CN105778999B - A kind of preparation method of high melt drop temperature microwax - Google Patents
A kind of preparation method of high melt drop temperature microwax Download PDFInfo
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- CN105778999B CN105778999B CN201410786113.9A CN201410786113A CN105778999B CN 105778999 B CN105778999 B CN 105778999B CN 201410786113 A CN201410786113 A CN 201410786113A CN 105778999 B CN105778999 B CN 105778999B
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Abstract
The invention discloses a kind of preparation method of high melt drop temperature microwax.This method uses sweatbox, the proper temperature increase high temperature constant temperature stage during cooling, the solid particle of mixing is uniformly paved with wax layer surface after cooling procedure terminates, and wax layer is forced air flow through in the sweating effort that heats up, is carried out in liquid composition.The present invention is on the basis of common sweating method, increase the high temperature constant temperature process for the process that cools and the pressure separation process of heating sweating effort, accelerate liquid composition and the separating rate of solids fraction, and separating effect is enhanced, this solvent-free de-oiling method of sweating de-oiling is produced the crystallite wax product of high melt drop temperature.The inventive method has the advantages that plant investment is low, production process is simple and operating cost is low, solvent-free pollution.
Description
Technical field
The invention belongs to pertroleum wax production technical field, more particularly to a kind of preparation method of high melt drop temperature microwax.
Background technology
The general name of the pertroleum wax obtained all kinds of wax products that are crude oil after refining is processed from wax-containing distillate, including liquid
Body paraffin, paraffin and microwax.The melt drop temperature of the crystallite wax product of specification is 67 DEG C~90 DEG C in national standard, typically by C30~
C60Cycloalkane, a small amount of positive structure and isoparaffin composition, there is the needle-like crystal structure more tiny than paraffin under solid-state.
Microwax is that decompression residuum is given birth to through steps such as dewaxing, de-oiling, refined and shapings again after propane equal solvent depitching
Production.
Dewaxing is that the process for the slack wax that oil content is 10~30% or so, dewaxing technique are prepared by raw material of lube cut
Mainly there are squeezing dewaxing and solvent dewaxing.De-oiling is that the process of waxy stone of the oil content below 2%, de-oiling are prepared using slack wax as raw material
Technique mainly has sweating de-oiling and solvent deoiling.Waxy stone through clay-filtered or hydrofinishing and shaping, packaging and other steps, both may be used again
Obtain petroleum paraffin product.
Solvent deoiling process is in selective solvent（Acetone, benzene and toluene mixture；Or acetone, toluene；Or MEK,
Toluene）Solution in freeze, the method separated according to the difference of wax and oil solubility produces petroleum paraffin product.Solvent takes off
Oily technique have the advantages that production is continuous, wax high income, finished product wax oil content can it is very low, production cost is relatively low, be big at present
The main flow de-oiling technique of large-scale production petroleum paraffin product.But solvent dewaxing investment of production equipment is big；Needed in production process a large amount of
Using solvent, recycling design needs to consume substantial amounts of energy；Contain benzene homologues in solvent, environment can be impacted；Solvent is easy
Combustion, easily causes production accident.
Sweating de-oiling method is separated using the wax property different with oily fusing point.Point of various components in pertroleum wax
Son amount Bu Tong can all make its fusing point different with structure.When being all n-alkane structure, the larger n-alkane of molecular weight melts
Point is higher, and the fusing point of the less n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will
Less than n-alkane, and isomery degree more high-melting-point is lower, or even is just at normal temperatures liquid condition, i.e., usually said
Oil.Sweating de-oiling method only needed in process of production without using solvent, and in production process by raw material be heated to fusing point with
On temperature.
Common sweating degreasing process mainly includes the following steps that：（1）Preparation：Water is padded, is full of sweatbox with water
Ware plate lower space；（2）Charging：Load sweatbox when raw material is heated to more than fusing point being in a liquid state；（3）Decrease temperature crystalline：By original
Material progressively cools to below its fusing point 10~20 DEG C with the rate of temperature fall no more than 4 DEG C/h.In cooling procedure, fusing point highest
Component first is come out with thick fibrous crystal morphological crystal, as wax layer temperature continues to reduce, other components by fusing point by height to
Low order crystallizes to form solid successively；（4）Heat up sweating：After wax layer temperature reaches default cooling final temperature, put
Fall to pad water；Raw material is slowly heated to default sweating final temperature again.In the sweating effort that heats up, various components press fusing point
Order from low to high is successively fused into liquid and flowed out（Under wax）, the wax layer residue that finally obtains（On wax）It is exactly Gao Rong
The wax of point, low oil-containing；（5）Crude product is collected：Heating sweating effort terminates follow-up high-temperature of continuing rising, is taken out with fusing on wax, i.e.,
For crude product；（6）Product purification, shaping, packaging：Subtractive process generally use is clay-filtered：It is warming up to after crude product is melted
Predetermined temperature, add carclazyte and simultaneously filtered after constant temperature was stirred to the scheduled time；It is again purpose product through being molded, packing.
Common sweating de-oiling technique can produce the soap wax and low melt point paraffin under solid-state with thick flaky crystal structure,
Can not produce has the crystallite wax product of tiny needle-like crystal structure under solid-state.There is experiment to show, common sweating de-oiling technique life
When producing crystallite wax product, even if using the method for extending sweating sessions and improving sweating final temperature, containing on sweating later stage wax
Oil mass is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, so so far there are no with sweating de-oiling technique
Produce the report of microwax and high melt drop temperature crystallite wax product.Only part producer uses sweating de-oiling technique productions soap wax at present
With low melt point paraffin product.
For many years, sweating de-oiling technique has obtained some development, such as CN89214332 in production equipment and process aspect（It is vertical
Formula 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（A kind of Efficient paraffin sweatbox）、
CN201320127680.4（Tubular type paraffin deoiler）Deng being improved in sweating de-oiling production equipment；CN91206202
（A kind of high-efficient sweat pot for paraffin wax）Improved in sweating de-oiling technique.But these methods, which can not still produce, meets relevant criterion
Crystallite wax product, high melt drop temperature crystallite wax product can not be produced.
The primes crystallite wax product that the highest trade mark of the crystallite wax product of specification is No. 90 in national standard at present（Drip melt
87~92 DEG C of point）, at present also only have a manufacturer production 90 primes crystallite wax product.To the microwax of higher melt drop temperature
Product, have no the report of associated production technology and product.
Compared with solvent deoiling technique, sweating de-oiling technique has that plant investment is few, production process is simple and operating cost
Low advantage, it is often more important that, sweating de-oiling technique is to be currently known unique nothing for commercial scale petroleum paraffin product
Solvent deoiling method, in promotion green low-carbon, today of environmental protection and energy saving, using the need of sweating de-oiling technique productions crystallite wax product
Ask more urgent.Meanwhile develop more than No. 90（More than 92 DEG C of melt drop temperature）High melt drop temperature crystallite wax product to meet related society
Meeting demand, and very urgent task.
The content of the invention
For prior art and the deficiency of product, the present invention provides a kind of production method of high melt drop temperature microwax, specifically
It is to use sweatbox that ground, which is said, and on the basis of common sweating method, the proper temperature increase during cooling is high
The warm constant temperature stage, and increase the cryogenic thermostat stage after cooling procedure terminates and the constant temperature stage of heating sweating effort；Cold
But the metallic particles of mixing is uniformly paved with after process terminates on wax layer surface, and wax is forced air flow through in the sweating effort that heats up
Layer, carries out liquid composition, accelerates separating rate and enhance separating effect, make this solvent-free de-oiling method of sweating de-oiling
The crystallite wax product of high melt drop temperature can be produced.
A kind of preparation method of high melt drop temperature microwax of the present invention, including herein below：
（1）Water is padded in sweatbox；
（2）Using commodity microwax 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 cools to preset temperature, i.e., 10 DEG C~20 DEG C below raw material fusing point, and cryogenic thermostat
For a period of 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 temperature-rise period；
（5）Collect on wax；
（6）After refined, shaping it is high melt drop temperature crystallite wax product on wax.
In the preparation method of the high melt drop temperature microwax of the present invention, wherein the melt drop temperature of described commodity microwax is 87 DEG C
~92 DEG C.Described high melt drop temperature microwax refers to microwax of the melt drop temperature more than 92 DEG C.
In the high melt drop temperature microwax preparation method of the present invention, preferably in step（3）After middle raw material decrease temperature crystalline（Refer to low
Warm constant temperature terminates）And in step（4）Before heating sweating effort（Now wax layer is in solid state）, it is uniform on the surface of wax layer
It is paved with the solid particle of 10~100 mesh, preferably 20~50 mesh.The density of solid particle is generally higher than 4 g/cm3, can be with right and wrong gold
Material, the preferred densities such as category, metal and alloy are 6~12 g/cm3Metal and alloying pellet, such as zinc, iron, copper, lead and its conjunction
The more stable low price metal material of the chemical property such as gold.The solid of two or more different densities can be selected
Grain, two or more solid particles can ratio mixing similar in parts by weight.Two kinds of adjacent solid particle materials of density it is close
It is 1~5 g/cm to spend difference3.Density described herein refers to the density for forming the material of solid particle, rather than the heap of solid particle
Density.Sweating effort can reclaim solid particle and clean to reuse after terminating.
In the high melt drop temperature microwax preparation method of the present invention, described sweatbox is generally sweating ware, and in wax layer
Dismountable sealing system and pressue device added above and/or increase vacuum plant below wax layer.Described pressure air-flow
Increase pressure above wax layer is utilized in by wax layer（Air pressure）And/or pressure is reduced below wax layer（Air pressure）, make wax layer
Form what pressure differential was realized up and down.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 air
Pressure, to force air flow through wax layer.
In the high melt drop temperature microwax preparation method of the present invention, step（3）In described temperature-fall period, in high-temperature constant temperature section
The preferably 1.5 DEG C/h~2.5 DEG C/h of rate of temperature fall before.
In the high melt drop temperature microwax preparation method of the present invention, step（3）The high-temperature constant temperature section of described temperature-fall period
Proper temperature is+2.0 DEG C of -1.0 DEG C~melt drop temperature of raw material microwax melt drop temperature, preferably raw material microwax melt drop temperature~melt drop temperature
+1.0℃；The time of the high-temperature constant temperature section for the process that cools is generally 0~4.0 hour, preferably 1.0~4.0 hours.
In the high melt drop temperature microwax preparation method of the present invention, the drop in described temperature-fall period after high-temperature constant temperature section
Warm speed preferably 1.0 DEG C/h~2.0 DEG C/h.
In the high melt drop temperature microwax preparation method of the present invention, melted wherein the final temperature to cool is preferably raw material microwax
Point is following 12 DEG C~15 DEG C.
In the high melt drop temperature microwax preparation method of the present invention, described cools to preset temperature, increases low temperature
The constant temperature stage, the time in the cryogenic thermostat stage for the process that cools was 0~3.0 hour, preferably so that solid crystal is more abundant
For 1.0~3.0 hours.
In the high melt drop temperature microwax preparation method of the present invention, the heating rate preferably 1.0 of described heating sweating effort
DEG C/h~2.0 DEG C/h.The predetermined temperature of temperature-rise period is less than 2 DEG C~10 DEG C of purpose product melt drop temperature.
In the high melt drop temperature microwax preparation method of the present invention, described heating sweating to the preset temperature for producing product
Afterwards, preferably the constant temperature stage is increased so that wax and oil separation are more abundant.The time in constant temperature stage be 0~5.0 hour, preferably 1.0
~5.0 hours.
In the high melt drop temperature microwax preparation method of the present invention, the heating rate and rate of temperature fall of said wax layer, Ke Yitong
Cross air bath, water-bath, oil bath or other feasible modes to be controlled, it is preferred to use oil bath is controlled.Using oil bath etc.
When mode controls heating rate and rate of temperature fall, chuck, chuck and removable coil pipe and the circulatory system can be increased outside sweating ware
It is connected, the circulatory system has program cooling/heating function, and the circulatory system adds the materials such as oil as circulatory mediator；Will after charging
Coil pipe is immersed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the high melt drop temperature microwax preparation method of the present invention, the described wax layer that forces air flow through can be in heating sweating
Process any stage is implemented, and preferably implements initial stage in heating sweating.
In the high melt drop temperature microwax preparation method of the present invention, the described wax layer that forces air flow through is by wax layer
Portion increases pressure（Air pressure）Realize, apply 0.2~1.5 atmospheric pressure such as above wax layer（Gauge pressure）Pressure, and under wax layer
Side remains normal pressure.
In the high melt drop temperature microwax preparation method of the present invention, the described wax layer that forces air flow through is by under wax layer
Side reduces pressure（Air pressure）Realize, as remained normal pressure above wax layer, and the pressure below wax layer be maintained -0.2~-
0.8 atmospheric pressure（Gauge pressure）.
Sweating de-oiling method is to carry out separation production petroleum paraffin product using the wax property different with oily fusing point, but right
In crystallite wax product, because its main component is cycloalkane and isoparaffin, chemical composition is complicated, causes crystals upon crystallization structure
More tiny densification, to liquid composition（The wax of oil and low melting point）Discharge form huge filter flow resistance power, this results in only leaning on
Solids fraction is difficult to be kept completely separate with liquid composition in the common sweating effort of gravity natural separation.Therefore common sweating de-oiling work
Skill can not produce the crystallite wax product for meeting relevant criterion, can not produce the crystallite wax product of high melt drop temperature.
The present invention is in order that the method for this solvent-free production pertroleum wax of sweating de-oiling can prepare high melt drop temperature microwax
Product, by the further investigation to common sweating effort, it is difficult to liquid composition separate reason for solids fraction, by rising
Used in warm sweating effort and force air flow through the method that wax layer carries out liquid composition, while further preferably in the process of cooling
The middle increase high temperature constant temperature stage, and after the process of cooling terminates（I.e. before heating sweating effort）Uniformly it is paved with wax layer surface
The method of solid particle is improved；Increase cryogenic thermostat stage and the heating sweating to preset temperature for the process that cools simultaneously
The processes such as constant temperature stage afterwards.
Research for microwax sweating effort shows, in sweating effort, liquid composition is gradually arranged along crystalline portion
Go out, the situation that similar oil flows in capillary.Due to the tiny fine and close crystalline texture of microwax, can make to liquid composition shape
Into filter flow resistance power increased dramatically, cause common sweating method to produce microwax and high melt drop temperature crystallite wax product.
Increasing the high temperature constant temperature stage during cooling can make the crystallization of microwax bigger, beneficial to heating sweating
The discharge of liquid composition in journey.Research for microwax crystallization process shows that the chemical composition of microwax is to determine crystalline
The main reason of state, while the condition of cooling procedure can also influence crystal habit, especially at the temperature near fusing point
Influence of the cooling condition to crystal habit is most obvious.Microwax existing partially crystallizable when being cooled near fusing point separates out, this portion
Crystalline solid is divided now to increase the high temperature constant temperature stage as the nucleus for being subsequently formed crystallization, nucleus can be enable fully to increase
It is long, larger sized crystal is formed, although this larger sized crystal is thick not as the crystallization of low melt point paraffin, this
Discharge of the crystal structure of kind increase to sweating stage oil is also highly beneficial.
After the process of cooling terminates solid is uniformly paved with wax layer surface（It is preferred that metal）Particle, while sent out in heating
The discharge that wax layer is also beneficial to liquid composition in heating sweating effort is forced air flow through during sweat.In the process knot that cools
Shu Hou（I.e. before heating sweating effort）, now wax layer be in solid state, be uniformly paved with solid particle on wax layer surface.Heating up
In sweating effort, as wax layer temperature raises, wax layer softens, and because the density of solid particle is larger, it under gravity will
With slower velocity sedimentation, so as to form the thin channel run through up and down in wax layer, and filter flow resistance power is reduced, and be advantageous to
The quick discharge of liquid composition.Different densities are different with the sinking speed of the solid particle of particle diameter, using the solid particle of mixing
It can ensure that the different height in wax layer in the overall process of sweating de-oiling has the passage of more discharge liquid composition.Simultaneously
Wax layer is forced air flow through, carries out liquid composition, so as to enhance separating effect.It is aided with the cryogenic thermostat rank of cooling procedure again
Section makes solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction and liquid composition separate more abundant etc. side
Method, sweating de-oiling technique is set to produce crystallite wax product, it might even be possible to produce the crystallite wax product of high melt drop temperature.
It is an advantage of the invention that：The method for carrying out liquid composition by using wax layer is forced air flow through, accelerate solid
The separating rate of state component and liquid composition, and enhance separating effect.And make hybrid solid particle in the sweating effort that heats up
In wax layer surface settlement, the upper and lower thin channel through wax layer of formation, the quick discharge of liquid composition is also beneficial to.So that
Sweating de-oiling technique is obtained to can be used in producing high melt drop temperature crystallite wax product.The square law device of the present invention invests low, production process
Simple and operating cost is low, solvent-free pollution environment.
Embodiment
Sweating ware top connects dismountable sealing device and is connected with surge tank and compressor, and/or under sweating ware
Portion connects surge tank and vavuum pump；Increase chuck outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function；Using microwax as raw material, load sweating ware after heating fusing, by coil pipe submergence in the feed
It is and fixed；Low-temperature oil is passed through in chuck and coil pipe to reduce near wax layer temperature to raw material melt drop temperature temperature and during one section of constant temperature
Between；Hybrid solid particle is uniformly paved with wax layer surface；Heat cycles oil improves wax layer temperature；Connection sealing device simultaneously starts pressure
Contracting machine is with wax layer malleation formed above, and/or starts vavuum pump with wax layer negative pressure formed below, to force air flow through
Wax layer；Wax layer temperature reaches preset temperature and constant temperature stops sweating degreasing process afterwards for a period of time.Through essence under the wax of on wax or part
It is high melt drop temperature crystallite wax product after system, shaping, packaging.
1-2 illustrates the preparation method of the high melt drop temperature microwax of the present invention by the following examples.
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 processes such as product purification.
（1）Preparation
The sealing system on sweating ware top is connected with surge tank and compressor.In sweating ware bottom installation surge tank simultaneously
Connect vavuum pump.
Pad water in sweating ware ware plate bottom.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, to lead
Deep fat is medium；Start circulation system function, circulation oil medium is warming up to 97 DEG C.
（2）Charging
With No. 90 microwaxes（Nanyang wax Fine Chemical Works produce, 90.35 DEG C of fusing point；90.77 DEG C of melt drop temperature；Oil content
1.76%）For raw material, sweating ware 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, wax layer temperature is dropped to 91.0 DEG C and perseverance with 2.0 DEG C/h rate of temperature fall
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystal fully increases；Drop to wax layer temperature again with 1.5 DEG C/h rate of temperature fall
78.0 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.
Under one wax of sweating ware outlet connection（Part I sweating effluent, similarly hereinafter）Storage tank；Connect sweating ware top seal
Device；Start compressor and keep buffering pressure inside the tank stabilization in 1.0~1.2 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section
Keep normal pressure；Start circulation system function, wax layer temperature is increased to 92.0 DEG C and constant temperature with 1.5 DEG C/h heating rate
2.0 hours so that the solids fraction in wax layer is sufficiently separated with liquid composition；Stop compressor.Remove sealing device.
Storage tank under the sweating ware outlet wax of changing-over two；Open vavuum pump and keep buffering pressure inside the tank stabilization -0.4~-0.6
Individual atmospheric pressure（Gauge pressure）, wax layer top keeps normal pressure；Wax layer temperature is set to be increased to 94.0 DEG C and perseverance with 1.5 DEG C/h heating rate
Warm 4.0 hours so that the solids fraction in wax layer 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 to receive on wax；Continue the temperature of rise recycle oil to 110 DEG C, with fusing
Take out on wax, as crude product.
（6）Product purification
Crude product is high melt drop temperature crystallite wax product after clay-filtered, shaping and packaging（Ⅰ）.
Under two waxes through it is clay-filtered, shaping and packaging after be high melt drop temperature crystallite wax product（Ⅱ）.
High melt drop temperature microwax product property：
High melt drop temperature crystallite wax product（Ⅰ）：Melt drop temperature：96.8 DEG C, oil content：0.93%.
Crystallite wax product（Ⅰ）Yield be 14.8%（Relative to raw material microwax）.
Crystallite wax product（Ⅱ）：Melt drop temperature：93.0 DEG C, oil content：2.35%.
Crystallite wax product（Ⅱ）Yield be 8.45%（Relative to raw material microwax）.
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 mixed metal particles reclaim,（6）The processes such as product purification.
（1）Preparation
Lead particle, copper particle and the zinc particle of the mesh of 20 mesh~40 are screened out, by weight being 1：1：1 is well mixed.
The sealing system on sweating ware top is connected with surge tank and compressor.In sweating ware bottom installation surge tank simultaneously
Connect vavuum pump.
Pad water in sweating ware ware plate bottom；Double-deck Medium speed filter paper is spread in sweating ware bottom.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, to lead
Deep fat is medium；Start circulation system function, circulation oil medium is warming up to 97 DEG C.
（2）Charging
With No. 90 microwaxes（Property is the same as embodiment 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, wax layer temperature is dropped to 91.0 DEG C and perseverance with 2.0 DEG C/h rate of temperature fall
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystal fully increases；Drop to wax layer temperature again with 1.5 DEG C/h rate of temperature fall
78.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.
The hybrid particles of foregoing lead, copper and zinc are paved with wax layer surface.
Close the refrigerating function of the circulatory system.
（4）Heating-constant temperature sweating
Discharge sweating ware pad water.
Storage tank under one wax of sweating ware outlet connection；Connect sweating ware sealing device for upper portion of annular；Start compressor and keep buffering
Pressure inside the tank is stable in 1.0~1.2 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system
Function, wax layer temperature is set to be increased to 92.0 DEG C and constant temperature 2.0 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 compressor.Remove sealing device.
Storage tank under the sweating ware outlet wax of changing-over two；Open vavuum pump and keep buffering pressure inside the tank stabilization -0.4~-0.6
Individual atmospheric pressure（Gauge pressure）, wax layer top keeps normal pressure；Wax layer temperature is set to be increased to 94.0 DEG C and perseverance with 1.5 DEG C/h heating rate
Warm 4.0 hours so that the solids fraction in wax layer is sufficiently separated with liquid composition.
Stop vavuum pump, terminate sweating degreasing process.
（5）Crude product is collected and mixed metal particles recovery
Sweating ware exports changing-over crude product storage tank to receive on wax；Continue the temperature of rise recycle oil to 110 DEG C, with fusing
Take out on wax, as crude product.
The mixed metal particles on filter paper are collected, cleaning, are dried in case reusing.
（6）Product purification
Crude product is high melt drop temperature crystallite wax product after clay-filtered, shaping and packaging（Ⅲ）.
Under two waxes through it is clay-filtered, shaping and packaging after be high melt drop temperature crystallite wax product（Ⅳ）.
High melt drop temperature microwax product property：
High melt drop temperature crystallite wax product（Ⅲ）：
Melt drop temperature：97.6 DEG C, oil content：0.58%.
Crystallite wax product（Ⅲ）Yield be 14.6%（Relative to raw material microwax）.
Crystallite wax product（Ⅳ）：
Melt drop temperature：93.3 DEG C, oil content：1.59%.
Crystallite wax product（Ⅳ）Yield be 9.52%（Relative to raw material microwax）.
The production method of the high melt drop temperature microwax of the present invention is can be seen that by embodiment 1-2, using sweatbox,
During cooling using high temperature constant temperature and the constant temperature of cryogenic thermostat and sweating degreasing process, after cooling procedure terminates in wax
The methods of layer surface is uniformly paved with the metallic particles of mixing, forces air flow through wax layer in the sweating effort that heats up, accelerate solid
The separating rate of state component and liquid composition, and solids fraction and the separating effect of liquid composition are enhanced, sweating can be used
The method of this solvent-free production pertroleum wax of de-oiling prepares high melt drop temperature crystallite wax product.
Claims (21)
1. a kind of preparation method of high melt drop temperature microwax, including herein below：
（1）Water is padded in sweatbox；
（2）Using the commodity microwax that melt drop temperature is 87 DEG C~92 DEG C as raw material, load sweatbox after heating fusing；
（3）Wax layer is cooled to by proper temperature, high temperature constant temperature 1.0~4.0 hours with 1.0 DEG C/h~3.0 DEG C/h speed；Again with
0.5 DEG C/h~2.5 DEG C/h speed cools to preset temperature, i.e., 10 DEG C~20 DEG C below raw material fusing point, and cryogenic thermostat
1.0~3.0 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 temperature-rise period；
（5）Collect on wax；
（6）After refined, shaping it is high melt drop temperature crystallite wax product on wax；
Wherein, described high melt drop temperature microwax refers to microwax of the melt drop temperature more than 92 DEG C.
2. 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
Fang Zengjia air pressure and/or air pressure is reduced below wax layer, wax layer is formed what pressure differential was realized up and down；Described pressure differential is
0.1~5.0 atmospheric pressure.
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. in accordance with the method for claim 3, it is characterised in that the density of the solid particle is more than 4 g/cm3。
5. in accordance with the method for claim 4, it is characterised in that described solid particle is zinc, iron, copper, lead and its alloy
In one or more.
6. in accordance with the method for claim 5, it is characterised in that select the solid particle of two or more different densities.
7. in accordance with the method for claim 6, it is characterised in that the solid particle of described two or more different densities
In, the density contrast of two kinds of adjacent solid particle materials of density is 1~5 g/cm3。
8. in accordance with the method for claim 1, it is characterised in that step（3）In rate of temperature fall before high-temperature constant temperature section
For 1.5 DEG C/h~2.5 DEG C/h.
9. in accordance with the method for claim 1, it is characterised in that described proper temperature is -1.0 DEG C of raw material melt drop temperature~drop
+ 2.0 DEG C of fusing point.
10. in accordance with the method for claim 1, it is characterised in that step（3）In rate of temperature fall after high-temperature constant temperature section
For 1.0 DEG C/h~2.0 DEG C/h.
11. in accordance with the method for claim 1, it is characterised in that step（3）The final temperature of middle cooling is raw material microwax
12 DEG C~15 DEG C below melt drop temperature.
12. 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。
13. in accordance with the method for claim 1, it is characterised in that step（4）In predetermined temperature be less than purpose product drip
2 DEG C~10 DEG C of fusing point.
14. in accordance with the method for claim 1, it is characterised in that step（4）The time of middle constant temperature is 0~5.0 hour.
15. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Top increase air pressure is realized：Apply the gauge of 0.2~1.5 atmospheric pressure above wax layer, and kept below wax layer normal
Pressure.
16. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Lower section reduces what air pressure was realized：Normal pressure is kept above wax layer, and the gauge below wax layer is maintained -0.2~-0.8
Individual atmospheric pressure.
17. in accordance with the method for claim 2, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
18. in accordance with the method for claim 3, it is characterised in that the mesh number of the solid particle is 20~50 mesh.
19. in accordance with the method for claim 4, it is characterised in that the density of the solid particle is 6~12 g/cm3。
20. in accordance with the method for claim 9, it is characterised in that described proper temperature be raw material melt drop temperature~melt drop temperature+
1.0℃。
21. in accordance with the method for claim 14, it is characterised in that step（4）The time of middle constant temperature is 1.0~5.0 hours.
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| CN201410786113.9A CN105778999B (en) | 2014-12-18 | 2014-12-18 | A kind of preparation method of high melt drop temperature microwax |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410786113.9A CN105778999B (en) | 2014-12-18 | 2014-12-18 | A kind of preparation method of high melt drop temperature microwax |
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| CN105778999B true CN105778999B (en) | 2017-11-24 |
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|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1189527A (en) * | 1997-01-27 | 1998-08-05 | 王福祥 | Quick sweating wax making tech. |
| CN102533333A (en) * | 2012-01-16 | 2012-07-04 | 无锡信达胶脂材料有限公司 | Preparation method of paraffin for pharmaceutic adjuvants |
| CN103102971A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation method for wax temperature-sensitive medium for temperature control valve |
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|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1189527A (en) * | 1997-01-27 | 1998-08-05 | 王福祥 | Quick sweating wax making tech. |
| CN103102971A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation method for wax temperature-sensitive medium for temperature control valve |
| CN102533333A (en) * | 2012-01-16 | 2012-07-04 | 无锡信达胶脂材料有限公司 | Preparation method of paraffin for pharmaceutic adjuvants |
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| CN105778999A (en) | 2016-07-20 |
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