stream can be implemented by wax layer in sweating effort any stage, preferably implement initial stage in heating.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described pressure gas
Flow and be utilized in what increase air pressure above wax layer was realized by wax layer, the pressure that can such as apply above wax layer is 0.2~1.5
Atmospheric pressure（Gauge pressure）, and remain normal pressure below wax layer.
The present invention sweating and prepare in high normal hydrocarbon content, the method for narrow carbon number distribution wax product, described pressure gas
Stream can also be used by wax layer reduces air pressure realization below wax layer.Normal pressure is remained above preferred wax layer, and in wax layer
The pressure of lower section is maintained -0.2~-0.8 atmospheric pressure（Gauge pressure）.
Common sweating separation method is to carry out separation production petroleum paraffin product using the different property of various component fusing points,
But the petroleum paraffin product for fusing point at 70 DEG C or so, because the material such as cycloalkane and isoparaffin increases in raw material, chemistry
Composition is complicated, causes the more tiny densification of crystals upon crystallization structure, the discharge to liquid composition forms huge filter flow resistance power, this
Result in and only be difficult to be kept completely separate with liquid composition by solids fraction in the common sweating effort of gravity natural separation.Therefore it is common
Sweating de-oiling technique can not produce wax product of the fusing point more than 70 DEG C.
For some specialities, such as thermostat Wax dielectric and phase-change wax, from the association of performance and chemical composition
Journal of Sex Research understands, only normal hydrocarbon content more than 80%, the content of content highest carbon number more than 15% when, could meet makes
With requiring：I.e. for thermostat Wax dielectric, there is more than 8mm stroke within the temperature range of 10~12 DEG C；To phase-change wax
For, there is more than 200J/g latent heat in 15 DEG C of transition temperature range.Using oil or pertroleum wax as raw material, prepare higher just
Structure hydrocarbon content（Such as more than 90%）With narrower carbon number distribution（The content more than 25% of content highest carbon number）Product, performance
Upper increase is limited, but processing cost is greatly increased, economically improper.And the positive structure of commodity oil wax of the fusing point more than 70 DEG C
Hydrocarbon content is general below 70%, and the content of wherein content highest carbon number is general below 10%, therefore can not meet these
The use requirement of specialities.
The present invention in order that sweating separation it is this it is solvent-free production pertroleum wax method can prepare high normal hydrocarbon content, it is narrow
Carbon number distribution wax product, for carbon number distribution in common petroleum wax product chemical composition is wider and normal paraffin content it is relatively low be to make
The reason for some special wax product technologies are required can not be met into common petroleum wax product, carbon number is reduced using sweating separation method
The dispersion of distribution improves normal paraffin content simultaneously；It is difficult to separate original with liquid composition for solids fraction in common sweating effort
Cause, the method that wax layer carries out liquid composition is forced air flow through by being used in sweating effort, while further preferably in cooling
Increase the high temperature constant temperature stage in temperature-fall period, and after the process of cooling terminates（I.e. before heating sweating effort）On wax layer surface
The uniform method for being paved with solid particle is improved；Increase simultaneously temperature-fall period the cryogenic thermostat stage and heating sweating to default
The processes such as the constant temperature stage after temperature.These measures allow sweating separation method to prepare normal hydrocarbon content more than 80%, content
Wax product of the content of highest carbon number more than 15%.
Research for pertroleum wax sweating effort shows that liquid composition is gradually discharged along crystalline portion in sweating effort
, situation about being flowed similar to liquid in capillary.Because fusing point is in 70 DEG C or so of the tiny fine and close crystallization knot of pertroleum wax
Structure, can make to increased dramatically the filter flow resistance power of liquid composition formation, this results in the common hair for only leaning on gravity natural separation process
Sweat method can not prepare high normal hydrocarbon content, the wax product of narrow carbon number distribution.
Increasing the high temperature constant temperature stage in temperature-fall period can make the crystallization of pertroleum wax bigger, beneficial to liquid in sweating effort
The discharge of component.Research for pertroleum wax crystallization process shows that its chemical composition is the main factor for determining crystal habit,
The condition of cooling procedure can also influence crystal habit simultaneously, and especially the cooling condition at the temperature near fusing point is to crystalline
The influence of state is most obvious.Fusing point is when 70 DEG C or so of pertroleum wax is being cooled near fusing point, the n-alkane of larger molecular weight
Form crystallization to separate out, this partially crystallizable body can now increase the high temperature constant temperature stage as the nucleus for being subsequently formed crystallization, can
So that nucleus can fully increase, larger sized crystal is formed, although this larger sized crystal is not so good as low melt point paraffin
Crystallization it is thick like that, but this increase crystal structure to the sweating stage discharge liquid composition be also highly beneficial.
Uniformly be paved with solid particle on wax layer surface after crystallization process terminates forces air-flow to lead in sweating effort simultaneously
Cross the discharge that wax layer is also beneficial to liquid composition in sweating effort.After crystallization process terminates（I.e. before sweating effort）, now wax
Layer is in solid state, and solid particle is uniformly paved with wax layer surface（It is preferred that metallic particles）.In sweating effort, wax layer is with temperature
Degree is raised and softened, and metallic particles is big due to density, under gravity by with slower velocity sedimentation, is formed in wax layer
The thin channel run through down, reduces filter flow resistance power, is conducive to the quick discharge of liquid composition.The solid of different densities and particle diameter
The sinking speed of particle is different, using the solid particle of mixing can ensure in sweating overall process wax layer different height all
There is the passage of more discharge liquid composition.Wax layer is forced air flow through simultaneously, carries out liquid composition to enhance solid-state
The separating effect of component and liquid composition.Being aided with the cryogenic thermostat stage of cooling procedure again makes solid crystal more abundant, Yi Jifa
The constant temperature stage of sweat process makes solids fraction separate the method such as more abundant with liquid composition, sweating separation method is prepared height
Normal hydrocarbon content, narrow carbon number distribution wax product.
Commonly angle between sweating ware ware plate and baffle plate is 90 °, and wax layer is shunk in sweating effort, when forcing air flow through wax
Layer when, sometimes produce air-flow through gap between wax layer and ware plate flow through and without the phenomenon of wax layer.In the inventive method, increase
Angle between sweating ware ware plate and baffle plate, increase effectively the resistance between wax layer and ware plate, it can be ensured that air-flow by wax layer with
Carry out liquid composition.
It is an advantage of the invention that：Using the method that wax layer carries out liquid composition is forced air flow through, solid-state group is enhanced
Divide the separating effect with liquid composition；By settling hybrid solid particle in sweating effort, wax layer is run through above and below formation
Thin channel, be more favorable to the quick discharge of liquid composition；So that sweating separation method can prepare high normal hydrocarbon
Content is more than 80%, wax product of the content of content highest carbon number more than 15%, and these products may be used as thermostat use
Wax dielectric or phase transformation wax product.The inventive method plant investment is low, production process is simple and operating cost is low, solvent-free pollution ring
Border.
Brief description of the drawings
Fig. 1-2 is the wax product prepared by 1-2 of the embodiment of the present invention respectively（Ⅰ）、（Ⅱ）The row of the thermostat push rod of preparation
Journey performance curve.Abscissa is temperature in figure, and ordinate is stroke.
Embodiment
Increase the angle between sweating ware ware plate and baffle plate；Sweating ware top connects dismountable sealing device and and surge tank
Connected with compressor, and/or surge tank and vavuum pump are connected in sweating ware bottom；Increase chuck outside sweating ware, chuck with it is removable
Moving plate pipe is connected with the circulatory system, and the circulatory system has program cooling/heating function；Using the suitable paraffin of fusing point as raw material, plus
Load sweating ware after heat fusing；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature is reduced near raw material melting temperature simultaneously
Constant temperature is for a period of time；It is preferred that being uniformly paved with hybrid solid particle on wax layer surface；The high wax layer temperature of heat cycles water extraction；Wax layer temperature
Degree reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time.Start compressor in sweating effort with wax layer above shape
Into malleation, and/or start vavuum pump with wax layer negative pressure formed below, to force air flow through wax layer；On wax through it is refined, into
It is the wax product that normal hydrocarbon content is more than 80%, the content of content highest carbon number is more than 15% after type, packaging.
1-2 illustrates sweating of the present invention and prepares high normal hydrocarbon content, the production of narrow carbon number distribution wax by the following examples
The method of product.
Embodiment 1
The present embodiment includes：（1）Preparation,（2）Charging,（3）Cooling-high temperature constant temperature-cooling-cryogenic thermostat knot
Brilliant,（4）Heating-constant temperature sweating,（5）Crude product collection,（6）The process such as product purification and shaping, packaging.
（1）Preparation
By sweating ware（Angle between sweating ware ware plate and baffle plate is 120 °）The sealing system on top and surge tank and compression
Machine is connected.Surge tank is installed in sweating ware bottom and vavuum pump is connected.
Sweating ware ware plate bottom pad water.
The chuck of sweating ware is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with water
For heat-conducting medium.
Start the heating function of the circulatory system, water-cycling-media is warming up to 78 DEG C.
（2）Charging
With No. 72 semi-refined waxs（Dalian Petrochemical Industry Company produces, and its property is：72.5 DEG C of fusing point；Normal paraffin content 68.25%；
Most carbon numbers（C43）Content 8.92%；22.67 DEG C of DSC fusion ranges, latent heat 182.36J/g）For raw material, added after heating fusing
Sweating ware.Coil pipe is immersed in raw material wax layer and fixed.
（3）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, make wax layer temperature drop to 73.0 DEG C and permanent with 2.0 DEG C/h rate of temperature fall
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Wax layer temperature drop is made extremely with 1.5 DEG C/h rate of temperature fall again
62.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.
Close the refrigerating function of the circulatory system.
（4）Heating-constant temperature sweating
Discharge sweating ware pad water.
Storage tank under sweating ware outlet connection wax；Connect sweating ware sealing device for upper portion of annular；Start compressor and keep surge tank
Interior pressure stability is in 1.0~1.2 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system work(
Can, wax layer temperature is increased to 72.0 DEG C with 1.5 DEG C/h heating rate.
Stop compressor.Remove sealing device.
Open vavuum pump and keep buffering pressure inside the tank stable in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top is protected
Hold normal pressure；Wax layer temperature is set to be increased to 75.0 DEG C and constant temperature 4.0 hours with 1.5 DEG C/h heating rate so that solid-state in wax layer
Component is sufficiently separated with liquid composition.
Stop vavuum pump, terminate sweating degreasing process.
（5）Crude product is collected
Sweating ware exports changing-over crude product storage tank（Ⅰ）To receive on wax；Continue the temperature of rise recirculated water to 90 DEG C, with molten
Change and take out on wax, as crude product（Ⅰ）.
（6）Product purification and shaping, packaging
Crude product is high normal hydrocarbon content, narrow carbon number distribution wax product after clay-filtered, shaping and packaging（Ⅰ）.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅰ）Yield be 14.6%（Relative to raw material 72# semi-refined waxs）.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅰ）Property：
76.2 DEG C of fusing point；Normal paraffin content 83.56%；Most carbon numbers（C44）Content 16.27%.
By high normal hydrocarbon content, narrow carbon number distribution wax product（Ⅰ）The stroke of the thermostat product push rod of preparation-temperature is closed
System is as shown in Figure 1.It will be seen from figure 1 that thermostat push rod stroke stroke at 74 DEG C is less than stroke between 1mm, 72 DEG C~82 DEG C
More than 8mm, meet technical requirements of the nominal temperature for 72 DEG C of thermostats.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅰ）Fusing point（DSC method）：77.51℃；Latent heat of phase change：
218.52J/g；DSC fusion ranges：12.38℃.
Embodiment 2
The present embodiment includes：（1）Preparation,（2）Charging,（3）Cooling-high temperature constant temperature-cooling-cryogenic thermostat knot
Brilliant,（4）Heating-constant temperature sweating,（5）Crude product is collected and metallic particles is reclaimed,（6）Product purification and shaping, packaging were waited
Journey.
（1）Preparation
The lead particle and zinc particle of the mesh of 20 mesh~40 are screened out, by weight being 1：1 is well mixed.
By sweating ware（Angle between sweating ware ware plate and baffle plate is 150 °）The sealing system on top and surge tank and compression
Machine is connected.Surge tank is installed in sweating ware bottom and vavuum pump is connected.
Sweating ware ware plate bottom pad water；Double-deck Medium speed filter paper is spread in sweating ware bottom；
The sweating ware of chuck is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with water
For heat-conducting medium；
Start the heating function of the circulatory system, water-cycling-media is warming up to 78 DEG C.
（2）Charging
With No. 72 semi-refined waxs（Property be the same as Example 1）For raw material, the sweating ware that filter paper is completed in bottom is added after heating fusing.
Coil pipe is immersed in raw material wax layer and fixed.
（3）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, make wax layer temperature drop to 73.0 DEG C and permanent with 2.0 DEG C/h rate of temperature fall
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Wax layer temperature drop is made extremely with 1.5 DEG C/h rate of temperature fall again
62.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.
Close the refrigerating function of the circulatory system.
（4）Heating-constant temperature sweating
Foregoing lead, zinc hybrid particles are uniformly paved with wax layer surface.
Discharge sweating ware pad water.
Storage tank under sweating ware outlet connection wax；Connect sweating ware sealing device for upper portion of annular；Start compressor and keep surge tank
Interior pressure stability is in 1.0~1.2 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system work(
Can, wax layer temperature is increased to 72.0 DEG C with 1.5 DEG C/h heating rate；
Stop compressor.Remove sealing device.
Open vavuum pump and keep buffering pressure inside the tank stable in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top is kept
Normal pressure；Wax layer temperature is set to be increased to 75.0 DEG C and constant temperature 4.0 hours with 1.5 DEG C/h heating rate so that solid-state group in wax layer
Divide and be sufficiently separated with liquid composition.
Stop vavuum pump, terminate sweating degreasing process.
（5）Crude product is collected and metallic particles is reclaimed
Sweating ware exports changing-over crude product storage tank（Ⅱ）To receive on wax；Continue the temperature of rise recirculated water to 90 DEG C, with
Fusing is taken out on wax, as crude product（Ⅱ）.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
（6）Product purification and shaping, packaging
Crude product is high normal hydrocarbon content, narrow carbon number distribution wax product after clay-filtered, shaping and packaging（Ⅱ）.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅱ）Yield be 14.2%（Relative to raw material 72# semi-refined waxs）.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅱ）Property：
76.5 DEG C of fusing point；Normal paraffin content 86.35%；Most carbon numbers（C44）Content 17.23%.
By high normal hydrocarbon content, narrow carbon number distribution wax product（Ⅱ）The stroke of the thermostat product push rod of preparation-temperature is closed
System is as shown in Figure 2.Figure it is seen that thermostat push rod stroke stroke at 74 DEG C is less than stroke between 1mm, 72 DEG C~82 DEG C
More than 8mm, meet technical requirements of the nominal temperature for 72 DEG C of thermostats.
High normal hydrocarbon content, narrow carbon number distribution wax product（Ⅱ）Fusing point（DSC method）：78.23℃；Latent heat of phase change：
230.15J/g；DSC fusion ranges：10.65℃.
Sweating of the present invention can be seen that by embodiment 1-2 and high normal hydrocarbon content, narrow carbon number distribution wax product is prepared
Method, by using metallic particles is spread on wax layer surface to run through the tiny duct of wax layer above and below being formed in sweating effort, and
The methods such as wax layer are forced air flow through in sweating effort, solids fraction and the separating effect of liquid composition is enhanced, can be made
High normal hydrocarbon content of the fusing point more than 70 DEG C, narrow carbon number distribution wax are prepared with the method for this solvent-free production paraffin of sweating
Product, these can be used as thermostat Wax dielectric or phase transformation wax product.
Claims (28)
1. a kind of sweating and high normal hydrocarbon content, the method for narrow carbon number distribution wax product are prepared, including herein below：
（1）Water is padded in sweatbox；
（2）Using paraffin grade wax as raw material, load sweatbox after heating fusing；The fusing point of the paraffin grade wax is 60~74 DEG C；
（3）Wax layer is cooled to by proper temperature, high temperature constant temperature 0.01~4.0 hour with 1.0 DEG C/h~3.0 DEG C/h speed；Again
5 DEG C~20 DEG C, and cryogenic thermostat 0.01 are cooled to below final temperature, i.e. raw material fusing point with 0.5 DEG C/h~2.5 DEG C/h speed
~3.0 hours；
（4）Discharge the pad water in sweatbox；Then heated up with 0.5 DEG C/h~2.5 DEG C/h speed, wax layer reaches predetermined temperature
Constant temperature for a period of time, then stops sweating afterwards；Wax layer is wherein forced air flow through in sweating effort；
（5）Collect on wax；
（6）On wax high normal hydrocarbon content, narrow carbon number distribution wax product are obtained after refined, shaping, packaging.
2. in accordance with the method for claim 1, it is characterised in that the fusing point of the 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 middle raw material decrease temperature crystalline and in step
（4）Heat up before sweating effort, the solid particle of 10~100 mesh is uniformly paved with the surface of wax layer.
4. according to the method described in claim 3, it is characterised in that the density of described solid particle is more than 4 g/cm3。
5. in accordance with the method for claim 4, it is characterised in that described solid particle is selected from zinc, iron, copper, lead and its conjunction
One or more in gold.
6. in accordance with the method for claim 5, it is characterised in that described solid particle selects two or more different densities
Solid particle, the density contrasts of two kinds of adjacent solid particle materials of density is 1~5 g/cm3, two or more solid particles press
The close ratio mixing of parts by weight.
7. in accordance with the method for claim 3, it is characterised in that described method also includes：Sweating effort is reclaimed after terminating
Solid particle simultaneously cleans to reuse.
8. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Reduction air pressure below Fang Zengjia air pressure and/or wax layer, makes to form what pressure differential was realized above and below wax layer, described pressure differential is 0.1
~5.0 atmospheric pressure.
9. in accordance with the method for claim 1, it is characterised in that step（3）Drop of the temperature-fall period before high temperature constant temperature
Warm speed is 1.5 DEG C/h~2.5 DEG C/h, and the rate of temperature fall after high temperature constant temperature 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 step（3）Described in proper temperature for raw material fusing point-
+ 2.0 DEG C of 1.0 DEG C~fusing point.
11. in accordance with the method for claim 1, it is characterised in that step（3）Described in high temperature constant temperature time be 1.0
~4.0 hours.
12. in accordance with the method for claim 1, it is characterised in that step（3）Described cooling final temperature is raw material fusing point
8 DEG C below~15 DEG C.
13. in accordance with the method for claim 1, it is characterised in that step（3）The time of the cryogenic thermostat is 1.0~3.0
Hour.
14. in accordance with the method for claim 1, it is characterised in that step（4）In heating rate be 1.0 DEG C/h~2.0
℃/h。
15. in accordance with the method for claim 1, it is characterised in that step（4）The predetermined temperature of middle heating is less than purpose production
1 DEG C~10 DEG C of the fusing point of product.
16. in accordance with the method for claim 1, it is characterised in that step（4）Described in time of constant temperature be 0~5.0 small
When.
17. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is appointed in sweating effort
The meaning stage implements.
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 wax layer
Top increase air pressure is realized：Apply the gauge of 0.2~1.5 atmospheric pressure above wax layer, and remained below wax layer
Normal pressure.
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 wax layer
Lower section reduction pressure is realized：Normal pressure is kept above wax layer, and the gauge below wax layer is maintained -0.2~-0.8
Individual atmospheric pressure.
20. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware, sweating ware ware plate with
Angle between baffle plate is 90 °~170 °.
21. in accordance with the method for claim 3, it is characterised in that the mesh number of the solid particle is 20~50 mesh.
22. according to the method described in claim 4, it is characterised in that the density of described solid particle is 6~12 g/cm3。
23. in accordance with the method for claim 8, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
24. in accordance with the method for claim 10, it is characterised in that step（3）Described in proper temperature be raw material fusing point
+ 1.0 DEG C of~fusing point.
25. in accordance with the method for claim 16, it is characterised in that step（4）Described in constant temperature time be 0.01~5.0
Hour.
26. in accordance with the method for claim 25, it is characterised in that step（4）Described in constant temperature time be 1.0~5.0
Hour.
27. in accordance with the method for claim 17, it is characterised in that described forces air flow through wax layer in heating reality at initial stage
Apply.
28. in accordance with the method for claim 20, it is characterised in that the angle between described sweating ware ware plate and baffle plate is
120 °~150 °.
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| Application Number | Priority Date | Filing Date | Title |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410786121.3A CN105754658B (en) | 2014-12-18 | 2014-12-18 | A kind of sweating and prepare high normal hydrocarbon content, the method for narrow carbon number distribution wax product |
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| CN105754658B true CN105754658B (en) | 2017-10-27 |
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| CN109810725B (en) * | 2019-03-15 | 2021-05-25 | 上海焦耳蜡业有限公司 | Particle-based wax sweating method |
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 |
-
2014
- 2014-12-18 CN CN201410786121.3A patent/CN105754658B/en active Active
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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