CN106883879B - A method of producing paraffin - Google Patents

Abstract

The invention discloses a kind of 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, 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, to improve purpose product yield, and high melting point paraffin can be produced.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

A method of producing paraffin

Technical field

The invention belongs to pertroleum wax production technical fields, more particularly to a kind of method for producing paraffin.

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.Paraffin be in crude oil lube cut through dewaxing, de-oiling, purification and molding Production, typically contain C₂₀~C₅₀The components such as n-alkane, isoparaffin and a small amount of 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 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.

To common sweating de-oiling technique, in sweating effort although wax and oily two class components are respectively at solid and liquid State, but be also difficult to be kept completely separate.To make the oil content of final products meet the requirements, generallys use and extend sweating sessions and improve The method of sweating final temperature.Extending sweating sessions will lead to production cycle extension；Improving sweating final temperature will lead to product Yield decline.

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 of the fusing point at 70 DEG C or so.Have experiments have shown that, common sweating de-oiling technique production fusing point is at 70 DEG C or so High melting point paraffin when, even if using sweating sessions and the method that improves sweating final temperature, containing on sweating later period wax is extended Oil mass is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, so common sweating de-oiling technique is not suitable for Production fusing point meets semi-refined or full refining product standard high melting point paraffin, especially oil-containing figureofmerit not at 70 DEG C or so It is able to satisfy the technical requirements of relevant criterion.

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 cannot still produce and meet semi-refined or full refining product standard high melting point paraffin.

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 the efficiency for improving sweating method, and use The demand that sweating de-oiling technique produces high melting point paraffin is also 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 paraffin, is specifically filled using sweating It sets, on the basis of common sweating process, preferably incorporation can decompose generation gas under stress after raw material heating fusing Inorganic salt powder；And the oil of liquid is carried out to force separation wax and oil, enhancing by wax layer using air-flow in sweating effort Separating effect simultaneously accelerates separating rate.Inorganic salts are absorbed in the thermostatic process and sweating effort of crystallization decomposes the nocuousness generated Gas.Unreacted inorganic salts and decomposition product are removed using water-washing method.The method of the present invention improves the yield of purpose product And shorten the production cycle, moreover it can be used to produce high melting point paraffin product；And 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 method producing paraffin of the invention, including the following contents:

(1) charge: using oil content less than 30%, fusing point be 45 DEG C~70 DEG C slack wax as raw material, heating fusing (usually plus More than heat to fusing point 1 DEG C~5 DEG C) it is packed into sweatbox afterwards；

(2) it crystallizes: being cooled to 8 DEG C~20 DEG C of raw material fusing point or less of predetermined temperature with 1.0 DEG C/h~4.0 DEG C/h rate Degree, and constant temperature is for a period of time；

(3) sweating: with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；Wax layer is forced air flow through in temperature-rise period；Wax Layer stops sweating after reaching predetermined temperature；

(4) it refines: being purpose product after being refined, being formed on wax.

In method of the invention, less than 30%, melting range is generally the oil content (in mass) of the raw material slack wax 45 DEG C~70 DEG C.Slack wax raw material can be dewaxed slack wax obtained for vacuum 1st side cut, second line of distillation, the line that subtracts three or the line distillate that subtracts four.

Process of the present invention it is preferred incorporation can decompose the nothing for generating gas under stress after raw material heating fusing Machine salt powder, the pressure (gauge pressure) are generally 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.It is described Inorganic salt powder can slowly be decomposed in sweating effort and release gas and itself and decomposition product is soluble easily in water, can be with It is one or more of ammonium salt, carbonate, bicarbonate.The granularity of the inorganic salt powder is 50~500 mesh, additional amount Account for 0.1%~10.0%(weight of sweating raw material), preferred ratio is 0.2%~3.0%.Thermostatic process and sweating in crystallization Inorganic salts are absorbed in journey decomposes (nocuousness) gas generated.Unreacted inorganic salts are removed using water-washing method in subtractive process And decomposition product.

In method of the invention, the sweatbox is generally sweating ware, and added above dismountable close in wax layer Envelope system and pressurizing device are generated with inhibiting inorganic salts to decompose in the temperature-fall period of the charging of step (1) and step (2) crystallization Gas escape wax layer.The pressure (gauge pressure) is 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.

In method of the invention, the sweatbox is sweating ware, and wax layer pressurizing 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 0.1~5.0 atmospheric pressure, Preferably 0.2~2.0 atmospheric pressure, to force air flow through wax layer.

In method of the invention, the rate of temperature fall of the raw material wax layer crystallization process preferably 1.5 DEG C/h~3.0 DEG C/h.Institute State 10 DEG C~15 DEG C of cooling final temperature preferred raw material slack wax fusing point or less.

In method of the invention, the time in the constant temperature stage of the raw material wax layer crystallization process is 0.1~3.0 h, preferably 1.0~3.0 h, while pressure is gradually decreased to normal pressure.The reduction speed of the pressure is generally 0.01~150 atm/h, excellent It is selected as 0.2~80 atm/h, more preferably 0.3~10 atm/h.

In method of the invention, the heating rate of the raw material wax layer sweating effort preferably 1.0 DEG C/h~2.0 DEG C/h.Institute The predetermined temperature for stating heating is lower than 2 DEG C~10 DEG C of fusing point of purpose product.

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.

It is described to force air flow through wax layer and implement in sweating effort any stage in method of the invention, preferably Implement at sweating initial stage.

In method of the invention, the wax layer that forces air flow through is utilized in what increase air pressure above wax layer was realized, The pressure of 0.2~2.0 atmospheric pressure (gauge pressure) can such as be applied above wax layer, and remain normal pressure below wax layer.

In method of the invention, the wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized, Normal pressure can be such as kept above wax layer, and the pressure of -0.2~-1.0 atmospheric pressure (gauge pressure) is maintained below wax layer.

In method of the invention, the sweatbox can also connect gas absorption system, in the constant temperature mistake of crystallization Inorganic salts are absorbed in journey and sweating effort decomposes the pernicious gas generated.Absorption system uses liquid absorption mode.

Sweating de-oiling method is to be separated using wax and oil property with different melting points to produce paraffin, but in sweating 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, and wax and oil are difficult to be kept completely separate in the common sweating effort of gravity natural separation.For fusing point at 70 DEG C The high melting point paraffin of left and right causes crystals upon crystallization structure more fine and compact since chemical composition is more complicated, is commonly sending out Wax and oil are more difficult to separate during sweat, therefore common sweating de-oiling technique cannot produce fusing point and meet half essence at 70 DEG C or so The high melting point paraffin of refining or full refining product standard.

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 is difficult to be kept completely separate reason by the further investigation to common sweating effort for wax and oil, The separation for forcing wax and oil by the method that wax layer carries out fluid oil using air-flow in sweating effort, enhances separating effect And accelerate separating rate.Incorporation is decomposable under stress further preferably after raw material heating fusing simultaneously generates the inorganic of gas Salt powder, these substances slowly settle in the wax layer of liquid due to granularity is smaller.It keeps being cooled to raw material under pressure condition 10 DEG C~15 DEG C below fusing point, and constant temperature 0.1h~3.0h is so that wax layer crystallization is more abundant；It is gradually dropped in thermostatic process simultaneously Low-pressure is 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-like State, inorganic salts slowly decompose the gas released during this, micro-bubble can be formed in wax layer, these micro-bubbles are formed Space be easy to be formed several tiny channels in sweating effort in wax layer, to be conducive to row oily in sweating effort Out.The oil for carrying out liquid by wax layer using air-flow in sweating effort simultaneously enhances separation to force separation wax and oil Effect simultaneously accelerates separating rate.

The invention has the advantages that by using air-flow to force in sweating effort by the method that wax layer carries out fluid oil The separation of wax and oil, enhances separating effect and accelerates separating rate；The gas generated is decomposed in wax using inorganic salts simultaneously Short space is formed in layer, the quick discharge of oil is also beneficial to, to reach raising wax product yield and shorten the production cycle Purpose, and high melting point paraffin can be produced.Method of the invention is low with plant investment, production process is simple and operating cost The advantages that with low, safety, energy conservation and solvent-free pollution environment, so that the method for this solvent-free production paraffin of sweating de-oiling is more Highly effective.

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；In sweating effort, start compressor with formed above just in wax layer Pressure, and/or starting vacuum pump is in wax layer negative pressure formed below, to force air flow through wax layer；Wax layer temperature reaches default Stop sweating after temperature；It is purpose product after washing, clay-filtered, molding, packaging on wax.It can send out through these means In the case that the time in sweat stage reduces 30%~50%, purpose product yield is set to improve 5~15 percentages, and Gao Rong can be produced Point paraffin.

Illustrate the method for present invention production paraffin below by way of specific embodiment.

Comparative example 1

This comparative example includes: the processes such as (1) preparation, (2) crystallization, (3) sweating, (4) purification.

(1) 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 53 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.Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 3.0~3.2 atmospheric pressure (gauge pressure).

With (50.6 DEG C of fusing point, oil content 21.4%) of Daqing crude oil second line of distillation slack wax for raw material, after being heated to 53 DEG C of fusings Sweating ware is added under 3.0~3.2 atmospheric pressure (gauge pressure).

(2) it crystallizes

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, and constant temperature 1.0h is so that wax layer crystallization is more abundant.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 3.6~3.8atm/h.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) is to receive under wax；Start compressor and keeps adding Pressure buffering pressure inside the tank is stablized keeps normal pressure below 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware ware plate；Start cyclic system The heating function of system makes wax layer temperature be increased to 43.0 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 on -0.5~-0.7 atmospheric pressure (gauge pressure), wax layer Square air pressure keeps normal pressure；Continue to make wax layer temperature be increased to 49.0 DEG C with the heating rate of 1.5 DEG C/h.Stop vacuum pump, terminates hair Sweat process (the sweating effort time is 8 hours).

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).

(4) it refines

Crude product (I) is purpose product after washing, clay-filtered, molding, packaging.

Product (I) property: 54.3 DEG C of fusing point, oil content 1.47% meet commodity 54^#The relevant technical requirements of semi-refined wax. 54^#Semi-refined wax product yield is 43.7%(relative raw material slack wax).

Comparative example 2

This comparative example includes: the processes such as (1) preparation, (2) crystallization, (3) sweating, (4) purification.

(1) 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 61 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 the Daqing crude oil line slack wax that subtracts four (initial boiling point: 410 DEG C, 90% distillate a little: 520 DEG C；58.5 DEG C of fusing point；Oil content 26.9%) it is raw material, sweating ware is added under 3.4~3.6 atmospheric pressure (gauge pressure) after being heated to 61 DEG C of fusings.

(2) it crystallizes

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, and constant temperature 1.0h is so that wax layer crystallization is more abundant.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 4.0~4.3atm/h.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) is to receive under wax；Starting compressor is simultaneously kept Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware ware plate.Starting circulation The heating function of system 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 wax layer temperature be increased to 70.0 DEG C with the heating rate of 2.0 DEG C/h.Stop vacuum pump, terminates hair Sweat process.

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).

(4) it refines

Crude product (II) is purpose product after washing, clay-filtered, molding, packaging.

Product (II) property: fusing point: 72.3 DEG C, oil content: 0.78%.Meet commodity 72^#The related skill of fully refined paraffin wax Art requirement.72^#Fully refined paraffin wax product yield is 12.3%(relative to slack wax raw material).

Embodiment 1

The present embodiment includes: the processes such as (1) preparation, (2) crystallization, (3) sweating, (4) purification.

(1) 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 53 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, respectively with 5% H₂SO₄Solution and 5% NaOH solution as absorbing medium.Starting pressure Contracting machine simultaneously keeps pressurized buffer pressure inside the tank to stablize in 3.0~3.2 atmospheric pressure (gauge pressure).

It grinds and screens out 100 mesh~200 mesh ammonium hydrogen carbonate.It is with Daqing crude oil second line of distillation slack wax (with comparative example 1) Raw material is heated to the aforementioned ammonium hydrogen carbonate powder of the incorporation 0.8% under 3.0~3.2 atmospheric pressure (gauge pressure) after 53 DEG C of fusings, mixes Sweating ware is added after closing uniformly；Pressurized buffer pressure inside the tank is kept to stablize in 3.0~3.2 atmospheric pressure.

(2) it crystallizes

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, and constant temperature 1.0h is so that wax layer crystallization is more abundant.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 3.6~3.8atm/h.The constant temperature stage gas of discharge passes sequentially through 5% H₂SO₄Solution and 5% NaOH solution with absorb ammonium bicarbonate breaks down generation ammonia and carbon dioxide.Close the system of the circulatory system Cold function.

(3) 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 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware ware plate.Starting circulation The heating function of system makes wax layer temperature be increased to 43.0 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 on -0.5~-0.7 atmospheric pressure (gauge pressure), wax layer Square air pressure keeps normal pressure；Continue to make wax layer temperature be increased to 49.0 DEG C with the heating rate of 1.5 DEG C/h.It is discharged in sweating effort Gas passes sequentially through 5% H₂SO₄Solution and 5% NaOH solution with absorb ammonium bicarbonate breaks down generation ammonia and carbon dioxide.

Stop vacuum pump, terminate sweating effort (the sweating effort time is 8 hours).The outlet of sweating ware is changed to connection crude product storage Tank (III)；Continuation heat cycles water is warming up to 70 DEG C and is taken out on wax with fusing, as crude product (III).

(4) it refines

Crude product (III) is purpose product after washing, clay-filtered, molding, packaging.

Product (III) property: 54.2 DEG C of fusing point, oil content 1.23% meet commodity 54^#The relevant technical requirements of semi-refined wax. 54^#Semi-refined wax product yield is 48.5%(relative raw material slack wax).

Embodiment 2

The present embodiment includes: the processes such as (1) preparation, (2) crystallization, (3) sweating, (4) purification.

(1) 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 61 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 and keep pressurized buffer pressure inside the tank stablize 3.4~ 3.6 atmospheric pressure (gauge pressure).

It grinds and screens out 100 mesh~200 mesh sodium bicarbonate.Subtracting four with Daqing crude oil, line slack wax (with comparative example 2) is Raw material is heated to the aforementioned sodium bicarbonate powder of the incorporation 1.5% under 3.4~3.6 atmospheric pressure (gauge pressure) after 61 DEG C of fusings, mixes Sweating ware is added after closing uniformly；Pressurized buffer pressure inside the tank is kept to stablize in 3.4~3.6 atmospheric pressure.

(2) it crystallizes

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, and constant temperature 1.0h is so that wax layer crystallization is more abundant.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 4.0~4.3 atm/h.The gas being discharged in thermostatic process passes through 5% NaOH Solution decomposes the carbon dioxide generated to absorb sodium bicarbonate.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) is to receive under wax；Starting compressor is simultaneously kept Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware ware plate.

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.Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize above -0.5~-0.7 atmospheric pressure (gauge pressure), wax layer Air pressure keeps normal pressure.Continue to make wax layer temperature be increased to 70.0 DEG C with the heating rate of 2.0 DEG C/h.The gas being discharged in sweating effort Body is absorbed sodium bicarbonate by 5% NaOH solution and decomposes the carbon dioxide generated.

Stop vacuum pump, terminates sweating effort.The outlet of sweating ware is changed to connection crude product storage tank (IV)；Continue heat cycles water It is warming up to 80 DEG C to take out on wax with fusing, as crude product (IV).

(4) it refines

Crude product (IV) is purpose product after washing, clay-filtered, molding, packaging.

Product (IV) property: fusing point: 72.5 DEG C, oil content: 0.46%.Meet commodity 72^#The related skill of fully refined paraffin wax Art requirement.72^#Fully refined paraffin wax product yield is 15.2%(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 (sweating effort time be 14 hours).It is taken out on wax after sweating, is after clay-filtered, molding Purpose product.

Product property: 55.6 DEG C of fusing point, oil content 1.75% meet commodity 54^#The relevant technical requirements of semi-refined wax.54^#Half Refining wax product yield is 37.4%.

By comparing the method that example and embodiment can be seen that present invention production paraffin, air-flow is used in sweating effort The separation that wax and oil are forced by the method that wax layer carries out fluid oil, enhances separating effect and accelerates separating rate；Benefit The quick discharge for forming short space in wax layer and being more favorable to oil is decomposed with inorganic salts, to improve purpose wax product receipts Rate (embodiment 1 and comparative example 1 increase 4.8 percentage points, and embodiment 1 increases 11.1 percentage points compared with comparative example 3). And by embodiment 2 as can be seen that method of the invention can produce high melting point paraffin of the fusing point at 70 DEG C or more.

Claims (21)

1. a kind of method for producing paraffin, including the following contents:

(1) charge: using oil content less than 30%, fusing point be 45 DEG C~70 DEG C slack wax as raw material, heating fusing after mix under stress Enter and can decompose the inorganic salt powder for generating gas, is packed into sweatbox；

(2) it crystallizes: being cooled to 8 DEG C~20 DEG C of raw material fusing point or less of predetermined temperature with 1.0 DEG C/h~4.0 DEG C/h rate, and Constant temperature is for a period of time；

(3) sweating: with the heating of 0.5 DEG C/h~3.0 DEG C/h rate；Wax layer is forced air flow through in temperature-rise period；Wax layer reaches Stop sweating after to predetermined temperature；The predetermined temperature is lower than 2 DEG C~10 DEG C of purpose product fusing point；

(4) 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 salt powder is selected from ammonium salt, carbonate, carbonic acid One or more of hydrogen salt.

4. according to the method for claim 3, which is characterized in that the granularity of the inorganic salt powder is 50~500 mesh.

5. according to the method for claim 1, 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 1, which is characterized in that in the charging process of step (1) and the cooling of step (2) Apply air pressure in journey above wax layer, the gas generated to inhibit inorganic salts to decompose escapes wax layer.

7. according to the method for claim 1, which is characterized in that the pressure is 0.5~15.0 atmosphere of gauge Pressure.

8. according to the method for claim 1, which is characterized in that force air flow through wax layer use described in step (3) 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 Power 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 (2) be 2.0 DEG C/h~ 3.0℃/h。

10. according to the method for claim 1, which is characterized in that predetermined temperature described in step (2) be raw material fusing point with Lower 10 DEG C~15 DEG C.

11. according to the method for claim 1, which is characterized in that the time of constant temperature described in step (2) is 0.1~3.0h.

12. according to the method for claim 11, which is characterized in that gradually decrease pressure while constant temperature described in step (2) Power is to normal pressure.

13. according to the method for claim 1, which is characterized in that the rate of heating described in step (3) 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 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.

16. 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.

17. 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.

18. 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.

19. according to the method for claim 4, which is characterized in that the pressure is 1.0~8.0 atmosphere of gauge Pressure.

20. according to the method for claim 8, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.

21. according to the method for claim 11, which is characterized in that the time of constant temperature described in step (2) be 1.0~ 3.0h。