CN105733679A - Sweating and soap wax and paraffin producing method - Google Patents
Sweating and soap wax and paraffin producing method Download PDFInfo
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- CN105733679A CN105733679A CN201510928645.6A CN201510928645A CN105733679A CN 105733679 A CN105733679 A CN 105733679A CN 201510928645 A CN201510928645 A CN 201510928645A CN 105733679 A CN105733679 A CN 105733679A
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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
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
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Abstract
The invention discloses a sweating and soap wax and paraffin producing method. In the method, a sweating apparatus is employed, and on the basis of a common sweating and deoiling process, a low-boiling-point liquid is added to a raw material, and wax and oil are forcedly separated by carrying liquid-phase oil through a wax layer through air flow during a temperature-increased sweating process, thereby improving separation effect and accelerating separation, so that yield of target products is increased and production period is reduced, and also paraffin being about 70 DEG C in melting point can be produced. The method is low in investment, is simple in production process, is low in operation cost and is free of solvent pollution.
Description
Technical field
The invention belongs to pertroleum wax production technical field, particularly relate to a kind of diaphoresis and the method producing soap wax and paraffin.
Background technology
Pertroleum wax is the general name of all kinds of wax products that crude oil prepares after refining processing from wax-containing distillate, including liquid paraffin, soap wax, paraffin and microwax.Soap wax and paraffin are that in crude oil, lube cut produces through steps such as dewaxing, removing oil, refining and molding, typically contain C20～C30N-alkane, the component such as a small amount of isoparaffin and cycloalkane, usual fusing point is 40 DEG C～74 DEG C.
Dewaxing is the process preparing the slack wax that oil content is about 10～30% with lube cut for raw material, and dewaxing technique mainly has squeezing dewaxing and solvent dewaxing.Removing oil is the process of the scale wax preparing oil content less than 2% with slack wax for raw material, and removing oil technique mainly has diaphoresis removing oil and solvent deoiling.Scale wax, then through clay-filtered or hydrofinishing and molding, packaging and other steps, can obtain commodity oil wax.
Solvent deoiling method be according to wax with oil in selective solvent (acetone, benzene and toluene mixture；Or acetone, toluene；Or butanone, toluene) in the character of different solubility wax is easily separated with oil.Solvent deoiling technique have production process continuously, wax yield is high, finished product wax oil content can very low, the advantage such as production cost is relatively low, be the main flow removing oil technique of current large-scale production petroleum paraffin product.But solvent deoiling explained hereafter equipment investment is big；Needing in production process to use solvent in a large number, recycling design needs to consume substantial amounts of energy；Containing benzene homologues in solvent, environment can be impacted；Solvent is inflammable, it is easy to cause production accident.
Diaphoresis de-oiling method is that the character utilizing wax different with oil fusing point is easily separated.In pertroleum wax, the molecular weight of various components and structure difference all can make its fusing point different.When being all n-alkane structure, the fusing point of the n-alkane that molecular weight is bigger is higher, and the fusing point of the n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will lower than n-alkane, and isomery degree more high-melting-point is more low, even at normal temperatures just in liquid condition, and namely usually said oil.Diaphoresis de-oiling method does not use solvent in process of production, and has only to the temperature more than by heating raw materials to fusing point in production process.
Common diaphoresis degreasing process mainly comprises the steps that (1) preparation: pad water, is full of sweatbox ware plate lower space with water；(2) charging: load sweatbox when heating raw materials is in a liquid state to fusing point；(3) decrease temperature crystalline: raw material is progressively cooled to below its fusing point 10～20 DEG C with the rate of temperature fall being not more than 4 DEG C/h.In cooling procedure, various components are pressed the fusing point crystallization successively of order from high to low and are formed solid；(4) intensification diaphoresis: after wax layer temperature reaches the cooling final temperature preset, bleed off pad water；Raw material is heated to lentamente default diaphoresis final temperature again.In intensification sweating effort, various components are successively fused into liquid by fusing point order from low to high and flow out (under wax), and wax layer residue (on wax) finally obtained is exactly the wax of high-melting-point, low oil-containing；(5) thick product is collected: intensification sweating effort terminates follow-up high-temperature of continuing rising, to melt on taking-up wax, is thick product；(6) product purification, molding, packaging: subtractive process generally adopts clay-filtered: will thick product melt after be warming up to predetermined temperature, add hargil and constant temperature stirring filtered to the scheduled time；Then through molding, pack product for the purpose of namely.
To common diaphoresis de-oiling method, although wax and oily two class components are respectively at solid and liquid condition in intensification sweating effort, but it also is difficult to be kept completely separate.For making the oil content of final products meet the requirements, generally adopt the method extending sweating sessions and improving diaphoresis final temperature.Extend sweating sessions and can cause that the production cycle is long；Improving diaphoresis final temperature can make part wax remove with oil, causes that product yield declines.
Common diaphoresis de-oiling method can produce fusing point at the soap wax of 40 DEG C～60 DEG C and low melt point paraffin.Compared with solvent deoiling method, diaphoresis removing oil is intermittently operated, and product yield is relatively low, the production cycle is longer, but diaphoresis de-oiling method has the advantages such as small investment, production process is simple, operating cost is low, still has part producer using the method to produce soap wax and low melt point paraffin product at present.
For many years, diaphoresis de-oiling method obtains some development at production equipment and process aspect, such as CN89214332(vertical 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(Efficient paraffin sweatbox), CN201320127680.4(tubular type paraffin deoiler) etc., diaphoresis removing oil production equipment has done improvement；CN91206202(high-efficient sweat pot for paraffin wax) in diaphoresis removing oil technique, done improvement.But these methods still suffer from the shortcomings such as product yield is relatively low, the production cycle is longer.
Diaphoresis de-oiling method is to be currently known the unique solvent-free de-oiling method for industrial-scale production soap wax and low melt point paraffin product, is increasingly subject to the concern of people in today of promotion environmental protection, low-carbon energy-saving.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of diaphoresis and the method producing soap wax and paraffin, specifically adopts sweatbox, on the basis of common diaphoresis removing oil technique, preferably under stress mixes low-boiling point liquid after heating raw materials fusing；And utilize air-flow to carry out the oil of liquid to force to separate wax and oil by wax layer in intensification sweating effort, enhance separating effect and accelerate separating rate.Constant temperature and sweating effort reclaim low-boiling point liquid.The inventive method not only increases the yield of purpose product and shortens the production cycle, and can produce the high melting point paraffin that fusing point is at about 70 DEG C, has the advantages such as plant investment is low, production process is simple and operating cost is low, solvent-free pollution simultaneously.
A kind of diaphoresis of the present invention and the method for production soap wax and paraffin, including herein below:
(1) in sweatbox, water is padded；
(2) with the oil content slack wax less than 30% for raw material, heating to fusing point 3 DEG C～8 DEG C, raw material loads sweatbox after all melting；
(3) predetermined temperature of below slack wax fusing point 8 DEG C～20 DEG C constant temperature a period of time it is cooled to the speed of 1.0 DEG C/h～4.0 DEG C/h；
(4) the pad water in sweatbox is discharged, then with the ramp of 0.5 DEG C/h～3.0 DEG C/h；Temperature-rise period forces air flow through wax layer；Wax layer stops diaphoresis after reaching predetermined temperature；
(5) collect on wax；
(6) on wax after refining, molding namely for the purpose of product.
In the method for the present invention, the oil content (in mass) of described raw material slack wax is less than 30%, and its melting range is generally 25 DEG C～70 DEG C.Raw material slack wax can be atmosphere 3rd side cut, normal four lines, vacuum 1st side cut, second line of distillation, the line that subtracts three, the line distillate that subtracts four is through the prepared slack wax that dewaxes.
Process of the present invention it is preferred under stress mix low-boiling point liquid after heating raw materials melts.Described pressure (gauge pressure) is generally 0.5～20.0 atmospheric pressure, it is preferred to 1.0～10.0 atmospheric pressure.Described low-boiling point liquid is Organic substance, and itself and raw material have good intersolubility, and boiling point at ambient pressure is lower than the predetermined temperature cooled, and boiling point under high pressure is higher than the maximum temperature of reinforced process.Described low-boiling point liquid can be one or more in the Organic substance that the boiling points such as alkane, alkene, alkynes, alkadienes, alcohol, aldehyde, ether, ester, halogenated hydrocarbons are suitable, it is preferred to alkane, alcohol, ester etc. and raw material have good intersolubility, without special odor and the material that has no side effect.The addition of described low-boiling point liquid accounts for 0.1%～5.0%(weight of raw material slack wax), it is preferred that ratio is 0.3%～2.0%.Constant temperature and sweating effort reclaim low-boiling point liquid.
In the method for the present invention, described sweatbox is generally diaphoresis ware, and at wax layer dismountable sealing system added above and pressue device, to ensure to be in liquid condition reinforced with maintenance low-boiling point liquid in cooling procedure.Described pressure (gauge pressure) is 0.5～20.0 atmospheric pressure, it is preferred to 1.0～10.0 atmospheric pressure.
In the method for the present invention, described sweatbox is generally diaphoresis ware, and the angle between diaphoresis ware ware plate and baffle plate is 90 °～170 ° (not including 90 °), it is preferred to 120 °～150 °.
In the method for the present invention, described diaphoresis ware is at wax layer pressue device added above and/or increases vacuum equipment below wax layer.The described wax layer that forces air flow through adopts increase pressure (air pressure) and/or reduction pressure (air pressure) below wax layer above wax layer, makes wax layer upper and lower form pressure differential and realizes.Described pressure differential is generally 0.1～5.0 atmospheric pressure, it is preferred to 0.2～2.0 atmospheric pressure, to force air flow through wax layer.
In the method for the present invention, the rate of temperature fall of described paraffin layer preferably 2.0 DEG C/h～3.0 DEG C/h.
In the method for the present invention, below the cooling final temperature preferred feedstock slack wax fusing point of described paraffin layer 10 DEG C～15 DEG C.
In the method for the present invention, constant temperature 0～3.0h after the cooling termination of described paraffin layer, it is preferable that 0.1～3.0h, it is most preferred that 1.0～3.0h, reduce pressure gradually to normal pressure simultaneously.
In the method for the present invention, the heating rate of described paraffin layer preferably 1.0 DEG C/h～2.0 DEG C/h.The predetermined temperature of described intensification is the fusing point 2 DEG C～10 DEG C lower than purpose product.
In the method for the present invention, the programming rate of said wax layer and cooling rate, it is possible to be controlled by air bath, water-bath, oil bath or other feasible modes.When adopting water-bath or oil bath mode to control wax layer heating rate and rate of temperature fall, chuck can be increased outside diaphoresis ware, chuck is connected with removable coil pipe and blood circulation, and blood circulation has programmed cooling/heating function, and blood circulation adds water or heat conduction wet goods material as circulatory mediator；By coil pipe submergence and be fixed in wax layer after charging, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the method for the present invention, described force air flow through wax layer and can implement in intensification sweating effort any stage, it is preferable that implement at the intensification diaphoresis initial stage.
In the method for the present invention, the described wax layer that forces air flow through is utilized in above wax layer to increase what air pressure realized, as at the pressure of wax layer 0.2～2.0 atmospheric pressure (gauge pressure) applied above, and remained normal pressure below wax layer.
In the method for the present invention, the described wax layer that forces air flow through is utilized in below wax layer to reduce what air pressure realized, as kept normal pressure above wax layer, and maintain the pressure of-0.2～-1.0 atmospheric pressure (gauge pressure) below wax layer.
In the method for the present invention, described sweatbox connects recovery system, to reclaim low-boiling point liquid.Recovery system can adopt the multiple feasible modes such as liquid absorption or refrigeration system, it is preferred to liquid absorption system.
Diaphoresis de-oiling method is that the character utilizing wax different with oil fusing point is easily separated to produce soap wax and low melt point paraffin product, but in intensification sweating effort, in wax layer, the wax of solid-state and the oil of liquid are difficult to separate, this is that intermolecular force is bigger owing to wax and two kinds of components of oil are all nonpolar hydrocarbon molecules；The wax crystallization of solid-state forms capillary pipe structure simultaneously, and oil has stronger adsorption, and this results in and only is difficult to be kept completely separate by wax and oil in the common sweating effort of gravity natural separation.Generally adopt the method such as prolongation sweating sessions, raising diaphoresis final temperature to make the oil content of final products meet the requirements, but this can cause that again production cycle length, wax product yield are low.And for the fusing point high melting point paraffin product at about 70 DEG C, owing to chemical composition is more complicated, cause the more tiny densification of crystals upon crystallization structure, discharging of fluid oil is formed huge filter flow resistance, though adopt extend sweating sessions, improve the methods such as diaphoresis final temperature and can not produce fusing point about 70 DEG C meet semi-refined or full refining product standard high melting point paraffin product.These all have impact on the extensive use of diaphoresis de-oiling method.
The present invention is by the further investigation to common sweating effort, it is difficult to be kept completely separate reason for wax and oil, by adopting the method that air-flow carries out fluid oil by wax layer to force wax and oil separating in intensification sweating effort, enhance separating effect and accelerate separating rate；Simultaneously it is also preferred that under stress mix low-boiling point liquid after heating raw materials fusing, these materials boiling point under stress higher than now raw material temperature and in liquid condition, and due to have a good intersolubility with raw material and dispersed in the feed；Keep being cooled to by raw material under pressure condition below fusing point 10 DEG C～15 DEG C, and constant temperature 0.1h～3.0h is so that wax layer crystallization is more abundant；In thermostatic process, it is gradually lowered pressure to normal pressure simultaneously, now raw material is in softer solid state, and temperature is higher than the boiling point (or bubble point) under low-boiling point liquid normal pressure, low-boiling point liquid slowly decline with pressure and vaporize gradually (or in intensification sweating effort behind gradually vaporization), homodisperse micro-bubble can be formed in wax layer, the space that these micro-bubbles are formed is prone to form some tiny passages in wax layer in sweating effort, thus being conducive to the discharge of oil in intensification sweating effort.Utilize air-flow to carry out the oil of liquid to force to separate wax and oil by wax layer simultaneously in intensification sweating effort, enhance separating effect and accelerate separating rate.
Angle between common diaphoresis ware ware plate and baffle plate is 90 °, and in sweating effort, wax layer shrinks, when forming pressure differential up and down to force air flow through wax layer at wax layer, produce sometimes air-flow slit flow through between wax layer and ware plate cross and without the phenomenon of wax layer.In the inventive method, increase the angle between diaphoresis ware ware plate and baffle plate, increase the resistance between wax layer and ware plate, it can be ensured that air-flow passes through wax layer to carry out fluid oil.
The invention have the advantage that by adopting the method that air-flow carries out fluid oil by wax layer to force wax and oil separating in intensification sweating effort, enhance separating effect and accelerate separating rate；Utilize low-boiling point liquid vaporization to form homodisperse micro-bubble in wax layer simultaneously, be also beneficial to the quick discharge of oil, thus having reached improve wax product yield and shorten the purpose of production cycle.The square law device investment of the present invention is low, production process is simple and operating cost is low, solvent-free contaminated environment, make the method highly effective more of this solvent-free production soap wax of diaphoresis removing oil and low melt point paraffin, it might even be possible to for producing the high melting point paraffin that fusing point is at about 70 DEG C.
Detailed description of the invention
Increase the angle between diaphoresis ware ware plate and baffle plate；Diaphoresis ware top connects dismountable sealing device and is connected with surge tank and compressor, and/or connects surge tank and vacuum pump in diaphoresis ware bottom；With slack wax for raw material, after adding heat fusing and preferably under stress mixing low-boiling point liquid, load diaphoresis ware；Wax layer heating-cooling speed is controlled with water-bath；Keep making wax layer temperature be down to preset temperature constant temperature a period of time under pressure, thermostatic process is gradually lowered the pressure of more than paraffin layer to normal pressure；In intensification sweating effort, start compressor with in wax layer malleation formed above, and/or start vacuum pump with in wax layer negative pressure formed below, in order to force air flow through wax layer；Wax layer temperature stops diaphoresis degreasing process after reaching preset temperature；Product for the purpose of on wax after clay-filtered, molding, packaging being.By these means, make diaphoresis method to produce high melting point paraffin that fusing point is at about 70 DEG C；And for soap wax and low melt point paraffin, when time decreased 30%～50% in intensification diaphoresis stage, purpose product yield can be made to improve 5～10 percentage points.
1-5 illustrates diaphoresis of the present invention and the method producing soap wax and paraffin by the following examples.
Embodiment 1
The present embodiment includes: the processes such as (1) preparation, (2) charging, (3) decrease temperature crystalline, (4) intensification diaphoresis, (5) thick product collection, (6) product purification.
(1) preparation
The sealing system on diaphoresis ware (angle between diaphoresis ware ware plate and baffle plate is 120 °) top is connected with surge tank and compressor.Diaphoresis ware ware plate bottom pad water.
Diaphoresis ware chuck and removable coil pipe are connected with blood circulation, coil pipe are fixed on diaphoresis ware；With water for medium；Start the heating function of blood circulation, make recirculated water be warming up to 45 DEG C.
(2) charging
With normal four line slack waxs (fusing point 41.5 DEG C, oil content 13.2%) for raw material, heat and after melting to 45 DEG C, add diaphoresis ware；The sealing system on diaphoresis ware top is installed and connects with pressurized buffer tank and compressor；Start compressor and keep pressurized buffer pressure inside the tank stable 5.0～5.2 atmospheric pressure (gauge pressure).
(3) cooling-thermostatical crystallization
Start the refrigerating function of blood circulation, control wax layer temperature and drop to 30.0 DEG C so that wax layer crystallization forms solid with the rate of temperature fall of 2.0 DEG C/h, and constant temperature 1.0h is so that wax layer crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank by emptying system and is gradually decrease to normal pressure.Close the refrigerating function of closed loop system.
(4) intensification diaphoresis
Discharge diaphoresis ware pad water.The outlet of diaphoresis ware connects intermediate storage tank to receive under wax；Start compressor and keep pressurized buffer pressure inside the tank stable 1.2～1.4 atmospheric pressure (gauge pressure), and remaining normal pressure below wax layer；Start the heating function of blood circulation, make wax layer temperature be increased to 42.0 DEG C with the heating rate of 1.5 DEG C/h and carry out diaphoresis removing oil.Stop compressor, terminate diaphoresis degreasing process (total heating-up time is 8 hours).
(5) thick product is collected
The outlet of diaphoresis ware changes the thick product storage tank of connection into；Blood circulation continues to be heated to 60 DEG C to melt on taking-up wax, is thick product.
(6) product purification
Thick product after clay-filtered, molding, packaging namely for the purpose of product.
Product property: fusing point 47.6 DEG C, oil content 1.47%, meets the associated specifications of commodity soap wax top grade product.Soap wax product yield is 40.8%(relative raw material slack wax).
Embodiment 2
The present embodiment includes: the processes such as (1) preparation, (2) charging, (3) cooling-thermostatical crystallization, (4) intensification diaphoresis, (5) thick product collection, (6) product purification.
(1) preparation
The sealing system on diaphoresis ware (angle between diaphoresis ware ware plate and baffle plate is with embodiment 1) top is connected with surge tank and compressor；Pressurized buffer tank emptying system and diaphoresis ware lower exhaust port are connected with recovery system respectively, with liquid paraffin for absorbing medium.
Diaphoresis ware ware plate bottom pad water.Diaphoresis ware chuck and removable coil pipe are connected with blood circulation, coil pipe are fixed on diaphoresis ware；With water for medium；Start the heating function of blood circulation, make recirculated water be warming up to 45 DEG C.
(2) charging
With normal four line slack waxs (character is with embodiment 1) for raw material, heat the isopentane mixing 0.5% after melting to 45 DEG C under 5.0～5.2 atmospheric pressure (gauge pressure), add diaphoresis ware；Keep pressurized buffer pressure inside the tank stable at 5.0～5.2 atmospheric pressure.
(3) cooling-thermostatical crystallization
Start the refrigerating function of blood circulation, control wax layer temperature and drop to 30.0 DEG C so that wax layer crystallization forms solid with the rate of temperature fall of 2.0 DEG C/h, and constant temperature 1.0h is so that wax layer crystallization is more abundant.
The constant temperature stage controls pressurized buffer pressure inside the tank by emptying system and is gradually decrease to normal pressure.Expellant gas passes through liquid paraffin to reclaim low-boiling point liquid isopentane.Close the refrigerating function of closed loop system.
(4) intensification diaphoresis
Discharge diaphoresis ware pad water.The outlet of diaphoresis ware connects intermediate storage tank to receive under wax；Start compressor and keep pressurized buffer pressure inside the tank stable 1.2～1.4 atmospheric pressure (gauge pressure), and remaining normal pressure below wax layer；Start the heating function of blood circulation, make wax layer temperature be increased to 42.0 DEG C with the heating rate of 1.5 DEG C/h and carry out diaphoresis removing oil.
In intensification sweating effort, expellant gas passes through liquid paraffin to reclaim low-boiling point liquid isopentane.Stop compressor, terminate diaphoresis degreasing process (total heating-up time is 8 hours).
(5) thick product is collected
The outlet of diaphoresis ware changes the thick product storage tank of connection into；Blood circulation continues to be heated to 60 DEG C to melt on taking-up wax, is thick product.
(6) product purification
Thick product after clay-filtered, molding, packaging namely for the purpose of product.
Product property: fusing point 47.5 DEG C, oil content 1.32%, meets the associated specifications of commodity soap wax top grade product.Soap wax product yield is 42.7%(relative raw material slack wax).
Embodiment 3
The present embodiment includes: the processes such as (1) preparation, (2) charging, (3) cooling-thermostatical crystallization, (4) intensification diaphoresis, (5) thick product collection, (6) product purification.
(1) preparation
Surge tank is installed in diaphoresis ware (diaphoresis ware ware plate is 150 ° with the angle between baffle plate) bottom and is connected vacuum pump.Diaphoresis ware ware plate bottom pad water.
Diaphoresis ware chuck and removable coil pipe are connected with blood circulation, coil pipe are fixed on diaphoresis ware；With water for medium；Start the heating function of blood circulation, make recirculated water be warming up to 55 DEG C.
(2) charging
With second line of distillation slack wax (fusing point 50.6 DEG C, oil content 21.4%) for raw material, heat and after melting to 55 DEG C, add diaphoresis ware；The sealing system on diaphoresis ware top is installed and connects with pressurized buffer tank and compressor；Start compressor and keep pressurized buffer pressure inside the tank stable 5.0～5.2 atmospheric pressure (gauge pressure).
(3) cooling-thermostatical crystallization
Start the refrigerating function of blood circulation, control wax layer temperature and drop to 37.0 DEG C so that wax layer crystallization forms solid with the rate of temperature fall of 2.0 DEG C/h, and constant temperature 2.0 hours is so that wax layer crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank by emptying system and is gradually decrease to normal pressure.Close the refrigerating function of closed loop system.
(4) intensification diaphoresis
Discharge diaphoresis ware pad water.The outlet of diaphoresis ware connects intermediate storage tank to receive under wax；Start vacuum pump and keep pressure-reducing cushioning pressure inside the tank stable-0.5～-0.7 atmospheric pressure (gauge pressure), and remaining normal pressure above wax layer；Start the heating function of blood circulation, control wax layer and make wax layer temperature be increased to 49.0 DEG C with the heating rate of 1.5 DEG C/h to carry out diaphoresis removing oil.Stop vacuum pump, terminate sweating effort (total heating-up time is 8 hours).
(5) thick product is collected
The outlet of diaphoresis ware changes the thick product storage tank of connection into receive on wax；Blood circulation continues heating wax layer and is warming up to 70 DEG C to melt on taking-up wax, is thick product.
(6) product purification
Thick product after clay-filtered, molding, packaging namely for the purpose of product.
Product property: fusing point 55.1 DEG C, oil content 1.52%, meets commodity 54#The technology requirement that semi-refined wax is relevant.54#Semi-refined wax product yield is 44.5%(relative raw material slack wax).
Embodiment 4
The present embodiment includes: the processes such as (1) preparation, (2) charging, (3) cooling-thermostatical crystallization, (4) intensification diaphoresis, (5) thick product collection, (6) product purification.
(1) preparation
In diaphoresis ware (diaphoresis ware ware plate with the angle between baffle plate with embodiment 3) bottom, surge tank it is installed and is connected vacuum pump；Diaphoresis ware ware plate bottom pad water.
Diaphoresis ware chuck and removable coil pipe are connected with blood circulation, coil pipe are fixed on diaphoresis ware；With water for medium；Start the heating function of blood circulation, make recirculated water be warming up to 55 DEG C.
The sealing system on diaphoresis ware top is installed and connects with pressurized buffer tank and compressor；The emptying system of pressurized buffer tank and diaphoresis ware lower part outlet are connected with recovery system respectively, with liquid paraffin for absorbing medium.
(2) charging
With second line of distillation slack wax (character is with embodiment 3) for raw material, heat the methyl formate mixing 1.0% after melting to 55 DEG C under 5.0～5.2 atmospheric pressure (gauge pressure), add diaphoresis ware；Keep pressurized buffer pressure inside the tank stable 5.0～5.2 atmospheric pressure (gauge pressure).
(3) cooling-thermostatical crystallization
Start the refrigerating function of blood circulation, control wax layer temperature and drop to 37.0 DEG C so that wax layer crystallization forms solid with the rate of temperature fall of 2.0 DEG C/h, and constant temperature 2.0 hours is so that wax layer crystallization is more abundant.
The constant temperature stage controls pressurized buffer pressure inside the tank by emptying system and is gradually decrease to normal pressure.Expellant gas passes through liquid paraffin to reclaim low-boiling point liquid methyl formate.Close the refrigerating function of closed loop system.
(4) intensification diaphoresis
Discharge diaphoresis ware pad water.The outlet of diaphoresis ware connects intermediate storage tank to receive under wax；Start vacuum pump and keep pressure-reducing cushioning pressure inside the tank stable in-0.5～-0.7 atmospheric pressure (gauge pressure), and remaining normal pressure above wax layer；Start the heating function of blood circulation, control wax layer and make wax layer temperature be increased to 49.0 DEG C with the heating rate of 1.5 DEG C/h to carry out diaphoresis removing oil.
In intensification sweating effort, expellant gas passes through liquid paraffin to reclaim low-boiling point liquid methyl formate.Stop vacuum pump, terminate sweating effort (total heating-up time is 8 hours).
(5) thick product is collected
The outlet of diaphoresis ware changes the thick product storage tank of connection into receive on wax；Blood circulation continues heating wax layer and is warming up to 70 DEG C to melt on taking-up wax, is thick product.
(6) product purification
Thick product after clay-filtered, molding, packaging namely for the purpose of product.
Product property: fusing point 55.5 DEG C, oil content 1.33%, meets commodity 54#The technology requirement that semi-refined wax is relevant.54#Semi-refined wax product yield is 47.2%(relative raw material slack wax).
Embodiment 5
The present embodiment includes: the processes such as (1) preparation, (2) charging, (3) cooling-thermostatical crystallization, (4) intensification diaphoresis, (5) thick product collection, (6) product purification.
(1) preparation
In diaphoresis ware (diaphoresis ware ware plate with the angle between baffle plate with embodiment 3) bottom, surge tank it is installed and is connected vacuum pump.Diaphoresis ware ware plate bottom pad water.Diaphoresis ware chuck and removable coil pipe are connected with blood circulation, coil pipe are fixed on diaphoresis ware；With water for medium；Start the heating function of blood circulation, make recirculated water be warming up to 65 DEG C.
The sealing system on diaphoresis ware top is installed and connects with pressurized buffer tank and compressor；The emptying system of pressurized buffer tank and diaphoresis ware lower part outlet are connected with recovery system respectively, with liquid paraffin for absorbing medium.
(2) charging
With the line slack wax that subtracts four (the line slack wax character that subtracts four: initial boiling point: 410 DEG C, 90% distillate a little: 520 DEG C；Fusing point 58.5 DEG C；Oil content 26.9%) for raw material, heat the pentane mixing 0.7% after melting to 65 DEG C under 5.0～5.2 atmospheric pressure (gauge pressure), add diaphoresis ware；Keep pressurized buffer pressure inside the tank stable 5.0～5.2 atmospheric pressure (gauge pressure).
(3) cooling-thermostatical crystallization
Start the refrigerating function of blood circulation, control wax layer temperature and drop to 45.0 DEG C so that wax layer crystallization forms solid with the rate of temperature fall of 2.0 DEG C/h, and constant temperature 2.0 hours is so that wax layer crystallization is more abundant.
The constant temperature stage controls pressurized buffer pressure inside the tank by emptying system and is gradually decrease to normal pressure.Expellant gas passes through liquid paraffin to reclaim low-boiling point liquid pentane.Close the refrigerating function of closed loop system.
(4) intensification diaphoresis
Discharge diaphoresis ware pad water.The outlet of diaphoresis ware connects intermediate storage tank to receive under wax；Start compressor and keep the stable maintenance normal pressure below 1.3～1.5 atmospheric pressure (gauge pressure), diaphoresis ware ware plate of buffering pressure inside the tank；Start circulation system function, make wax layer temperature be increased to 65.0 DEG C with the heating rate of 2.0 DEG C/h.
Stop compressor.Start vacuum pump and keep pressure-reducing cushioning pressure inside the tank stable in-0.5～-0.7 atmospheric pressure (gauge pressure), and remaining normal pressure above wax layer；Blood circulation controls wax layer makes wax layer temperature be increased to 70.0 DEG C with the heating rate of 1.0 DEG C/h.
In intensification sweating effort, expellant gas passes through liquid paraffin to reclaim low-boiling point liquid pentane.Stop vacuum pump, terminate sweating effort.
(5) thick product is collected
The outlet of diaphoresis ware changes the thick product storage tank of connection into receive on wax；Continue to raise blood circulation temperature to 90 DEG C, to melt on taking-up wax, be the thick product of high melting point paraffin.
(6) product purification and molding, packaging
Thick product is high melting point paraffin product after clay-filtered, molding, packaging.
High melting point paraffin product property: fusing point: 72.6 DEG C, oil content: 0.48%.Meet the associated specifications of commodity 72# paraffin wax fully refined.72# paraffin wax fully refined product yield is that 14.3%(is relative to slack wax raw material).
Comparative example 1
With normal four line slack waxs (character is with embodiment 1) for raw material, after adding heat fusing, add common sweat tank.Wax layer temperature is made to drop to 30.0 DEG C with the rate of temperature fall of 2.0 DEG C/h；Make wax layer temperature be increased to 42.0 DEG C with the heating rate of 1.0 DEG C/h and carry out diaphoresis removing oil (total heating-up time was for 12 hours).Diaphoresis takes out residue in sweat tank after terminating, after clay-filtered, molding namely for the purpose of product.
Product property: fusing point 47.3 DEG C, oil content 1.71%, meets the technology requirement of commodity soap wax.Soap wax product yield is 34.1%.
Comparative example 2
With second line of distillation slack wax (character is with embodiment 3) for raw material, after adding heat fusing, add common sweat tank.Wax layer temperature is made to drop to 37.0 DEG C with the rate of temperature fall of 2.0 DEG C/h；Make wax layer temperature be increased to 51.0 DEG C with the heating rate of 1.0 DEG C/h and carry out diaphoresis removing oil (total heating-up time was for 14 hours).Diaphoresis is taken out on wax after terminating, after clay-filtered, molding namely for the purpose of product.
Product property: fusing point 55.6 DEG C, oil content 1.75%, meets commodity 54#The technology requirement that semi-refined wax is relevant.54#Semi-refined wax product yield is 37.4%.
By embodiment 1-5 it can be seen that the method for diaphoresis of the present invention and production soap wax and paraffin, by the angle of change diaphoresis ware ware plate and baffle plate, increase the improvement to sweatbox such as pressurization and/or vacuum facility；By adding low-boiling point liquid, and in intensification sweating effort, force air flow through the improvement to sweating process such as wax layer；Accelerate wax and oil separating speed, and enhance wax and oil separating effect, make diaphoresis method to produce high melting point paraffin (embodiment 5) that fusing point is at about 70 DEG C；And for soap wax and low melt point paraffin, (embodiment 1 adds 6.7 percentage points and 8.6 percentage points than comparative example 1 respectively with embodiment 2 can to improve purpose wax product yield；Embodiment 3,4 adds 7.1 percentage points and 9.8 percentage points than comparative example 2 respectively) and (time in intensification diaphoresis stage, embodiment 1 reduces 33% and 33% respectively with embodiment 2 than comparative example 1 to shorten the production cycle；Embodiment 3,4 reduces 43% and 43% than comparative example 1 respectively).
Claims (20)
1. a method for diaphoresis and production soap wax and paraffin, including herein below:
(1) in sweatbox, water is padded；
(2) with oil content less than 30%, melting range be raw material for the slack wax of 25 DEG C～70 DEG C, add and load sweatbox after heat fusing；
(3) predetermined temperature of below slack wax fusing point 8 DEG C～20 DEG C constant temperature a period of time it is cooled to the speed of 1.0 DEG C/h～4.0 DEG C/h；
(4) the pad water in sweatbox is discharged, then with the ramp of 0.5 DEG C/h～3.0 DEG C/h；Temperature-rise period forces air flow through wax layer；Wax layer stops diaphoresis after reaching predetermined temperature；
(5) collect on wax；
(6) on wax after refining, molding namely for the purpose of product.
2. in accordance with the method for claim 1, it is characterized in that, step (2) Raw under stress mixes low-boiling point liquid after adding heat fusing, described low-boiling point liquid boiling point at ambient pressure is lower than the predetermined temperature cooled, and boiling point under high pressure is higher than the maximum temperature of the reinforced process of step (2).
3. in accordance with the method for claim 2, it is characterised in that one or more in alkane, alkene, alkynes, alkadienes, alcohol, aldehyde, ether, ester, halogenated hydrocarbons of described low-boiling point liquid.
4. in accordance with the method for claim 3, it is characterised in that one or more in alkane, alcohol and ester of described low-boiling point liquid.
5. the content described in claim 2, it is characterised in that the addition of described low-boiling point liquid accounts for the 0.1%～5.0% of raw material slack wax weight, it is preferred to 0.3%～2.0%.
6. in accordance with the method for claim 2, it is characterised in that at wax layer air pressure applied above in step (2) and step (3), to ensure to be in liquid condition reinforced with maintenance low-boiling point liquid in temperature-fall period.
7. in accordance with the method for claim 6, it is characterised in that described air pressure is 0.5～20.0 atmospheric pressure of gauge, it is preferred to 1.0～10.0 atmospheric pressure.
8. in accordance with the method for claim 1, it is characterized in that, the wax layer employing that force air flow through described in step (4) increases air pressure above wax layer and/or reduces air pressure below wax layer, make wax layer upper and lower form pressure differential to realize, described pressure differential is 0.1～5.0 atmospheric pressure, it is preferred to 0.2～2.0 atmospheric pressure.
9. in accordance with the method for claim 1, it is characterised in that described in step (3), the speed of cooling is 2.0 DEG C/h～3.0 DEG C/h.
10. in accordance with the method for claim 1, it is characterised in that the predetermined temperature described in step (3) is below raw material slack wax fusing point 10 DEG C～15 DEG C.
11. in accordance with the method for claim 1, it is characterised in that the time of constant temperature described in step (3) is 0～3.0h, it is preferable that 0.1～3.0h.
12. in accordance with the method for claim 11, it is characterised in that while constant temperature, be gradually lowered pressure to normal pressure.
13. in accordance with the method for claim 1, it is characterised in that the speed heated up described in step (4) is 1.0 DEG C/h～2.0 DEG C/h.
14. in accordance with the method for claim 1, it is characterised in that the predetermined temperature heated up described in step (4) is the fusing point 2 DEG C～10 DEG C lower than purpose product.
15. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is implemented in intensification sweating effort any stage, it is preferable that implement at the intensification diaphoresis initial stage.
16. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through adopts increase air pressure above wax layer to realize, and at wax layer 0.2～2.0 atmospheric gauge applied above, and remains normal pressure below wax layer.
17. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through adopts reduction air pressure below wax layer to realize, and keeps normal pressure, and maintain-0.2～-1.0 atmospheric gauge below wax layer above wax layer.
18. according to the arbitrary described method of claim 2-7, it is characterised in that reclaim low-boiling point liquid in constant temperature and intensification sweating effort.
19. in accordance with the method for claim 18, it is characterised in that adopt liquid to absorb or the mode of refrigeration system reclaims low-boiling point liquid.
20. in accordance with the method for claim 1, it is characterised in that described sweatbox is diaphoresis ware, the angle between diaphoresis ware ware plate and baffle plate is 90 °～170 °, it is preferred to 120 °～150 °.
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| CN106188110A (en) * | 2016-07-13 | 2016-12-07 | 北京化工大学 | A kind of metallic organic framework functional fluorescence material and preparation method and applications |
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| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106188110A (en) * | 2016-07-13 | 2016-12-07 | 北京化工大学 | A kind of metallic organic framework functional fluorescence material and preparation method and applications |
| CN106188110B (en) * | 2016-07-13 | 2019-05-17 | 北京化工大学 | A kind of metal-organic framework functional fluorescence material and preparation method and applications |
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