CN106883886B - A method of producing microwax - Google Patents
A method of producing microwax Download PDFInfo
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- CN106883886B CN106883886B CN201510928608.5A CN201510928608A CN106883886B CN 106883886 B CN106883886 B CN 106883886B CN 201510928608 A CN201510928608 A CN 201510928608A CN 106883886 B CN106883886 B CN 106883886B
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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
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1081—Alkanes
- C10G2300/1085—Solid paraffins
Abstract
The invention discloses a kind of methods for producing microwax.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, generation gas is decomposed using inorganic salts simultaneously, and short space is formed in wax layer, it is also beneficial to the quick discharge of oil, so that sweating de-oiling method be allow to produce 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, safety, energy conservation and solvent-free pollution.
Description
Technical field
The invention belongs to pertroleum wax production technical fields, more particularly to a kind of method for producing microwax.
Background technique
The general name of the pertroleum wax all kinds of wax products obtained that are crude oil after refining processing from wax-containing distillate, including liquid
Body paraffin, soap manufacturing paraffin, paraffin and microwax.Microwax be decompression residuum after propane equal solvent depitching again through dewaxing, de-oiling,
Purification and molding and etc. production, generally by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition.Usually
The dropping point of microwax is 65 DEG C~92 DEG C, has the needle-like crystal structure more tiny than soap manufacturing paraffin and paraffin under solid-state.
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 the base oil wax below of oil content 2% is prepared using slack wax as raw material,
De-oiling technique mainly has solvent deoiling and sweating de-oiling.Base oil wax is again through clay-filtered or hydrofinishing and molding, packaging etc.
Commodity oil wax can be obtained in step.
Solvent deoiling method is according to wax and oil in selective solvent (acetone, benzene and toluene mixture；Or acetone, toluene；
Or methyl ethyl ketone, toluene) in the property of different solubility separated.Solvent deoiling technique with production process, receive by continuous, wax
Rate is high, finished product wax oil content can very low, lower production costs the advantages that, be the mainstream of current large-scale production petroleum paraffin product
De-oiling technique.But solvent deoiling technique investment of production equipment 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 separated using wax and oil property with different melting points.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 biggish n-alkane of molecular weight melts
Point is higher；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will be lower than n-alkane, and isomery degree gets over high-melting-point just
It is lower, or even be at normal temperature just in liquid condition, i.e., usually said oil.
Common sweating de-oiling technique mainly comprises the steps that (1) preparation: pad water is (with water full of sweatbox
Ware plate lower space) charge (raw material is heated to being packed into sweatbox when fusing point or more is in a liquid state) afterwards；(2) crystallize: by raw material with
Rate of temperature fall no more than 4 DEG C/h progressively cools to 10~20 DEG C of its fusing point or less.In cooling procedure, various components press fusing point
Sequence from high to low successively crystallizes 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
Low to high sequence be successively fused into liquid and flow out the wax layer residue (on wax) finally obtained (under wax) be exactly high-melting-point,
The wax of low oil-containing；Continue to increase temperature, be taken out on wax with fusing, as crude product；(4) it refines: generalling use clay-filtered (incite somebody to action
It is warming up to predetermined temperature after crude product fusing, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the predetermined time)；It formed, packed again
It is purpose product.
Common sweating de-oiling technique can produce soap manufacturing paraffin and low melting point stone under solid-state with coarse flaky crystal structure
Wax cannot but produce the microwax under solid-state with tiny needle-like crystal structure.Have experiments have shown that, common sweating de-oiling technique is raw
When producing microwax, even if the oil content using the method for extending sweating sessions and improving sweating final temperature, on sweating later period wax
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 the production of sweating de-oiling technique
The report of crystallite wax product.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is lower, 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 method has obtained some development in production equipment and process aspect, such as CN89214332(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), a kind of Efficient paraffin sweatbox of CN201210508905.0(),
CN201320127680.4(tubular type paraffin deoiler) etc., it is improved in sweating production equipment；CN91206202(is 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 lower, production week for these methods
The disadvantages of phase is longer, and these methods cannot still produce the microwax for meeting relevant criterion.
Sweating de-oiling technique is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product,
In the today for advocating green low-carbon, environmental protection and energy saving, the demand using sweating de-oiling technique production microwax is more urgent.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method for producing microwax, specifically uses sweating
Device, preferably incorporation is decomposable under stress on the basis of common sweating process, after raw material heating fusing generates gas
Inorganic salt powder；And the oil of liquid is carried out to force separation wax and oil by wax layer using air-flow in sweating effort, increase
Strong separating effect simultaneously accelerates separating rate.Inorganic salts are absorbed in the thermostatic process and sweating effort of crystallization decomposes having for generation
Evil gas.Unreacted inorganic salts and decomposition product are removed using water-washing method.The method of the present invention have investment of production equipment it is low,
Production process is simple and operating cost is low, energy-saving safe and the advantages that solvent-free pollution.
A kind of method producing microwax of the invention, including the following contents:
A, first segment sweating, comprising:
(A1) charge: using oil content less than 30%, melting range be 55 DEG C~80 DEG C slack wax as raw material, heating fusing (one
As can be heated to 1 DEG C~5 DEG C of raw material fusing point or more) be packed into sweatbox afterwards；
(A2) 8 DEG C~20 DEG C of raw material fusing point or less cooling-thermostatical crystallization: are cooled to 1.0 DEG C/h~4.0 DEG C/h rate
Predetermined temperature, and constant temperature is for a period of time；
(A3) heating-constant temperature sweating: with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；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；
(A4) it refines: being intermediate products after refining on wax；With
B, second segment sweating, comprising:
(B1) charge: the intermediate products obtained using first segment sweating (generally can be heated to centre after heating fusing as raw material
More than product fusing point 1 DEG C~5 DEG C) it is packed into sweatbox；
(B2) cooling-thermostatical crystallization: with 1.0 DEG C/h~4.0 DEG C/h rate be cooled to 8 DEG C of intermediate products fusing point or less~
20 DEG C of predetermined temperature, and constant temperature is for a period of time；
(B3) heating-constant temperature sweating: and then with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；Wax layer reaches predetermined temperature simultaneously
Constant temperature stops sweating afterwards for a period of time；Wax layer is forced air flow through in sweating effort；
(B4) it refines: being purpose product after being refined, being formed on wax.
In the method for production microwax of the invention, the sweating includes two sections of sweating efforts of process (A) and process (B).
The first segment sweating of process (A) for reducing raw material oil content and make purpose product be enriched with, and the second segment sweating of process (B) after
Continuous de-oiling produces microwax.For the oil content (in mass) of process (A) the raw material slack wax less than 30%, melting range is general
It is 55 DEG C~80 DEG C, can is decompression residuum through slack wax made from depitching matter, dewaxing.Process (B) raw material is first segment
Intermediate products obtained by sweating.
In the method for production microwax of the invention, preferably incorporation is decomposable under stress after raw material heating fusing
The inorganic salt powder of gas is generated, the pressure (gauge pressure) is generally 0.5~15.0 atmospheric pressure, preferably 1.0~8.0
Atmospheric pressure.The inorganic salt powder can be decomposed slowly in sweating effort releases gas and itself and decomposition product is easy
It is dissolved in water, can be one or more of ammonium salt, carbonate, bicarbonate.The granularity of the inorganic salt powder be 50~
500 mesh, additional amount account for 0.1%~10.0%(weight of sweating raw material), preferred ratio is 0.2%~3.0%.In the constant temperature of crystallization
Inorganic salts are absorbed in process and sweating effort decomposes the pernicious gas generated.It is not anti-using water-washing method removal in subtractive process
The inorganic salts and decomposition product answered.
In the method for production microwax of the invention, the sweatbox is generally sweating ware, and increases more than wax layer
Add dismountable sealing system and pressurizing device, to crystallize in the charging process of step (A1), (B1) and step (A2), (B2)
Inhibit inorganic salts to decompose the gas generated in temperature-fall period and escapes wax layer.The pressure (gauge pressure) is 0.5~15 atmospheric pressure,
Preferably 1~8 atmospheric pressure.
In the method for production microwax of the invention, the sweatbox is sweating ware, and wax layer it is added above plus
Pressure device and/or increase vacuum plant below wax layer.In step (A3) and step (B3) sweating effort, the pressure gas
Stream is used by wax layer to be increased air pressure above wax layer and/or reduces air pressure below wax layer, and wax layer upper and lower is made to form pressure
Difference is realized.The pressure difference is generally 0.1~5 atmospheric pressure, preferably 0.2~2 atmospheric pressure, to force air flow through wax
Layer.
In the method for production microwax of the invention, the drop of step (A2) and step (B2) the raw material wax layer crystallization process
Warm rate preferably 1.5 DEG C/h~2.5 DEG C/h.The predetermined temperature of cooling described in step (A2) be preferably shorter than 10 DEG C of slack wax fusing point~
15℃；And the predetermined temperature of step (B2) described cooling is preferably shorter than 10 DEG C~15 DEG C of intermediate products fusing point.
It is excellent after being cooled to predetermined temperature in step (A2) and step (B2) in the method for production microwax of the invention
Choosing increases the constant temperature stage so that solid crystal is more abundant.The time in constant temperature stage be 0.1~3 hour, preferably 1~3 hour, together
When gradually decrease pressure to normal pressure.The reduction speed of the pressure is generally 0.01~150 atm/h, preferably 0.2~80
Atm/h, more preferably 0.3~10 atm/h.
In the method for production microwax of the invention, the heating rate of raw material wax layer is excellent in step (A3) and step (B3)
Select 1.0 DEG C/h~2.0 DEG C/h.The predetermined temperature to heat up in step (A3) is the step lower than 2 DEG C~10 DEG C of fusing point of intermediate products
(B3) predetermined temperature to heat up in is lower than 2 DEG C~10 DEG C of fusing point of purpose product.
In the method for production microwax of the invention, the sweating that heats up in step (A3) and step (B3) is to producing product
After preset temperature, preferably the increase constant temperature stage, the time in constant temperature stage was 0~5 hour, excellent so that the separation of wax and oil is more abundant
It is selected as 0.1~5 hour, most preferably 1~5 hour.
In method of the 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, collet can be increased outside sweating ware, collet is connected with removable coil pipe and the circulatory system, collet, disk
Pipe etc. can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature；The circulatory system has program cooling/heating function, circulation
The substances such as water or conduction oil are added as circulatory mediator in system.
In the method for production microwax of the invention, the wax layer that forces air flow through can be in sweating effort arbitrary order
Section is implemented, and preferably implements at sweating initial stage.
In the method for production microwax of the invention, the wax layer that forces air flow through is utilized in increase above wax layer
What air pressure was realized, it can such as apply the pressure of 0.2~2.0 atmospheric pressure (gauge pressure) above wax layer, and remained often below wax layer
Pressure.
In the method for production microwax of the invention, the wax layer that forces air flow through is utilized in reduction below wax layer
What air pressure was realized, normal pressure can be such as kept above wax layer, and -0.2~-1.0 atmospheric pressure (gauge pressure) are maintained below wax layer
Pressure.
In the method for production microwax of the invention, the sweatbox can also connect absorption system, to crystallize
Thermostatic process and sweating effort in absorb inorganic salts decompose generate pernicious gas.Absorption system uses liquid absorption mode.
Sweating de-oiling method be separated using wax and oil property with different melting points to produce pertroleum wax, but for
Crystallite wax product, since its main component is isoparaffin and cycloalkane, chemical composition is complicated, leads to crystals upon crystallization structure more
Add fine and compact, huge filter flow resistance power is formed to the discharge of fluid oil, this results in the common hair for only leaning on gravity natural separation
Wax and oil are difficult to be kept completely separate during sweat.Therefore common sweating de-oiling technique cannot produce the microwax production for meeting relevant criterion
Product.
The present invention passes through to allow the method for this solvent-free production pertroleum wax of sweating de-oiling to produce crystallite wax product
Further investigation to common sweating effort is difficult to the reason of separating for wax and oil, by logical using air-flow in sweating effort
Crossing the method that wax layer carries out fluid oil forces oil to enhance separating effect with the separation of wax and accelerate separating rate；Increase
The constant temperature stage of crystallization process is conducive to make wax layer crystallization more abundant, at the same the constant temperature stage for increasing sweating effort be conducive to wax and
Oil is sufficiently separated.Incorporation can decompose the inorganic salt fines for generating gas under stress further preferably after raw material heating fusing simultaneously
End, these substances slowly settle in the wax layer of liquid due to granularity is smaller.It keeps that raw material is cooled to fusing point under pressure condition
10 DEG C below~15 DEG C, and constant temperature 0.1h~3h is so that wax layer crystallization is more abundant；Pressure is gradually decreased in thermostatic process simultaneously
To normal pressure.Raw material is cooled to wax layer in the time terminated after fusing point or less to sweating effort and is in softer solid state, this mistake
Inorganic salts slowly decompose the gas released in journey, micro-bubble can be formed in wax layer, the space that these micro-bubbles are formed
It is easy to be formed several tiny channels in sweating effort in wax layer, to be conducive to discharge oily in sweating effort.These
Improvement allows sweating de-oiling technique to produce crystallite wax product.
This have the advantage that: the method by using air-flow to carry out fluid oil by wax layer in sweating effort
The separation for forcing wax and oil, enhances separating effect and accelerates separating rate；The gas generated is decomposed using inorganic salts simultaneously
Short space is formed in wax layer, is also further conducive to the quick discharge of oil, so that it is micro- to produce sweating de-oiling technique
Brilliant wax product.Method of the invention has that plant investment is low, production process is simple and operating cost is low, safety, energy conservation and without molten
The advantages that environment, is polluted in agent.
Specific embodiment
Sweating ware top connects dismountable sealing device and connect with pressurized buffer tank and compressor, and/or in sweating
Ware lower part connects pressure-reducing cushioning tank and vacuum pump；Raw material heating is melted and is filled after preferably mixing inorganic salt powder under stress
Enter sweating ware；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature is down to preset temperature and constant temperature for a period of time；In sweating
In the process, starting compressor is in wax layer positive pressure formed above, and/or starting vacuum pump is to use in wax layer negative pressure formed below
To force air flow through wax layer；Wax layer temperature reaches preset temperature and constant temperature stops sweating afterwards for a period of time；By two sections of hair
It is crystallite wax product after refining on wax after sweat de-oiling.
The method of production microwax of the invention is illustrated by the following examples.
Embodiment 1
The present embodiment includes A: first segment sweating and B: second segment sweating two parts.
A: first segment sweating
This process includes: (A1) preparation, (A2) cooling-thermostatical crystallization, (A3) heating-constant temperature sweating, (A4) essence
The processes such as system.
(A1) preparation
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；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.The sealing system on sweating ware top is installed and is connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump.Starting compressor simultaneously keeps pressurized buffer pressure inside the tank steady
It is scheduled on 3.4~3.6 atmospheric pressure (gauge pressure).
With Daqing crude oil residue slack wax (initial boiling point: 420 DEG C, 90% distillate a little: 550 DEG C；63.0 DEG C of fusing point；Oil content
20.3%) it is raw material, sweating ware is added under 3.4~3.6 atmospheric pressure (gauge pressure) after being heated to 65 DEG C of fusings.
(A2) cooling-thermostatical crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2 DEG C/h drop to 52.0 DEG C so that
Wax layer crystallizes to form solid, and constant temperature 1 hour so that wax layer sufficient crystallising.The constant temperature stage controls pressurized buffer by emptying system
Pressure inside the tank is reduced to normal pressure with the rate of 4.0~4.4atm/h.Close the refrigerating function of the circulatory system.
(A3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (I) is to receive under wax；Start compressor and keeps adding
Pressure buffering pressure inside the tank is stablized keeps normal pressure below 1.3~1.5 atmospheric pressure (gauge pressure), sweating ware ware plate.Start cyclic system
System heating function, makes wax layer temperature be increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h.
Stop compressor.Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize in -0.5~-0.7 atmospheric pressure (table
Pressure), wax layer top air pressure keeps normal pressure；Continue that wax layer temperature is made to be increased to 72.0 DEG C and constant temperature with the heating rate of 2.0 DEG C/h
2.0 hours so that the wax in wax layer is sufficiently separated with oil.Stop vacuum pump, terminates sweating effort.
The outlet of sweating ware is changed to connect thick intermediate products storage tank (I) to receive on wax.Continue to increase circulating water temperature to 90
DEG C, it is taken out on wax with fusing, as thick intermediate products (I).
(A4) it refines
Thick intermediate products (I) through washing, it is clay-filtered be intermediate products (I), it is stand-by after molding.
Intermediate products (I) property: fusing point: 76.3 DEG C, oil content: 7.31%.Intermediate products (I) yield is 13.8%(phase
For raw material slack wax).
B: second segment sweating
This process includes: (B1) preparation, (B2) cooling-thermostatical crystallization, (B3) heating-constant temperature sweating, (B4) essence
The processes such as system.
(B1) preparation
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；The heating function for starting the circulatory system, makes recirculated water be warming up to 80 DEG C.
Water is padded below sweating ware ware plate.The sealing system on sweating ware top is installed and is connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump.Starting compressor simultaneously keeps pressurized buffer pressure inside the tank steady
It is scheduled on 3.6~3.8 atmospheric pressure (gauge pressure).
With the product (intermediate products (I)) of first segment sweating for raw material, it is heated to after 80 DEG C of fusings at 3.6~3.8 greatly
Sweating ware is added under air pressure (gauge pressure).
(B2) cooling-thermostatical crystallization
Start the circulatory system refrigerating function, with the rate of temperature fall of 2.0 DEG C/h make wax layer temperature drop to 66.0 DEG C so that
Wax layer crystallizes to form solid, and constant temperature 2.0 hours so that wax layer sufficient crystallising.The constant temperature stage is slow by emptying system control pressurization
It rushes pressure inside the tank and normal pressure is reduced to the rate of 4.3~4.6atm/h.Close the refrigerating function of the circulatory system.
(B3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (II) is to receive under wax；Starting compressor is simultaneously kept
Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.3~1.5 atmospheric pressure (gauge pressure), sweating ware ware plate.Starting circulation
System heating function makes wax layer temperature be increased to 70.0 DEG C with the heating rate of 1.5 DEG C/h.
Stop compressor.Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize in -0.5~-0.7 atmospheric pressure (table
Pressure), wax layer top air pressure keeps normal pressure；Continue that wax layer temperature is made to be increased to 74.0 DEG C and constant temperature with the heating rate of 1.5 DEG C/h
4.0 hours so that the wax in wax layer is sufficiently separated with oil.Stop vacuum pump, terminates sweating effort.
The outlet of sweating ware is changed to connection crude product storage tank (I) to receive on wax.Continue increase circulating water temperature to 90 DEG C, with
Fusing is taken out on wax, as crude product (I).
(B4) it refines
Crude product (I) is crystallite wax product (I) after washing, clay-filtered, molding and packaging.
Crystallite wax product (I) property: fusing point: 77.2 DEG C, oil content: 1.37%, needle penetration 18(1/10mm).Meet commodity
80#The associated specifications of microwax primes.The yield of crystallite wax product (I) is 7.1%(relative to raw material slack wax).
Embodiment 2
The present embodiment includes A: first segment sweating and B: second segment sweating two parts.
A: first segment sweating
This process includes: (A1) preparation, (A2) cooling-thermostatical crystallization, (A3) heating-constant temperature sweating, (A4) essence
The processes such as system.
(A1) preparation
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；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.The sealing system on sweating ware top is installed and is connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump；Pressurized buffer tank emptying system and sweating ware lower part are arranged
Port is connected with absorption system respectively, using 5% NaOH solution as absorbing medium.
Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 3.4~3.6 atmospheric pressure (gauge pressure).It grinds and sieves
Separate 100 mesh~200 mesh sodium bicarbonate.
With Daqing crude oil residue slack wax (with embodiment 1) for raw material, it is heated to after 65 DEG C of fusings in 3.4~3.6 atmosphere
The aforementioned sodium bicarbonate powder of incorporation 1.0% under (gauge pressure) is pressed, sweating ware is added after mixing；Keep pressurized buffer tank internal pressure
Power is stablized in 3.4~3.6 atmospheric pressure.
(A2) cooling-thermostatical 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 52.0 DEG C with
Make wax layer crystallize to form solid, and constant temperature 1.0 hours so that wax layer sufficient crystallising.The constant temperature stage is controlled by emptying system and is pressurizeed
It buffers pressure inside the tank and normal pressure is reduced to the rate of 4.0~4.4 atm/h.The gas of constant temperature stage discharge is molten by 5% NaOH
Liquid decomposes the carbon dioxide generated to absorb sodium bicarbonate.Close the refrigerating function of the circulatory system.
(A3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (III) is to receive under wax；Starting compressor is simultaneously kept
Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.3~1.5 atmospheric pressure (gauge pressure), sweating ware ware plate.Starting circulation
System heating function makes wax layer temperature be increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h.Stop compressor.
Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize on -0.5~-0.7 atmospheric pressure (gauge pressure), wax layer
Square air pressure keeps normal pressure；Continue to make with the heating rate of 2.0 DEG C/h wax layer temperature to be increased to 72.0 DEG C and constant temperature 2.0 hours so that
Wax in wax layer is sufficiently separated with oil.The gas being discharged in sweating effort absorbs sodium bicarbonate decomposition by 5% NaOH solution
The carbon dioxide of generation.Stop vacuum pump, terminates sweating effort.
The outlet of sweating ware is changed to connect thick intermediate products storage tank (II) to receive on wax.Continue to increase circulating water temperature to 90
DEG C, it is taken out on wax with fusing, as thick intermediate products (II).
(A4) it refines
Thick intermediate products (II) through washing, it is clay-filtered be intermediate products (II), it is stand-by after molding.
Intermediate products (II) property: fusing point: 76.8 DEG C, oil content: 5.15%.Intermediate products (II) yield is 16.2%
(relative to raw material slack wax).
B: second segment sweating
This process includes: (B1) preparation, (B2) cooling-thermostatical crystallization, (B3) heating-constant temperature sweating, (B4) essence
The processes such as system.
(B1) preparation
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；The heating function for starting the circulatory system, makes recirculated water be warming up to 80 DEG C.Water is padded below sweating ware ware plate.
The sealing system on sweating ware top is installed and is connected with pressurized buffer tank and compressor；It is installed in sweating ware lower part
Pressure-reducing cushioning tank simultaneously connects vacuum pump；Pressurized buffer tank emptying system and sweating ware lower exhaust port are connected with absorption system respectively
It connects, using 5% NaOH solution as absorbing medium.
Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 3.6~3.8 atmospheric pressure (gauge pressure).It grinds and sieves
Separate 100 mesh~200 mesh sodium bicarbonate.
With the product (intermediate products (II)) of first segment sweating for raw material, it is heated to after 80 DEG C of fusings at 3.6~3.8 greatly
The aforementioned sodium bicarbonate powder of incorporation 1.4% under air pressure (gauge pressure), is added sweating ware after mixing；It keeps in pressurized buffer tank
Pressure is stablized in 3.6~3.8 atmospheric pressure.
(B2) cooling-thermostatical crystallization
Start the circulatory system refrigerating function, with the rate of temperature fall of 2.0 DEG C/h make wax layer temperature drop to 66.0 DEG C so that
Wax layer crystallizes to form solid, and constant temperature 2.0 hours so that wax layer sufficient crystallising.The constant temperature stage is slow by emptying system control pressurization
It rushes pressure inside the tank and normal pressure is reduced to the rate of 4.3~4.6atm/h.The gas of constant temperature stage discharge passes through 5% NaOH solution
The carbon dioxide generated is decomposed to absorb sodium bicarbonate.Close the refrigerating function of the circulatory system.
(B3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (IV) is to receive under wax；Starting compressor is simultaneously kept
Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.3~1.5 atmospheric pressure (gauge pressure), sweating ware ware plate.
Sweating ware outlet connection intermediate storage tank (II) is to receive under wax.Start circulation system function, with 1.5 DEG C/h's
Heating rate makes wax layer temperature be increased to 70.0 DEG C.Stop compressor.
Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize on -0.5~-0.7 atmospheric pressure (gauge pressure), wax layer
Square air pressure keeps normal pressure；Continue to make with the heating rate of 1.5 DEG C/h wax layer temperature to be increased to 74.0 DEG C and constant temperature 4.0 hours so that
Wax in wax layer is sufficiently separated with oil.The gas being discharged in sweating effort absorbs sodium bicarbonate decomposition by 5% NaOH solution
The carbon dioxide of generation.
Stop vacuum pump, terminates sweating effort.The outlet of sweating ware is changed to connection crude product storage tank (II) to receive on wax.Continue
Circulating water temperature is increased to 90 DEG C, is taken out on wax with fusing, as crude product (II).
(B4) it refines
Crude product (II) is crystallite wax product (II) after washing, clay-filtered, molding and packaging.
Crystallite wax product (II) property: fusing point: 77.6 DEG C, oil content: 1.15%.Needle penetration 17(1/10mm).Meet quotient
The associated specifications of product 80# microwax primes.The yield of crystallite wax product (II) is 10.6%(relative to raw material slack wax).
The method that can be seen that present invention production microwax by embodiment 1-2 is set by increasing pressurization and/or vacuum
The improvement to sweatbox such as apply；It is decomposed using inorganic salts and forms short space in wax layer and forced in heating sweating effort
Improvement of the air-flow by wax layer etc. to sweating process；It enhances the separating effect of wax and oil and accelerates separating rate, to make
Sweating de-oiling technique can produce crystallite wax product.
Claims (24)
1. a kind of method for producing microwax, including the following contents:
A, first segment sweating, comprising:
(A1) charge: using oil content less than 30%, melting range be 55 DEG C~80 DEG C slack wax as raw material, heating fusing after pressing
The decomposable inorganic salt powder for generating gas is mixed under the conditions of power, is packed into sweatbox；
(A2) 8 DEG C~20 DEG C of raw material fusing point or less pre- cooling-thermostatical crystallization: is cooled to 1.0 DEG C/h~4.0 DEG C/h rate
Determine temperature, and constant temperature is for a period of time；
(A3) heating-constant temperature sweating: with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；Wax layer reaches predetermined temperature and one section of constant temperature
Stop sweating after time；Wax layer is forced air flow through in sweating effort；
(A4) it refines: being intermediate products after refining on wax；With
B, second segment sweating, comprising:
(B1) charge: the intermediate products obtained using first segment sweating is raw materials, and incorporation can divide under stress after heating fusing
Solution generates the inorganic salt powder of gas, is packed into sweatbox；
(B2) 8 DEG C~20 DEG C of intermediate products fusing point or less cooling-thermostatical crystallization: are cooled to 1.0 DEG C/h~4.0 DEG C/h rate
Predetermined temperature, and constant temperature is for a period of time；
(B3) heating-constant temperature sweating: and then with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；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；
(B4) it refines: being purpose product after being refined, being formed on wax.
2. according to the method for claim 1, which is characterized in that the inorganic salt powder decomposes release in sweating effort
Gas out, and itself and decomposition product are soluble easily in water.
3. according to the method for claim 2, which is characterized in that the inorganic salts are selected from ammonium salt, carbonate, bicarbonate
One or more of.
4. according to the method for claim 1, which is characterized in that the granularity of the inorganic salt powder is 50~500 mesh.
5. according to the method for claim 2, which is characterized in that the additional amount of the inorganic salt powder accounts for sweating raw material weight
The 0.1%~10.0% of amount.
6. according to the method for claim 2, which is characterized in that in step (A1), the charging process and (A2), (B2) of (B1)
Apply air pressure above wax layer in the temperature-fall period of crystallization, the gas generated to inhibit inorganic salts to decompose escapes wax layer.
7. according to the method for claim 6, which is characterized in that the air pressure is 0.5~15.0 atmosphere of gauge
Pressure.
8. according to the method for claim 1, which is characterized in that pressure air-flow described in step (A3) and step (B3) is logical
It crosses wax layer and uses and 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 real
Existing, the pressure difference is 0.1~5.0 atmospheric pressure.
9. according to the method for claim 1, which is characterized in that the rate of cooling described in step (A2) and step (B2) is
1.5 DEG C/h~2.5 DEG C/h.
10. according to the method for claim 1, which is characterized in that the predetermined temperature of cooling described in step (A2) is lower than original
10 DEG C~15 DEG C of slack wax fusing point of material；And the predetermined temperature of cooling described in step (B2) is lower than intermediate products fusing point 10 DEG C~15
℃。
11. according to the method for claim 1, which is characterized in that the constant temperature described in step (A2) and step (B2) when
Between be 0.1~3.0 hour.
12. according to the method for claim 11, which is characterized in that the constant temperature described in step (A2) and step (B2) it is same
When gradually decrease pressure to normal pressure.
13. according to the method for claim 1, which is characterized in that the rate of heating described in step (A3) and step (B3)
For 1.0 DEG C/h~2.0 DEG C/h.
14. according to the method for claim 1, which is characterized in that the predetermined temperature of heating described in step (A3) be lower than
2 DEG C~10 DEG C of the fusing point of intermediate products；The predetermined temperature of heating described in step (B3) be lower than purpose product 2 DEG C of fusing point~
10℃。
15. 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.
16. according to the method for claim 8, which is characterized in that the wax layer that forces air flow through uses in wax layer
Fang Zengjia air pressure is realized, applies the gauge of 0.2~2.0 atmospheric pressure above wax layer, and remains normal pressure below wax layer.
17. according to the method for claim 8, 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 table of -0.2~-1.0 atmospheric pressure is maintained below wax layer
Pressure pressure.
18. according to the method for claim 1, which is characterized in that constant temperature time described in step (A3) and step (B3)
It is 0.1~5 hour.
19. according to the method for claim 1, which is characterized in that use liquid in the thermostatic process and sweating effort of crystallization
Body absorption pattern absorbs inorganic salts and decomposes the gas generated；Unreacted inorganic salts are removed using water-washing method in subtractive process
And decomposition product.
20. according to the method for claim 1, which is characterized in that the sweatbox is sweating ware.
21. according to the method for claim 5, which is characterized in that the additional amount of the inorganic salt powder accounts for sweating raw material
The 0.2%~3.0% of weight.
22. according to the method for claim 7, which is characterized in that the air pressure is 1.0~8.0 atmosphere of gauge
Pressure.
23. according to the method for claim 8, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.
24. according to the method for claim 11, which is characterized in that the constant temperature described in step (A2) and step (B2) when
Between be 1.0~3.0 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510928608.5A CN106883886B (en) | 2015-12-15 | 2015-12-15 | A method of producing microwax |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510928608.5A CN106883886B (en) | 2015-12-15 | 2015-12-15 | A method of producing microwax |
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| CN106883886B true CN106883886B (en) | 2019-01-25 |
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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 CN201510928608.5A patent/CN106883886B/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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| Publication number | Publication date |
|---|---|
| CN106883886A (en) | 2017-06-23 |
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