CN106883888B - A kind of method of sweating and the high dropping point microwax of production - Google Patents
A kind of method of sweating and the high dropping point microwax of production Download PDFInfo
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- CN106883888B CN106883888B CN201510928625.9A CN201510928625A CN106883888B CN 106883888 B CN106883888 B CN 106883888B CN 201510928625 A CN201510928625 A CN 201510928625A CN 106883888 B CN106883888 B CN 106883888B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/42—Refining of petroleum waxes
Abstract
The invention discloses a kind of sweating and the methods of the high dropping point microwax of production.This method is on the basis of common sweating process, proper temperature in temperature-fall period increases the high temperature constant temperature stage, liquid composition is carried out by wax layer using air-flow in sweating effort, and it places solid mass in wax layer and pressure is applied to wax layer, it enhances the separating effect of solids fraction and liquid composition and accelerates separating rate so that this no-solvent process of sweating de-oiling can produce high dropping point crystallite wax product.The method of the present invention has many advantages, such as that investment of production equipment is low, production process is simple and operating cost is low, safe, energy saving and solvent-free pollution.
Description
Technical field
The invention belongs to pertroleum wax production technical fields, more particularly to a kind of sweating and produce high dropping point microwax
Method.
Background technology
The general name of the pertroleum wax all kinds of wax products obtained that are crude oil after refining is processed from wax-containing distillate, including liquid
Body paraffin, soap manufacturing paraffin, paraffin and microwax.In national standard the dropping point of the crystallite wax product of specification be 67 DEG C~92 DEG C, one
As by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition, there is under solid-state the needle-shaped knot more tiny than paraffin
Crystal structure.
Microwax be decompression residuum after propane equal solvent depitching again through dewaxing, de-oiling, refined and molding and etc. it is raw
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 2% waxy stone below of oil content, de-oiling are prepared using slack wax as raw material
Technique mainly has sweating de-oiling and solvent deoiling.Waxy stone is again through clay-filtered or hydrofinishing and molding, packaging and other steps, you can
Obtain crystallite wax product.
Solvent deoiling method is with oil according to wax in selective solvent（Acetone, benzene and toluene mixture；Or acetone, toluene；
Or methyl ethyl ketone, toluene）What the property of middle different solubility was detached.Solvent deoiling technique with production process, receive by continuous, wax
The advantages that rate is high, finished product wax oil content can be very low, production cost is relatively low is the mainstream of current large-scale production petroleum paraffin product
De-oiling technique.But solvent deoiling technique productions equipment investment is big；It needs largely to use solvent in production process, recycling design needs
Consume a large amount of energy；Contain benzene homologues in solvent, environment can be impacted；Solvent is inflammable, be easy to cause production accident.
Sweating de-oiling method is detached using wax and oil property with different melting point.Point of various hydro carbons 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 smaller n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane is wanted
Less than n-alkane, and isomery degree more high-melting-point is lower, or even is in just liquid condition at normal temperatures, i.e., usually said
Oil.
Common sweating de-oiling technique mainly includes the following steps that：（1）Preparation：Water is padded, is full of sweatbox with water
Ware plate lower space；Charging, raw material are heated to being packed into sweatbox when fusing point or more is in a liquid state；（2）Crystallization：By raw material with little
10~20 DEG C of its fusing point or less is progressively cooled in the rate of temperature fall of 4 DEG C/h.In cooling procedure, various components press fusing point by height
It is crystallized successively to low sequence and forms solid；（3）Sweating：After wax layer temperature reaches preset cooling final temperature, bleed off
Pad water；Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components by fusing point by as low as
High sequence is successively fused into liquid and flows out（Under wax）, the wax layer residue that finally obtains（On wax）It is exactly high-melting-point, low contains
The wax of oil；Continue to increase temperature after sweating effort, be taken out on wax with fusing, as crude product；（4）It is refined：Crude product is molten
It is warming up to predetermined temperature after change, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the predetermined time, then through being produced for the purpose of being molded, pack i.e.
Product.
Common sweating de-oiling technique can produce fusing point has coarse flaky crystal structure under 40 DEG C~60 DEG C of solid-state
Soap manufacturing paraffin and low melt point paraffin, cannot produce under solid-state with tiny needle-like crystal structure crystallite wax product.There is experiment table
It is bright, when common sweating de-oiling technique productions crystallite wax product, even if using extending sweating sessions and improving sweating final temperature
Method, the oil content on sweating later stage wax is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, institute so that
The present has no with the report of sweating de-oiling technique productions microwax and high dropping point crystallite wax product.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is relatively low, the production cycle is longer, but
Be sweating de-oiling technique have small investment, production process is simple, operating cost is low, production process is safe, it is energy saving and to environment without
The advantages that pollution, still has part of the manufacturer producing soap manufacturing paraffin product using this method at present.
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）, also only there are one the primes crystallite wax products that producer produces No. 90 at present.To the microwax of higher dropping point
Product has no the report of associated production technology and product.
For many years, sweating method 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 de-oiling production equipment；CN91206202
（A kind of high-efficient sweat pot for paraffin wax）It is improved in sweating de-oiling technique, but these improvement cannot still produce and meet relevant criterion
Crystallite wax product, high dropping point crystallite wax product can not be produced.
Sweating process is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product, is being carried
Advocate green low-carbon, environmental protection and energy saving today, the demand using sweating de-oiling technique productions crystallite wax product is more urgent.Meanwhile
Exploitation 90 or more（92 DEG C of dropping point or more）High dropping point crystallite wax product to meet related social demand, and it is very urgent
Task.
Invention content
In view of the deficiencies of the prior art, a kind of method that the present invention provides sweating and the high dropping point microwax of production, specifically
It is to use sweatbox that ground, which is said, and on the basis of common sweating de-oiling technique, the proper temperature in temperature-fall period increases high temperature
Constant temperature stage and cryogenic thermostat stage and the constant temperature stage of sweating effort；It is carried by wax layer using air-flow in sweating effort
Go out liquid composition（Wax oily and compared with low melting point）To force to detach solids fraction（The wax of higher melt）With liquid composition, enhance
Separating effect simultaneously accelerates separating rate.Solid mass is placed in wax layer pressure is applied to accelerate to wax layer in sweating effort
The separating rate of solids fraction and liquid composition simultaneously ensures airflow through wax layer, and this solvent-free separation method of sweating is allow to give birth to
The crystallite wax product of the high dropping point of output.The method of the present invention is low with investment of production equipment, production process is simple and operating cost
The advantages that low, safe, energy saving and solvent-free pollution.
A kind of sweating of the present invention and the method for the high dropping point microwax of production, including the following contents：
（1）Charging：The commodity microwax for being 87 DEG C~92 DEG C using dropping point is packed into sweating dress as raw material after heating fusing
It sets；
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization：Wax layer is cooled down with the rate of 1.0 DEG C/h~3.0 DEG C/h
To proper temperature, high temperature constant temperature is for a period of time；Again with the rate of 0.5 DEG C/h~2.5 DEG C/h be cooled to 5 DEG C of raw material fusing point or less~
20 DEG C of cooling final temperature, and cryogenic thermostat is for a period of time；
（3）Heating-constant temperature sweating：It is heated up with the rate of 0.5 DEG C/h~2.5 DEG C/h；Wax layer reaches predetermined temperature and constant temperature
Stop sweating after a period of time；Wax layer is forced air flow through in sweating effort；
（4）It is refined：After refined, molding, packaging it is high dropping point crystallite wax product on wax.
In the method for the present invention, the dropping point of the commodity microwax is 87 DEG C~92 DEG C.The high dropping point is micro-
Brilliant wax refers to microwax of the dropping point at 92 DEG C or more.
In the method for the present invention, in step（3）In sweating effort, preferably by placing solid mass on wax layer surface with right
Wax layer applies the pressure of 0.5kPa or more（Pressure）.Solid mass surfacing, overall dimensions are slightly less than sweatbox inner wall ruler
It is very little, internal to have perforative gap up and down.Solid mass edge and the gap of sweatbox inner wall are generally 0.01~50mm, preferably
0.1~20mm.The density of solid mass generally requires to be more than 4g/cm3, can be the materials such as nonmetallic, metal and alloy, preferably
Density is 6~12 g/cm3Metal and alloy, such as zinc, iron, copper, lead and its alloy chemical property it is more stable low price gold
Belong to material.
In the present invention, one of following manner may be used and place solid mass on wax layer surface to apply pressure to wax layer
（Pressure）：（1）The solid mass of 0.5kPa or more pressure can be generated by being added at one time in sweating effort, preferably be started in sweating
When be added at one time the solid mass that can generate 1.4~20.0kPa pressure.（2）In sweating effort several times（It is preferred that 2~3
It is secondary）Be added, i.e., the solid mass of 0.5kPa or more pressure can be generated by being added in every 0.1~20.0 h, preferably every 0.1~
The solid mass of 1.4~10.0kPa pressure can be generated by being added in 10.0 h.
The present invention method in, the sweatbox is sweating ware, and wax layer pressue device added above and/or
Increase vacuum plant below wax layer.In step（3）In sweating effort, the wax layer that forces air flow through uses above wax layer
Increase air pressure and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize.The pressure difference is general
For 10~500 kPa, preferably 20~200kPa, to force air flow through wax layer.
In the method for the present invention, the step（2）In the temperature-fall period of crystallization, the rate of temperature fall before high-temperature constant temperature section
It is preferred that 1.5 DEG C/h~2.5 DEG C/h.The proper temperature of the high-temperature constant temperature section of the temperature-fall period is raw material microwax dropping point-
+ 2.0 DEG C of 1.0 DEG C~dropping point, preferably raw material microwax dropping point~+1.0 DEG C of dropping point.The high-temperature constant temperature section of temperature-fall period
Time be 0~4.0 hour, preferably 0.1~4.0 hour, more preferably 1.0~4.0 hours.
In the method for the present invention, the step（2）Rate of temperature fall of the temperature-fall period of crystallization after high-temperature constant temperature section is excellent
Select 1.0 DEG C/h~2.0 DEG C/h.The cooling final temperature is preferably 8 DEG C~15 DEG C of raw material microwax dropping point or less.It is described
Be cooled to final temperature after, increase the cryogenic thermostat stage so that solid crystal is more abundant, time in cryogenic thermostat stage is 0~
3.0 hours, preferably 0.1~3.0 hour, more preferably 1.0~3.0 hours.
In the method for the present invention, the step（3）Sweating effort heating rate preferably 1.0 DEG C/h~2.0 DEG C/h.Its
Final temperature, that is, predetermined temperature of middle temperature-rise period is less than 2 DEG C~10 DEG C of purpose product dropping point.Described being warming up to is default
After temperature, increase the constant temperature stage so that solids fraction detaches more fully with liquid composition, the time in constant temperature stage is 0~5.0 small
When, preferably 0.1~5.0 hour, preferably 1.0~5.0 hours.
In the method for the present invention, the heating rate and cooling rate 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.Wax layer heating is controlled using water-bath or oil bath mode
When rate and rate of temperature fall, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function, the substances such as water or conduction oil are added as circulatory mediator in the circulatory system；Coil pipe is soaked after charging
Not and be fixed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the method for the present invention, the step（3）The wax layer that forces air flow through can be real in sweating effort any stage
It applies, preferably implements at sweating initial stage.
In the method for the present invention, the step（3）The wax layer that forces air flow through be utilized in above wax layer and increase air pressure
It realizes, can such as apply 20~200 kPa above wax layer（Gauge pressure）Air pressure, and wax layer below remain normal pressure.
In the method for the present invention, the step（3）The wax layer that forces air flow through be utilized in below wax layer and reduce air pressure
It realizes, such as can keep normal pressure in the air pressure above wax layer, and maintain -20~-80 kPa below wax layer（Gauge pressure）Air pressure.
Sweating separation method is to be detached using various components property with different melting point to produce pertroleum wax, for stone
Oily wax sweating process studies have shown that liquid composition is gradually discharged along crystalline portion in sweating effort, be similar to liquid
The case where being flowed in capillary.For crystallite wax product, since its main component is isoparaffin and cycloalkane, chemical composition
Complexity causes crystals upon crystallization structure more fine and compact, forms huge filter flow resistance power to the discharge of liquid composition, this just makes
It is difficult to be kept completely separate with liquid composition at solids fraction in the common sweating effort for only leaning on gravity natural separation.Therefore common sweating
De-oiling technique cannot produce the crystallite wax product for meeting relevant criterion, can not produce the crystallite wax product of high dropping point.
The present invention in order to allow sweating it is this it is solvent-free production pertroleum wax method produce high dropping point crystallite wax product,
By the further investigation to common sweating effort, the reason of being difficult to detach with liquid composition for solids fraction, by sweating
It uses in the process and forces air flow through wax layer, while increasing high temperature constant temperature stage and cryogenic thermostat rank further preferably in crystallization process
The processes such as the constant temperature stage of section and sweating effort；And in sweating effort by way of placing solid mass on wax layer surface
Pressure is applied to wax layer, these measures make the property of product disclosure satisfy that relevant technology requirement.
The reason of being difficult to detach for wax in sweating effort and oil, by being taken by wax layer using air-flow in sweating effort
The method for taking fluid oil out of forces the separation of liquid composition and solids fraction, enhances separating effect and accelerates separating rate；
The crystallization bigger of pertroleum wax can be made by increasing the high temperature constant temperature stage in crystallization process, be conducive to liquid composition in sweating effort
Discharge.For microwax crystallization process studies have shown that the chemical composition of raw material is to determine the main factor of crystal habit, together
When cooling procedure condition can also influence crystal habit, especially the cooling condition at the temperature near fusing point is to crystal habit
Influence it is most apparent.Microwax has partially crystallizable when being cooled near dropping point and is precipitated, this partially crystallizable body can conduct
It is subsequently formed the nucleus of crystallization, increases the high temperature constant temperature stage at this time, nucleus can be enable fully to increase, is formed larger sized
Crystal, although this larger sized crystal is coarse not as good as the crystallization of soap manufacturing paraffin and low melt point paraffin, to the sweating stage
It is also highly beneficial that liquid composition, which is discharged,.
In common sweating effort, with the gradual discharge of liquid composition, wax layer will produce contraction and the level of vertical direction
The contraction in direction, when above and below wax layer formed pressure difference to force air flow through wax layer when, it some times happens that air-flow through wax layer with
Gap is flowed through and the phenomenon that without wax layer between ware plate.In the method for the present invention, by the side for placing solid mass on wax layer surface
Formula applies wax layer the means of pressure, and the liquid composition coated in extrudable wax crystallization is to accelerate solids fraction and liquid group
The separating rate divided, it is often more important that wax layer can be made only to generate contraction of the contraction of vertical direction without generating horizontal direction,
Increase the resistance between wax layer and baffle and ware plate；Simultaneously because there is perforative gap up and down inside solid mass, it can be ensured that
Air-flow is by wax layer to carry out liquid composition.Being aided with the cryogenic thermostat stage of crystallization process again keeps solid crystal more abundant, with
And the constant temperature stage of sweating effort, so that solids fraction is detached with liquid composition the methods of more abundant so that sweating process can produce
The crystallite wax product of high dropping point.
It is an advantage of the invention that：Crystalline size is increased using high temperature crystallization；Liquid group is carried out by wax layer using air-flow
The method divided enhances the separating effect of solids fraction and liquid composition and accelerates separating rate；Lead in sweating effort simultaneously
Cross in wax layer place solid mass to accelerate the separating rate of solids fraction and liquid composition and ensure airflow through wax layer, from
And sweating process is allow to produce high dropping point crystallite wax product.The method of the present invention is low with plant investment, production process is simple
List and the advantages that operating cost is low, safe, energy saving and solvent-free pollution environment.
Specific implementation mode
Sweating ware top connects dismountable sealing device and is connect with pressurized buffer tank and compressor, and/or in sweating
Ware lower part connects pressure-reducing cushioning tank and vacuum pump；It is packed into sweating ware after micro-crystal wax feed heating fusing；With oil bath control wax layer liter,
Cooling rate；Wax layer temperature be down to raw material dropping point temperature nearby and constant temperature for a period of time；Continue to be cooled to preset temperature and perseverance
Warm a period of time；In sweating effort, start compressor in wax layer positive pressure formed above, and/or start vacuum pump in wax
Layer negative pressure formed below, to force air flow through wax layer；Preferably gradually increase solid pressure on wax layer surface in sweating effort
By force；Wax layer temperature reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；On wax after refined, molding, packaging i.e.
For high dropping point crystallite wax product.
The method for illustrating sweating of the present invention and the high dropping point microwax of production below by way of specific embodiment.
Comparative example 1
This comparative example includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）It rises
Temperature-constant temperature sweating,（4）The processes such as product purification.
（1）Preparation
By sweating ware（Inner wall is the square of 1m × 1m）Sealing system connected with pressurized buffer tank and compressor；
Pressure-reducing cushioning tank is installed and connects vacuum pump in sweating ware lower part；Sweating ware chuck and removable coil pipe are connect with the circulatory system,
Using conduction oil as medium；The heating function for starting the circulatory system, makes recycle oil be warming up to 97 DEG C.Fang Shui below sweating ware ware plate.
With No. 90 microwaxes（Nanyang wax Fine Chemical Works, 90.35 DEG C of fusing point；90.77 DEG C of dropping point；Oil content
1.76%）For raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and is fixed.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
The refrigerating function for starting the circulatory system makes wax layer temperature drop to 91.0 DEG C and perseverance with the rate of temperature fall of 2.0 DEG C/h
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystal fully increases；Wax layer temperature is set to drop to the rate of temperature fall of 1.5 DEG C/h again
80.0 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.
（3）Heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank（Ⅰ）To receive under wax；Connect sweating ware top seal
Device；Start compressor and keeps pressurized buffer tank internal pressure strong stability in 130~150kPa（Gauge pressure）, sweating ware ware plate lower section is protected
Hold normal pressure；Start circulation system function, so that wax layer temperature is increased to 88.0 DEG C with the heating rate of 1.5 DEG C/h.Stop compressing
Machine removes sealing device.
It opens vacuum pump and keeps surge tank internal pressure strong stability in -40~-60 kPa（Gauge pressure）, the air pressure holding of wax layer top
Normal pressure；Wax layer temperature is set to be increased to 94.0 DEG C of simultaneously constant temperature 4.0 hours with the heating rate of 1.0/h, so that the solid-state group in wax layer
Divide and is sufficiently separated with liquid composition.Stop vacuum pump, terminates sweating degreasing process.
Sweating ware exports changing-over crude product storage tank（Ⅰ）To receive on wax；Continue increase recycle oil temperature to 110 DEG C, with
Fusing is taken out on wax, as crude product（Ⅰ）.
（4）Product purification
Crude product（Ⅰ）It is high dropping point crystallite wax product after clay-filtered, molding, packaging（Ⅰ）.
High dropping point crystallite wax product（Ⅰ）Property：Dropping point：96.5 DEG C, oil content：0.87%.Crystallite wax product（Ⅰ）'s
Yield is 14.8%（Relative to raw material microwax）.
Embodiment 1
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）It rises
Temperature-constant temperature sweating,（4）Product purification.
（1）Preparation
It is several to prepare stainless steel plate, every piece of stainless steel plate overall dimensions are the m of 0.98 m × 0.98m × 0.02, and stainless
The through hole of 0.0015 m of equally distributed φ is bored on steel plate（It drills away from being risen at edge 0.01m, hole center spacing 0.04m）（Often
The pressure about 1.5kPa that block stainless steel plate generates）, spare.
By sweating ware（With comparative example 1）Sealing system connected with pressurized buffer tank and compressor；In sweating ware lower part
Installation pressure-reducing cushioning tank simultaneously connects vacuum pump；Sweating ware chuck and removable coil pipe are connect with the circulatory system, are with conduction oil
Medium；Start circulation system function, cycle oil medium is made to be warming up to 97 DEG C.Water is padded below sweating ware ware plate.
With No. 90 microwaxes（With comparative example 1）For raw material, sweating ware is added after heating fusing.Coil pipe is immersed in paraffin
It is in layer and fixed.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
The refrigerating function for starting the circulatory system makes wax layer temperature drop to 91.0 DEG C and perseverance with the rate of temperature fall of 2.0 DEG C/h
Temperature carries out high temperature constant temperature in 2.0 hours, so that crystal fully increases；Wax layer temperature is set to drop to the rate of temperature fall of 1.5 DEG C/h again
80.0 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.
（3）Heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；On wax layer surface, level is put
Set first piece of aforementioned stainless steel plate；Connect sweating ware sealing device for upper portion of annular；Start compressor and keeps pressure in pressurized buffer tank
Stablize in 130~150kPa（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system function, with 1.5 DEG C/h
Heating rate so that wax layer temperature is increased to 88.0 DEG C.Stop compressor.Remove sealing device.
Second piece of aforementioned stainless steel plate is placed on wax layer surface；Open vacuum pump and keep surge tank internal pressure strong stability-
40~-60 kPa（Gauge pressure）, wax layer top air pressure holding normal pressure；Wax layer temperature is set to be increased to 94.0 with the heating rate of 1.0/h
℃；The aforementioned stainless steel plate of third block is placed on wax layer surface；And constant temperature 4.0 hours is so that the solids fraction in wax layer and liquid group
Divide and is sufficiently separated.Stop vacuum pump, terminates sweating degreasing process.
The outlet of sweating ware is changed to connection crude product storage tank（Ⅱ）To receive on wax.Continue to increase the temperature of recycle oil to 110
DEG C, it is taken out on wax with fusing, as crude product（Ⅱ）.
（4）Product purification
Crude product（Ⅱ）It is high dropping point crystallite wax product after clay-filtered, molding, packaging（Ⅱ）.
High dropping point crystallite wax product（Ⅱ）Property：Dropping point：97.2 DEG C, oil content：0.41%.Crystallite wax product（Ⅰ）
Yield be 17.6%（Relative to raw material microwax）.
By embodiment 1 and comparative example 1 as can be seen that the method for sweating of the present invention and the high dropping point microwax of production, leads to
Cross the improvement for increasing pressurization and/or vacuum facility etc. to sweatbox；It is sent out by placing solid mass in wax layer, and in heating
The improvement to sweating process such as wax layer, the constant temperature stage for increasing cooling and temperature-rise period is forced air flow through during sweat；Enhancing
Solids fraction and the separating effect of liquid composition simultaneously accelerate separating rate, to make this solvent-free process life of sweating de-oiling
The high dropping point crystallite wax product of output.
Claims (24)
1. a kind of method of sweating and the high dropping point microwax of production, including the following contents：
（1）Charging：The microwax for being 87 DEG C~92 DEG C using dropping point is packed into sweatbox as raw material after heating fusing；
（2）Crystallization：Wax layer is cooled to proper temperature with the rate of 1.0 DEG C/h~3.0 DEG C/h, high temperature constant temperature is for a period of time；Again
The cooling final temperature of 5 DEG C~20 DEG C of raw material fusing point or less, and cryogenic thermostat are cooled to the rate of 0.5 DEG C/h~2.5 DEG C/h
For a period of time；
（3）Heating-constant temperature sweating：It is heated up with the rate of 0.5 DEG C/h~2.5 DEG C/h；Wax layer reaches one section of predetermined temperature and constant temperature
Stop sweating after time；Wax layer is forced air flow through in sweating effort, and places solid mass on wax layer surface with to wax layer
Apply the pressure of 0.5kPa or more；There is perforative hole up and down inside the solid mass；
（4）It is refined：After refined, molding, packaging it is high dropping point crystallite wax product on wax.
2. according to the method for claim 1, which is characterized in that the solid mass is 1.4 to the pressure that wax layer generates
~20.0 kPa.
3. according to method as claimed in claim 1 or 2, which is characterized in that the solid mass surfacing, overall dimensions are omited
Less than sweatbox inner wall size.
4. according to the method for claim 1, which is characterized in that the density of the solid mass is more than 4g/cm3。
5. according to the method for claim 4, which is characterized in that the material of the solid mass is selected from zinc, iron, copper, lead
And its alloy.
6. according to the method for claim 1, which is characterized in that described to place solid mass using following on wax layer surface
Mode：The solid mass of 0.5kPa or more pressure can be generated by being added at one time in sweating effort.
7. according to the method for claim 6, which is characterized in that be added at one time when sweating starts and can generate 1.4~
The solid mass of 20.0kPa pressure.
8. according to the method for claim 1, which is characterized in that described to place solid mass using following on wax layer surface
Mode：It is added several times in sweating effort, the solid weight that can generate 0.5kPa or more pressure is added in every 0.1~20.0 h
Object.
9. according to the method for claim 8, which is characterized in that 1.4~10.0 can be generated by being added in every 0.1~10.0 h
The solid mass of kPa pressure.
10. according to the method for claim 1, which is characterized in that step（3）Described in force air flow through wax layer use
Increase air pressure above wax layer and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize, the pressure
Poor by force is 10~500 kPa.
11. according to the method for claim 1, which is characterized in that step（2）In temperature-fall period before high-temperature constant temperature section
Rate of temperature fall be 1.5 DEG C/h~2.5 DEG C/h, rate of temperature fall after high-temperature constant temperature section is 1.0 DEG C/h~2.0 DEG C/h.
12. according to the method for claim 1, which is characterized in that step（2）Described in proper temperature be raw material drip melt
- 1.0 DEG C of point~+2.0 DEG C of dropping point.
13. according to the method for claim 8, which is characterized in that step（2）Described in proper temperature be raw material microwax
Dropping point~+1.0 DEG C of dropping point.
14. according to the method for claim 1, which is characterized in that step（2）The time of the high-temperature constant temperature section of middle temperature-fall period
0.1~4.0 hour.
15. according to the method for claim 1, which is characterized in that step（2）Described in the predetermined temperature that cools down be less than raw material
8 DEG C~15 DEG C of microwax dropping point.
16. according to the method for claim 1, which is characterized in that step（2）Described in time in cryogenic thermostat stage be
0.1~3.0 hour.
17. according to the method for claim 1, which is characterized in that step（3）Described in the heating rate of sweating effort be
1.0 DEG C/h~2.0 DEG C/h.
18. according to the method for claim 1, which is characterized in that step（3）Described in the predetermined temperature that heats up be less than mesh
2 DEG C~10 DEG C of product dropping point.
19. according to the method for claim 1, which is characterized in that step（3）Described in time of constant temperature be 0.1~5.0 small
When.
20. according to the method for claim 1, which is characterized in that step（3）Described in the wax layer that forces air flow through be to adopt
Increase what air pressure was realized above wax layer：Apply the gauge pressure pressure of 20~200 kPa above wax layer, and is kept below wax layer
For normal pressure.
21. according to the method for claim 1, which is characterized in that step（3）Described in the wax layer that forces air flow through sending out
Sweat initial stage implements.
22. according to the method for claim 20, which is characterized in that step（3）Described in the wax layer that forces air flow through be
Using the increase air pressure realization above wax layer：Apply the gauge pressure pressure of 20~200 kPa above wax layer, and is protected below wax layer
It holds as normal pressure.
23. according to the method for claim 20, which is characterized in that step（3）Described in the wax layer that forces air flow through be
Using the reduction air pressure realization below wax layer：Air pressure keeps normal pressure above wax layer, and -20~-80 are maintained below wax layer
The gauge pressure pressure of kPa.
24. according to the method for claim 10, which is characterized in that the pressure difference is 20~200kPa.
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Citations (3)
| 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 |
| CN1760278A (en) * | 2004-10-12 | 2006-04-19 | 中国石油天然气股份有限公司 | Wax-for preventing rubber |
| CN101649119A (en) * | 2009-03-20 | 2010-02-17 | 上海绿菱特种蜡制品厂 | Novel rubber protective wax |
-
2015
- 2015-12-15 CN CN201510928625.9A patent/CN106883888B/en active Active
Patent Citations (3)
| 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 |
| CN1760278A (en) * | 2004-10-12 | 2006-04-19 | 中国石油天然气股份有限公司 | Wax-for preventing rubber |
| CN101649119A (en) * | 2009-03-20 | 2010-02-17 | 上海绿菱特种蜡制品厂 | Novel rubber protective wax |
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| CN106883888A (en) | 2017-06-23 |
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