CN106883890B - A kind of sweating and the method for producing paraffin - Google Patents
A kind of sweating and the method for producing paraffin Download PDFInfo
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- CN106883890B CN106883890B CN201510928630.XA CN201510928630A CN106883890B CN 106883890 B CN106883890 B CN 106883890B CN 201510928630 A CN201510928630 A CN 201510928630A CN 106883890 B CN106883890 B CN 106883890B
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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
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Abstract
The invention discloses a kind of sweating and the methods for producing paraffin.This method is on the basis of common sweating de-oiling technique, the oil of liquid is carried out to force separation wax and oil by wax layer using air-flow in sweating effort, and apply pressure in wax layer to accelerate the separating rate of wax and oil and ensure airflow through wax layer in sweating effort, to improve purpose product yield while shorten the production cycle, and this solvent-free de-oiling method of sweating can be allow to produce high melting point paraffin 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 the method for producing paraffin.
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.Paraffin be in crude oil lube cut through dewaxing, de-oiling, refined and molding
Production, typically contain C20~C50The components such as n-alkane, a small amount of isoparaffin and cycloalkane, usual fusing point is 50 DEG C~
74℃。
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% scale wax below of oil content is prepared using slack wax as raw material, is taken off
Oily technique mainly has solvent deoiling and sweating de-oiling.Scale wax again through clay-filtered or hydrofinishing and molding, packaging and other steps,
It can be obtained commodity oil wax.
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；（4）It is refined：Continue to increase temperature after sweating effort, be taken out on wax with fusing, as crude product；Crude product essence
System：Generally use is clay-filtered（It is warming up to predetermined temperature after crude product is melted, carclazyte is added and constant temperature was stirred to the predetermined time
After filter）；It is again purpose product through being molded, packing.
To common sweating de-oiling technique, in sweating effort although wax and oily two class components are respectively at solid and liquid
State, but also be difficult to be kept completely separate.To make the oil content of final products meet the requirements, generally use extends sweating sessions and improves
The method of sweating final temperature.Extending sweating sessions can cause the production cycle long；Improving sweating final temperature can cause product to be received
Rate declines.
Common sweating de-oiling method can produce fusing point in 40 DEG C~60 DEG C of soap manufacturing paraffin and low melt point paraffin, be not suitable for
Produce high melting point paraffin product of the fusing point at 70 DEG C or so.Have experiments have shown that, common sweating de-oiling technique productions fusing point is at 70 DEG C
When the high melting point paraffin product of left and right, even if using the method for extending sweating sessions and improving sweating final temperature, the sweating later stage
Oil content on wax is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, so common sweating de-oiling work
Skill is not suitable for producing fusing point meets semi-refined or full refining product standard high melting point paraffin product at 70 DEG C or so, especially
Oil-containing figureofmerit cannot meet technical requirement.
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.
For many years, sweating de-oiling method has obtained some development, such as CN89214332 in production equipment and process aspect（It is vertical
Formula square multipul sections spacer diaphoresis tank）,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 that there are still product yields is relatively low for these methods,
The shortcomings of production cycle is longer, and cannot still produce and meet semi-refined or full refining product standard high melting point paraffin product.
Sweating de-oiling technique is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product,
Advocating environmentally protective, low-carbon energy-saving the concern for being increasingly subject to people today.To improving the efficiency of sweating method, or even use
The demand of sweating de-oiling technique productions high melting point paraffin product is also more urgent.
Invention content
In view of the deficiencies of the prior art, a kind of method that the present invention provides sweating and produces paraffin, specifically uses
Sweatbox carries out liquid using air-flow in sweating effort on the basis of common sweating de-oiling technique by wax layer
Oil to force separation wax and oil, in sweating effort by way of placing solid mass in wax layer to wax layer apply pressure with
Accelerate the separating rate of wax and oil and ensure airflow through wax layer, to improve purpose product yield while shorten production week
Phase, and can be used for production high melting point paraffin product.The method of the present invention have that investment of production equipment is low, production process is simple and
Operating cost is low, energy-saving safe and the advantages that solvent-free pollution.
A kind of sweating of the present invention and the method for producing paraffin, including the following contents：
（1）Charging：Slack wax using oil content less than 30% is packed into sweatbox as raw material after heating fusing；
（2）Crystallization：The pre- constant temperature of 8 DEG C~20 DEG C of slack wax fusing point or less is cooled to the rate of 1.0 DEG C/h~4.0 DEG C/h
Degree；
（3）Sweating：It is heated up with the rate of 0.5 DEG C/h~3.0 DEG C/h；Wax layer is forced air flow through in temperature-rise period；Wax
Layer stops sweating after reaching predetermined temperature；
（4）It is refined：After refined, molding it is purpose product on wax.
In the method for the present invention, the oil content of the raw material slack wax（In mass）Less than 30%, melting range is generally
45 DEG C~70 DEG C.Slack wax raw material can be vacuum 1st side cut, second line of distillation, the line that subtracts three or the line distillate that subtracts four through slack wax made from dewaxing.
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 pressure.Solid mass surfacing, overall dimensions are slightly less than sweatbox inner wall size（Such as, solid mass edge
It is generally 0.01~50mm, preferably 0.1~20mm with the gap of sweatbox inner wall）, inside have up and down perforative gap.Solid
The density of weight generally requires to be more than 4 g/cm3, can be the materials such as nonmetallic, metal and alloy, preferred density is 6~12
g/cm3Metal and alloy, such as zinc, iron, copper, lead and its more stable low price metal material of alloy chemical property.
In the present invention, one of following manner may be used, solid mass is placed on wax layer surface to apply pressure to wax layer
By force：（1）The solid mass of 0.5kPa or more pressure can be generated by being added at one time in sweating effort, preferably when sweating starts one
The solid mass that can generate 1.4~20.0kPa pressure is added in secondary property；（2）It is added several times in sweating effort, preferably 2~3
It is secondary, i.e., the solid mass that can generate 0.5kPa or more pressure is added in every 0.1~20.0 h, preferably in 0.1~10.0 h
The solid mass of 1.4~10.0kPa pressure can be generated by being added.
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.Described forces air flow through wax layer using the increase air pressure above wax layer and/or in wax layer
Lower section reduces air pressure, so that wax layer upper and lower is formed pressure difference and realizes.The pressure difference is generally 10~500 kPa, preferably
20~200 kPa, to force air flow through wax layer.
In the method for the present invention, rate of temperature fall preferably 1.5 DEG C/h~3.0 DEG C/h of the raw material wax layer crystallization process.Institute
State 10 DEG C~15 DEG C of cooling final temperature preferred raw material slack wax fusing point or less.
In the method for the present invention, heating rate preferably 1.0 DEG C/h~2.0 DEG C/h of the raw material wax layer sweating effort.Institute
The predetermined temperature for stating heating is 2 DEG C~10 DEG C of the fusing point less than purpose product.
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.
It is described to force air flow through wax layer and implement in sweating effort any stage in the method for the present invention, preferably
Implement at sweating initial stage.
In the method for the present invention, the wax layer that forces air flow through is utilized in what increase air pressure above wax layer was realized,
20~200 kPa can such as be applied above wax layer（Gauge pressure）Air pressure, and wax layer below remain normal pressure.
In the method for the present invention, the wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized,
Such as normal pressure can be kept in the air pressure above wax layer, and maintain -20~-100 kPa below wax layer（Gauge pressure）Air pressure.
Sweating de-oiling method is detached to produce paraffin, but in sweating using wax and oil property with different melting point
In the process, solid wax and the oil of liquid are difficult to be kept completely separate in wax layer, this is because wax and oily two kinds of components are all nonpolarity
Hydrocarbon molecules, intermolecular force is larger；Solid wax crystallization forms capillary pipe structure simultaneously, has stronger absorption to make oil
With this is resulted in only in the common sweating effort of gravity natural separation, and wax and oil are difficult to be kept completely separate.Generally use extends hair
The methods of sweat time, raising sweating final temperature make the oil content of final products meet the requirements, but this can lead to production week again
Phase is long, wax product yield is low.High melting point paraffin product for fusing point at 70 DEG C or so is led since chemical composition is more complicated
Cause crystals upon crystallization structure more fine and compact, wax and oil are more difficult to detach in common sweating effort, therefore common sweating is de-
Oily technique cannot produce fusing point and meet semi-refined or full refining product standard high melting point paraffin product at 70 DEG C or so.
The present invention in order to improve sweating de-oiling it is this it is solvent-free production paraffin method efficiency, it might even be possible to produce fusing point and exist
70 DEG C or so of high melting point paraffin product is difficult to be kept completely separate by the further investigation to common sweating effort for wax and oil
Reason is forced the separation of wax and oil by the method that wax layer carries out fluid oil using air-flow in sweating effort, enhanced point
From effect and accelerate separating rate.During common sweating process, with the gradual discharge of oil, wax layer will produce vertical direction
Contraction and horizontal direction contraction, when above and below wax layer formed pressure difference to force air flow through wax layer when, will produce sometimes
Air-flow flows through through gap between wax layer and ware plate and the phenomenon that without wax layer.In the method for the present invention, by being placed on wax layer surface
The mode of solid mass applies wax layer the means of pressure, and the oil coated in extrudable wax crystallization is to accelerate point of wax and oil
From speed, 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, increased
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 logical
It is fuel-displaced to carry to cross wax layer.
Compared with prior art, this have the advantage that：By passing through wax layer using air-flow in sweating effort
The method for carrying out fluid oil forces the separation of wax and oil, enhances separating effect and accelerates separating rate；Simultaneously in sweating
In the process by placing solid mass in wax layer to accelerate the separating rate of wax and oil and ensure airflow through wax layer, to reach
To improving product yield and shorten the purpose of production cycle, it might even be possible to produce high melting point paraffin product.The method of the present invention
Have many advantages, such as that plant investment is low, production process is simple and operating cost is low, safe, energy saving and solvent-free pollution environment so that
The method more highly effective of this solvent-free production paraffin of sweating de-oiling.
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 the heating fusing of raw material slack wax；Wax layer ascending, descending is controlled with water-bath
Warm speed；In sweating effort, start compressor in wax layer positive pressure formed above, and/or start vacuum pump with wax layer with
Lower formation negative pressure, to force air flow through wax layer；Preferably gradually increase solid pressure on wax layer surface in sweating effort；Wax
Layer temperature stops sweating effort after reaching preset temperature；It is purpose product to be after clay-filtered, molding, packaging on wax.Pass through
These means can make purpose product yield improve 3~15 percentages in the case where the time in sweating stage reduces 30%~50%
Point, and high melting point paraffin can be produced.
The method that 1-2 illustrates sweating of the present invention and produces paraffin by the following examples.
Comparative example 1
This comparative example includes：（1）Preparation,（2）Crystallization,（3）Sweating,（4）The processes such as refined.
（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 water as medium；The heating function for starting the circulatory system, makes recirculated water be warming up to 55 DEG C.Water is padded below sweating ware ware plate.
With Daqing crude oil second line of distillation slack wax（50.6 DEG C of fusing point, oil content 21.4%）For raw material, hair is added after heating fusing
Sweat ware；Coil pipe is immersed in raw material wax layer and is fixed.
（2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 37.0 DEG C with
Wax layer is set to crystallize to form solid.Close the refrigerating function of the circulatory system.
（3）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 120~140kPa（Gauge pressure）, sweating ware ware plate lower section is protected
Hold normal pressure.
The heating function for starting the circulatory system, makes wax layer temperature be increased to 43.0 DEG C with the heating rate of 1.5 DEG C/h.Stop pressing
Contracting machine.Remove sealing device.
Start vacuum pump and keeps pressure-reducing cushioning tank internal pressure strong stability in -50~-70 kPa（Gauge pressure）, wax layer top air pressure
Keep normal pressure；Continue to make wax layer temperature be increased to 49.0 DEG C of progress sweatings with the heating rate of 1.5 DEG C/h.Stop vacuum pump, terminates
Sweating effort（Sweating effort total time is 8 hours）.
（4）It is refined
The outlet of sweating ware is changed to connection crude product storage tank（Ⅰ）；Continue heat cycles water and is warming up to 70 DEG C with fusing taking-up wax
On, as crude product（Ⅰ）.
Crude product（Ⅰ）It is purpose product after clay-filtered, molding, packaging.
Product（Ⅰ）Property：54.7 DEG C of fusing point, oil content 1.52%, meet commodity 54#The relevant technology requirement of semi-refined wax.
54#Semi-refined wax product yield is 45.2%（Relative raw material slack wax）.
Comparative example 2
This comparative example includes：（1）Preparation,（2）Crystallization,（3）Sweating,（4）The processes such as refined.
（1）Preparation
By sweating ware（With embodiment 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, using water as medium；
The heating function for starting the circulatory system, makes recirculated water be warming up to 65 DEG C.Water is padded below sweating ware ware plate.
With the Daqing crude oil line slack wax that subtracts four（Initial boiling point：410 DEG C, 90% distillate a little：520℃；58.5 DEG C of fusing point；Oil content
26.9%）For raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and is fixed.
（2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 48.0 DEG C with
Wax layer is set to crystallize to form solid.Close the refrigerating function of the circulatory system.
（3）Sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；It is close to connect sweating ware top
Seal apparatus；Start compressor and keeps pressurized buffer tank internal pressure strong stability in 130~150kPa（Gauge pressure）, sweating ware ware plate lower section
Keep normal pressure.
The heating function for starting the circulatory system, makes wax layer temperature be increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h.Stop pressing
Contracting machine.Remove sealing device.
Start vacuum pump and keeps pressure-reducing cushioning tank internal pressure strong stability in -50~-70 kPa（Gauge pressure）, wax layer top air pressure
Keep normal pressure；Continue to make wax layer temperature be increased to 70.0 DEG C of progress sweatings with the heating rate of 2.0 DEG C/h.Stop vacuum pump, terminates
Sweating effort.
（4）It is refined
The outlet of sweating ware is changed to connection crude product storage tank（Ⅱ）；Continue heat cycles water and is warming up to 80 DEG C with fusing taking-up wax
On, as crude product（Ⅱ）.
Crude product（Ⅱ）It is purpose product after clay-filtered, molding, packaging.
Product（Ⅱ）Property：Fusing point：72.5 DEG C, oil content：0.75%.Meet commodity 72#The related skill of fully refined paraffin wax
Art requirement.72#Fully refined paraffin wax product yield is 11.1%（Relative to slack wax raw material）.
Embodiment 1
The present embodiment includes：（1）Preparation,（2）Crystallization,（3）Sweating,（4）The processes such as refined.
（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, using water as medium；
The heating function for starting the circulatory system, makes recirculated water be warming up to 55 DEG C.Water is padded below sweating ware ware plate.
With Daqing crude oil second line of distillation slack wax（With comparative example 1）For raw material, sweating ware is added after heating fusing；Coil pipe is submerged
It is in raw material wax layer and fixed.
（2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 37.0 DEG C with
Wax layer is set to crystallize to form solid.Close the refrigerating function of the circulatory system.
（3）Sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank（Ⅲ）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 keep in pressurized buffer tank stable gas pressure 120~
140kPa（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure.
The heating function for starting the circulatory system, makes wax layer temperature be increased to 43.0 DEG C with the heating rate of 1.5 DEG C/h.Stop pressing
Contracting machine.Remove sealing device.
Second piece of stainless steel plate is placed on wax layer surface；Start vacuum pump and keep in pressure-reducing cushioning tank stable gas pressure-
50~-70 kPa（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue to make wax layer temperature increase with the heating rate of 1.5 DEG C/h
To 49.0 DEG C.Stop vacuum pump, terminates sweating effort（Sweating effort total time is 8 hours）.
（4）It is refined
The outlet of sweating ware is changed to connection crude product storage tank（Ⅲ）；Continue heat cycles water and is warming up to 70 DEG C with fusing taking-up wax
On, as crude product（Ⅲ）.
Crude product（Ⅲ）It is purpose product after clay-filtered, molding, packaging.
Product（Ⅲ）Property：54.3 DEG C of fusing point, oil content 1.25%, meet commodity 54#The relevant technology requirement of semi-refined wax.
54#Semi-refined wax product yield is 49.3%（Relative raw material slack wax）.
Embodiment 2
The present embodiment includes：（1）Preparation,（2）Crystallization,（3）Sweating,（4）The processes such as refined.
（1）Preparation
It is several to prepare stainless steel plate（With embodiment 1）, 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, using water as medium；
The heating function for starting the circulatory system, makes recirculated water be warming up to 65 DEG C.Water is padded below sweating ware ware plate.
With the Daqing crude oil line slack wax that subtracts four（With comparative example 2）For raw material, sweating ware is added after heating fusing.Coil pipe is submerged
It is in raw material wax layer and fixed.
（2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 48.0 DEG C with
Wax layer is set to crystallize to form solid.Close the refrigerating function of the circulatory system.
（3）Sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank（Ⅳ）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 keep pressurized buffer tank internal pressure strong stability 130~
150kPa（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure.The heating function for starting the circulatory system, with the heating speed of 2.0 DEG C/h
Rate makes wax layer temperature be increased to 62.0 DEG C.Stop compressor, removes sealing device.
Second piece of stainless steel plate is placed on wax layer surface；Start vacuum pump and keep pressure-reducing cushioning tank internal pressure strong stability-
50~-70 kPa（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue to make wax layer temperature increase with the heating rate of 2.0 DEG C/h
To 70.0 DEG C of progress sweatings.Stop vacuum pump, terminates sweating effort.
（4）It is refined
The outlet of sweating ware is changed to connection crude product storage tank（Ⅳ）；Continue heat cycles water and is warming up to 80 DEG C with fusing taking-up wax
On, as crude product（Ⅳ）.
Crude product（Ⅳ）It is purpose product after clay-filtered, molding, packaging.
Product（Ⅳ）Property：Fusing point：72.7 DEG C, oil content：0.48%.Meet commodity 72#The related skill of fully refined paraffin wax
Art requirement.72#Fully refined paraffin wax product yield is 15.8%（Relative to slack wax raw material）.
Comparative example 3
With Daqing crude oil second line of distillation slack wax（With comparative example 1）For raw material, common sweat tank is added after heating fusing.With 2.0
DEG C/rate of temperature fall of h makes wax layer temperature drop to 37.0 DEG C；Wax layer temperature is set to be increased to 51.0 with the heating rate of 1.0 DEG C/h
DEG C carry out sweating de-oiling（Total heating-up time is 14 hours）.It is taken out on wax after sweating, is mesh after clay-filtered, molding
Product.
Product property：55.6 DEG C of fusing point, oil content 1.75%, meet commodity 54#The relevant technology requirement of semi-refined wax.54#Half
It is 37.4% to refine wax product yield.
By embodiment 1 and embodiment 2 as can be seen that the method for the present invention, passes through increase pressurization and/or vacuum facility etc.
Improvement to sweatbox；By placing solid mass in wax layer, and wax layer is forced air flow through in the sweating effort that heats up
Deng the improvement to sweating process；It enhances the separating effect of wax and oil and accelerates separating rate；To improve the production of purpose wax
Product yield（Embodiment 1 has increased separately 11.9 percentage points and 4.1 percentage points, embodiment compared with comparative example 3, comparative example 1
2 increase 4.7 percentage points compared with comparative example 2）And shorten the production cycle（The time in sweating stage, embodiment 1 relatively compare
Example 3 reduces 42.9%）.By embodiment 2 as can be seen that sweating of the present invention and the method for producing paraffin can produce fusing point height
In 70 DEG C of paraffin wax product.
Claims (16)
1. a kind of sweating and the method for producing paraffin, including the following contents：
（1）Charging：Using the slack wax that oil content is less than 30%, fusing point is 45 DEG C~70 DEG C as raw material, sweating dress is packed into after heating fusing
It sets；
（2）Crystallization：The predetermined temperature of 8 DEG C~20 DEG C of slack wax fusing point or less is cooled to the rate of 1.0 DEG C/h~4.0 DEG C/h；
（3）Sweating：It is heated up with the rate of 0.5 DEG C/h~3.0 DEG C/h；Wax layer is forced air flow through in temperature-rise period, and is passed through
Solid mass is placed to apply the pressure of 0.5kPa or more to wax layer on wax layer surface；Wax layer stops hair after reaching predetermined temperature
Sweat, the predetermined temperature are 2 DEG C~10 DEG C of the fusing point less than purpose product；Have inside the solid mass perforative up and down
Hole；
（4）It is refined：After refined, molding it is purpose product on wax.
2. according to the method for claim 1, which is characterized in that the solid mass surfacing, overall dimensions are smaller
In sweatbox inner wall size.
3. according to the method for claim 1, which is characterized in that the density of the solid mass is more than 4g/cm3。
4. according to the method for claim 1, which is characterized in that the solid mass is that density is 6~12g/cm3, solid
The material of weight is selected from one group of substance that zinc, iron, copper, lead and its alloy are constituted.
5. 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.
6. according to the method for claim 5, 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.
7. 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, i.e., the solid weight that can generate 0.5kPa or more pressure is added in every 0.1~20.0 h
Object.
8. according to the method for claim 7, 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.
9. 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.
10. according to the method for claim 9, which is characterized in that the pressure difference is 20~200 kPa.
11. according to the method for claim 1, which is characterized in that step（2）Described in the rate that cools down be 1.5 DEG C/h~
3.0℃/h。
12. according to the method for claim 1, which is characterized in that step（2）Described in predetermined temperature it is molten for raw material slack wax
Or less 10 DEG C~15 DEG C.
13. according to the method for claim 1, which is characterized in that step（3）Described in the rate that heats up be 1.0 DEG C/h~
2.0℃/h。
14. according to the method for claim 1, which is characterized in that described forces air flow through wax layer in sweating initial stage reality
It applies.
15. according to the method for claim 9, which is characterized in that the wax layer that forces air flow through uses in wax layer
Fang Zengjia air pressures are realized, apply the gauge pressure pressure of 10~500 kPa above wax layer, and remain normal pressure below wax layer.
16. according to the method for claim 9, which is characterized in that the wax layer that forces air flow through uses under wax layer
Side reduces air pressure and realizes, air pressure keeps normal pressure above wax layer, and the gauge pressure pressure of -20~-100 kPa is maintained below wax layer
By force.
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| CN201510928630.XA CN106883890B (en) | 2015-12-15 | 2015-12-15 | A kind of sweating and the method for producing paraffin |
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| CN201510928630.XA CN106883890B (en) | 2015-12-15 | 2015-12-15 | A kind of sweating and the method for producing paraffin |
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| CN106883890B true CN106883890B (en) | 2018-11-06 |
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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 |
| 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 |
-
2015
- 2015-12-15 CN CN201510928630.XA patent/CN106883890B/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 |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 发汗技术在相变石蜡开发中的应用;魏荣敏等;《石化技术》;20131231;第20卷(第4期);第21-24页 * |
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| CN106883890A (en) | 2017-06-23 |
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