CN107513432B - The method for preparing high dropping point microwax - Google Patents

The method for preparing high dropping point microwax Download PDF

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Publication number
CN107513432B
CN107513432B CN201610432974.6A CN201610432974A CN107513432B CN 107513432 B CN107513432 B CN 107513432B CN 201610432974 A CN201610432974 A CN 201610432974A CN 107513432 B CN107513432 B CN 107513432B
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wax layer
sweating
dropping point
wax
temperature
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CN107513432A (en
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孙剑锋
赵彬
王诗语
郭慧兵
张志银
陈保莲
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G73/00Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/42Refining of petroleum waxes

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention discloses the methods for preparing high dropping point microwax.This method is on the basis of common sweating process, liquid composition is carried out to force separation solids fraction and liquid composition by wax layer using air-flow in sweating effort, micro-bubble is formed in wax layer using the gas that the decomposable substance of dissolution in the feed generates simultaneously, it is also beneficial to the quick discharge of liquid composition, so that sweating method be allow to produce high dropping point crystallite wax product.The method of the present invention has many advantages, such as that equipment investment is low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution.

Description

The method for preparing high dropping point microwax
Technical field
The invention belongs to pertroleum wax production technical fields, more particularly to the method for preparing high dropping point 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, solid-state It is lower that there is the needle-like crystal structure more tiny than soap manufacturing paraffin and paraffin.The dropping point of the crystallite wax product standardized in national standard is 67 DEG C~92 DEG C.
Dewaxing is that the process for the slack wax that oil content is 10~30% or so is prepared by raw material of lube cut.De-oiling be with Slack wax is the process that raw material prepares the scale wax below of oil content 2%, and de-oiling technique mainly has solvent deoiling and sweating de-oiling.Slightly Through clay-filtered or hydrofinishing and molding, packaging and other steps, commodity oil wax can be obtained again in paraffin.
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, and the fusing point of the lesser n-alkane of molecular weight is lower;When molecular weight is identical, the fusing point of isoparaffin and cycloalkane is wanted Lower than n-alkane, and isomery degree more high-melting-point is lower, or even is at normal temperature just in liquid condition, i.e., usually said Oil.
Common sweating process 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) it crystallizes: by raw material with little 10~20 DEG C of its fusing point or less are progressively cooled in the rate of temperature fall of 4 DEG C/h.In cooling procedure, various components are by fusing point by height It is successively crystallized to low sequence and forms solid;(3) it sweating: after wax layer temperature reaches preset cooling final temperature, bleeds off Pad water;Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components by fusing point by as low as High sequence, which is successively fused into liquid and flows out the wax layer residue (on wax) finally obtained (under wax), to be exactly high-melting-point, low contains The wax of oil;(4) it refines: collection crude product (continue to increase temperature after sweating effort, be taken out on wax with fusing, as thick production Product), (predetermined temperature, mistake after addition carclazyte and constant temperature were stirred to the predetermined time are warming up to after melting crude product through clay-filtered Filter) after, reshaping, packaging are purpose product.
Common sweating process can produce soap manufacturing paraffin and low melt point paraffin under solid-state with coarse flaky crystal structure, but The microwax under solid-state with tiny needle-like crystal structure cannot be produced.Have experiments have shown that, common sweating process produces microwax When, though using sweating sessions and the method that improves sweating final temperature is extended, oil content and yield on sweating later period wax without It closes, i.e., the oil content on wax does not decline with the decline of yield, so so far there are no with sweating process production crystallite wax product Report.The highest trade mark of the crystallite wax product standardized in national standard is No. 90 (87~92 DEG C of dropping point), also only has one at present A producer produces No. 90 microwaxes of primes.For the crystallite wax product of higher dropping point, associated production technology and product are had no Report.
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 on sweating process, but these methods cannot still produce microwax.
Sweating process is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product, is being mentioned The today for advocating green low-carbon, environmental protection and energy saving, the demand using sweating process production crystallite wax product are more urgent.Meanwhile it developing The high dropping point crystallite wax product of No. 90 or more (92 DEG C of dropping point or more) is to meet related social demand, and very urgent times Business.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of methods for preparing high dropping point microwax, specifically It is using sweatbox, on the basis of common sweating process, addition oil-soluble is decomposable after raw material heating fusing generates gas Substance;And liquid composition (oil and compared with the wax of low melting point) is carried out to force point by wax layer using air-flow in sweating effort From solids fraction (wax of higher melt) and liquid composition, enhances separating effect and accelerate separating rate, keep sweating this Solvent-free separation method can prepare the crystallite wax product of high dropping point.The method of the present invention is with equipment investment is low, produced Journey is simple and operating cost is low, energy-saving safe and the advantages that solvent-free pollution.
A kind of method preparing high dropping point microwax of the invention, including the following contents:
(1) charge: the commodity microwax for being 87 DEG C~92 DEG C using dropping point is packed into sweating dress as raw material after heating fusing It sets;
(2) it crystallizes: wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h rate, at one section of high temperature constant temperature Between;5 DEG C~20 DEG C of raw material dropping point or less of cooling final temperature is cooled to 0.5 DEG C/h~2.5 DEG C/h rate again, and low Warm constant temperature is for a period of time;
(3) sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate;After wax layer reaches predetermined temperature and constant temperature for a period of time Stop sweating;Wax layer is forced air flow through in sweating effort;
(4) it refines: being high dropping point crystallite wax product after refining on wax.
In method of the invention, the dropping point of the source commodity microwax is 87 DEG C~92 DEG C.The high dropping point Microwax refers to microwax of the dropping point at 92 DEG C or more.
In method of the invention, after raw material heating fusing, it is preferably added to the decomposable oil soluble material for generating gas.Tool Sweating raw material is first heated and is melted by gymnastics conduct, then is packed into after the decomposable substance for generating gas of oil-soluble is dissolved in raw material Sweatbox.It includes organic azo compound, sulfonyl hydrazines compound, organic nitroso that the oil-soluble, which can decompose substance, Close object, organic peroxide etc., preferably one or more of organic azo compound and organic peroxide.Oil-soluble can divide The additional amount for solving substance is the 0.01%~15.00% of raw material weight, preferably 0.03%~8.00%.
Wherein, the organic azo compound is selected from azobisisoheptonitrile (ABVN), azodiisobutyronitrile (AIBN), idol One group of substance that nitrogen dicyclohexyl formonitrile HCN (ACCN) is constituted;The sulfonyl hydrazines compound is selected from benzene sulfonyl hydrazide, to toluene sulphur One group of substance that hydrazides, 4,4 '-bis oxides (benzene sulfonyl hydrazide) are constituted;The organic nitroso compounds are selected from dinitroso five Methenamine and/or N, N '-dimethyl N, N '-dinitroso phthalic amide;The organic peroxide is selected from peroxide Change dibenzoyl (BPO), dilauroyl peroxide (LPO), diacetyl peroxide, dicetyl peroxydicarbonate isopropyl ester (IPP), peroxidating One group of substance of the compositions such as two dicyclohexyl carbonates (DCPO).
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.In the sweating effort of step (3), the wax layer that forces air flow through is used in wax layer Fang Zengjia air pressure and/or air pressure is reduced below wax layer, so that wax layer upper and lower is formed pressure difference and realize.The pressure difference one As be 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, in the temperature-fall period of step (2) described crystallization, the rate of temperature fall before high-temperature constant temperature section It is preferred that 1.5 DEG C/h~2.5 DEG C/h.The proper temperature of the high-temperature constant temperature section of the temperature-fall period is raw material microwax dropping point- + 2.0 DEG C of 1.0 DEG C~dropping point, preferably raw material microwax dropping point~+1.0 DEG C of dropping point.The high-temperature constant temperature section of crystallization process Time be 0~4.0 hour, preferably 0.1~4.0 hour, more preferably 1.0~4.0 hours.
In method of the invention, rate of temperature fall of the temperature-fall period of step (2) described crystallization after high-temperature constant temperature section is excellent Select 1.0 DEG C/h~2.0 DEG C/h.The cooling final temperature is preferably 8 DEG C~15 DEG C of raw material microwax dropping point or less.It is described Be cooled to final temperature after, increase the cryogenic thermostat stage so that solid crystal is more abundant, the time in cryogenic thermostat stage is 0~ 3.0 hours, preferably 0.1~3.0 hour, more preferably 1.0~3.0 hours.
In method of the invention, the heating rate of sweating effort described in step (3) preferably 1.0 DEG C/h~2.0 DEG C/h.Its Final temperature, that is, predetermined temperature of middle temperature-rise period is lower than 2 DEG C~10 DEG C of purpose product dropping point.Described being warming up to is default After temperature, increase the constant temperature stage so that solids fraction separates more sufficiently with liquid composition, the time in constant temperature stage is 0~5.0 small When, preferably 0.1~5.0 hour, preferably 1.0~5.0 hours.
In 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 method of the invention, wax layer is forced air flow through described in step (3) can be real in sweating effort any stage It applies, preferably implements at sweating initial stage.
In method of the invention, wax layer is forced air flow through described in step (3) and is utilized in increase air pressure above wax layer It realizes, can such as apply the pressure of 0.2~2.0 atmospheric pressure (gauge pressure) above wax layer, and remain normal pressure below wax layer.
In method of the invention, wax layer is forced air flow through described in step (3) and is utilized in reduction air pressure below wax layer It realizes, normal pressure can be such as kept above wax layer, and maintain the pressure of -0.2~-0.8 atmospheric pressure (gauge pressure) below wax layer.
Sweating method is to be separated using wax and oil property with different melting points to produce pertroleum wax, is sent out for pertroleum wax Sweat process studies have shown that liquid composition is gradually discharged along crystalline portion in sweating effort, be similar to liquid in capillary The case where being flowed in pipe.For microwax, since its main component is isoparaffin and cycloalkane, chemical composition is complicated, causes Crystals upon crystallization structure is more fine and compact, forms huge filter flow resistance power to the discharge of liquid liquid component, this is resulted in only Solids fraction and liquid composition are difficult to be kept completely separate in the common sweating effort of gravity natural separation.Therefore common sweating process The crystallite wax product for meeting relevant criterion cannot be prepared, the crystallite wax product of high dropping point can not be prepared.
The present invention in order to allow sweating it is this it is solvent-free production pertroleum wax method prepare high dropping point crystallite wax product, By the further investigation to common sweating effort, it is difficult to the reason of separating with liquid composition for solids fraction, by sweating The method that use forces air flow through that wax layer carries out liquid composition in the process forces liquid composition to separate with solids fraction, enhances Separating effect simultaneously accelerates separating rate;The crystallization of pertroleum wax can be made more by increasing the high temperature constant temperature stage in crystallization process Greatly, be conducive to the discharge of liquid composition in sweating effort.For microwax crystallization process studies have shown that the chemical composition of raw material It is to determine the main factor of crystal habit, while the condition of cooling procedure also will affect crystal habit, especially in dropping point Influence of the cooling condition to crystal habit at a temperature of neighbouring is most obvious.Microwax has portion when being cooled near dropping point Crystallization is divided to be precipitated, this partially crystallizable body can be used as the nucleus for being subsequently formed crystallization, increases the high temperature constant temperature stage at this time, can make Nucleus can sufficiently increase, and form larger sized crystal, although this larger sized crystal is not so good as soap manufacturing paraffin and low melting point The crystallization of paraffin is coarse like that, but is also highly beneficial to sweating stage discharge liquid composition.Further preferably raw material heats simultaneously Oil-soluble is added after fusing can decompose substance, these substances are decomposable to generate gas, and has preferable dissolubility in the feed And it is dispersed in wax layer.Raw material is cooled to wax layer in the time terminated after dropping point or less to sweating effort and is in softer Solid state, decomposable substance slowly decomposes the gas released during this, can be formed in wax layer evenly dispersed small Bubble, the space that these micro-bubbles are formed is easy to be formed in sweating effort several tiny channels in wax layer, to have Conducive to the discharge of liquid composition in sweating effort.It is preferred that decomposing the gas for generating the nontoxic no special odor such as nitrogen or carbon dioxide Oil-soluble can decompose substance, and generate other materials molecular weight it is low, in sweating effort will with liquid oil arrange Wax layer out.The cryogenic thermostat stage for being aided with crystallization process again keeps solid crystal more abundant and the constant temperature stage of sweating effort makes Solids fraction separates the methods of more abundant with liquid composition, and sweating process is allowed to prepare the crystallite wax product of high dropping point.
The invention has the advantages that by using air-flow to increase in sweating effort by the method that wax layer carries out liquid composition Strong solids fraction and the separating effect of liquid composition simultaneously accelerate separating rate;Crystalline size is increased using high temperature crystallization, together Shi Liyong oil-soluble can decompose the gas that substance decomposition generates and form evenly dispersed micro-bubble in wax layer, be also beneficial to liquid The quick discharge of state component;To allow sweating process to prepare high dropping point crystallite wax product, and have plant investment low, raw Production process is simple and operating cost is low, safety, energy conservation and the advantages that solvent-free pollution environment.
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;Micro-crystal wax feed heating melts and is preferably added to the decomposable generation gas of oil-soluble Substance after be packed into sweating ware;Wax layer heating-cooling speed is controlled with oil bath;Wax layer temperature is down to raw material dropping point temperature nearby simultaneously High temperature constant temperature is for a period of time;Continue to be cooled to preset temperature and cryogenic thermostat for a period of time;In sweating effort, start compressor With in wax layer positive pressure formed above, and/or starting vacuum pump is 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 effort afterwards for a period of time;It is high dropping point after refining on wax Crystallite wax product.
1-3 illustrates the method that the present invention prepares high dropping point microwax by the following examples.
Comparative example 1
This comparative example includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter The processes such as temperature-constant temperature sweating, (4) product purification.
(1) preparation
Water is padded below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected;It is sending out Sweat ware lower part installation pressure-reducing cushioning tank simultaneously connects vacuum pump;Sweating ware collet and removable coil pipe are connect with the circulatory system, it will Coil pipe is fixed on sweating ware;Using conduction oil as medium, start the heating function of the circulatory system, recycle oil is made to be warming up to 94 DEG C.
With No. 90 microwaxes (Nanyang wax Fine Chemical Works, 90.35 DEG C of fusing point;90.77 DEG C of dropping point;Oil content 1.76%) it is raw material, sweating ware is added after being heated to 94 DEG C of fusings.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, so that wax layer temperature is dropped to 91.0 DEG C and perseverance with the rate of temperature fall of 2.0 DEG C/h Warm 2.0 hours progress high temperature constant temperatures, so that crystal sufficiently increases;Drop to wax layer temperature again with the rate of temperature fall of 1.5 DEG C/h 80.0 DEG C and 1.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.Close the refrigerating function of the circulatory system.
(3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (I) is to receive under wax;The close of sweating ware top is installed Envelope system;Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware ware Normal pressure is kept below plate;Start circulation system function, so that wax layer temperature is increased to 88.0 with the heating rate of 1.5 DEG C/h ℃.Stop compressor.
It opens vacuum pump and pressure-reducing cushioning pressure inside the tank is kept to stablize on -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer Square air pressure keeps normal pressure;Wax layer temperature is set to be increased to 94.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.0 DEG C/h, so that wax Solids fraction in layer is sufficiently separated with liquid composition.Stop vacuum pump, terminates sweating effort.
Sweating ware exports changing-over crude product storage tank (I) to receive on wax;Continue increase recycle oil temperature to 110 DEG C, with Fusing is taken out on wax, as crude product (I).
(4) product purification
Crude product (I) is high dropping point crystallite wax product (I) after clay-filtered, molding, packaging.
High dropping point crystallite wax product (I) property: dropping point: 96.2 DEG C, oil content: 0.88%.Crystallite wax product (I) Yield is 14.5%(relative to raw material microwax).
Embodiment 1
The present embodiment includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter The processes such as temperature-constant temperature sweating, (4) product purification.
(1) preparation
Water is padded below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected;It is sending out Sweat ware lower part installation pressure-reducing cushioning tank simultaneously connects vacuum pump;Sweating ware collet and removable coil pipe are connect with the circulatory system, it will Coil pipe is fixed on sweating ware;Using conduction oil as medium, start the heating function of the circulatory system, recycle oil is made to be warming up to 94 DEG C.
With No. 90 microwaxes (with comparative example 1) for raw material, 94 DEG C of fusings are heated to, 0.40% azo dicyclohexyl is added Sweating ware is added in formonitrile HCN after stirring.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, so that wax layer temperature is dropped to 91.0 DEG C and perseverance with the rate of temperature fall of 2.0 DEG C/h Warm 2.0 hours progress high temperature constant temperatures, so that crystal sufficiently increases;Drop to wax layer temperature again with the rate of temperature fall of 1.5 DEG C/h 80.0 DEG C and 1.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.Close the refrigerating function of the circulatory system.
(3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (II) is to receive under wax;Sweating ware top is installed Sealing system;Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 1.2~1.4 atmospheric pressure (gauge pressure), sweating ware Normal pressure is kept below ware plate;Start circulation system function, so that wax layer temperature is increased to 88.0 with the heating rate of 1.5 DEG C/h ℃.Stop compressor.
It opens vacuum pump and pressure-reducing cushioning pressure inside the tank is kept to stablize on -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer Square air pressure keeps normal pressure;Wax layer temperature is set to be increased to 94.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.0 DEG C/h, so that wax Solids fraction in layer is sufficiently separated with liquid composition.Stop vacuum pump, terminates sweating effort.
Sweating ware exports changing-over crude product storage tank (II) to receive on wax;Continue increase recycle oil temperature to 110 DEG C, with Fusing is taken out on wax, as crude product (II).
(4) product purification
Crude product (II) is high dropping point crystallite wax product (II) after clay-filtered, molding, packaging.
High dropping point crystallite wax product (II) property: dropping point: 96.0 DEG C, oil content: 0.61%.Crystallite wax product (II) Yield be 18.6%(relative to raw material microwax).
Embodiment 2
The present embodiment includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter The processes such as temperature-constant temperature sweating, (4) product purification.
(1) preparation
Water is padded below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected;It is sending out Sweat ware lower part installation pressure-reducing cushioning tank simultaneously connects vacuum pump;Sweating ware collet and removable coil pipe are connect with the circulatory system, it will Coil pipe is fixed on sweating ware;Using conduction oil as medium, start the heating function of the circulatory system, recycle oil is made to be warming up to 94 DEG C.
With No. 90 microwaxes (with comparative example 1) for raw material, 94 DEG C of fusings are heated to, 2.50% diacetyl peroxide is added, Sweating ware is added after stirring.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
With embodiment 1.
(3) heating-constant temperature sweating
With embodiment 1.
(4) product purification
With embodiment 1.
High dropping point crystallite wax product (III) property manufactured in the present embodiment: dropping point: 95.8 DEG C, oil content: 0.65%. The yield of crystallite wax product (III) is 17.3%(relative to raw material microwax).
Embodiment 3
The present embodiment includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter Temperature-constant temperature sweating, (4) product purification.
(1) preparation
Water is padded below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected;It is sending out Sweat ware lower part installation pressure-reducing cushioning tank simultaneously connects vacuum pump;Sweating ware collet and removable coil pipe are connect with the circulatory system, it will Coil pipe is fixed on sweating ware;Using conduction oil as medium, start the heating function of the circulatory system, recycle oil is made to be warming up to 94 DEG C.
With No. 90 microwaxes (with comparative example 1) for raw material, 94 DEG C of fusings are heated to, 5.60% diacetyl peroxide is added, Sweating ware is added after stirring.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
With embodiment 1.
(3) heating-constant temperature sweating
With embodiment 1.
(4) product purification
With embodiment 1.
High dropping point crystallite wax product (IV) property manufactured in the present embodiment: dropping point: 96.3 DEG C, oil content: 0.68%.The yield of crystallite wax product (IV) is 18.2%(relative to raw material microwax).
It can be seen that the method that the present invention prepares high dropping point microwax by comparing example and embodiment, added by increasing The improvement to sweatbox such as pressure and/or vacuum facility;It is formed in wax layer using the gas that oil-soluble can decompose substance generation Evenly dispersed short space, the constant temperature stage for forcing air flow through wax layer in sweating effort, increasing cooling and temperature-rise period Deng the improvement to sweating process;It enhances the separating effect of solids fraction and liquid composition and accelerates separating rate, to make Sweating process can prepare high dropping point crystallite wax product.

Claims (13)

1. the method for preparing high dropping point microwax, including the following contents:
(1) charge: as raw material, oil-soluble is added after heating fusing can decompose the commodity microwax for being 87 DEG C~92 DEG C using dropping point The substance of gas is generated, sweatbox is packed into;The decomposable substance for generating gas of the oil-soluble is selected from organic azo chemical combination At least one of one group of substance that object, sulfonyl hydrazines compound, organic nitroso compounds, organic peroxide are constituted;
(2) it crystallizes: wax layer being cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h rate, high temperature constant temperature 0.1~4.0 is small When;5 DEG C~20 DEG C of raw material dropping point or less of cooling final temperature is cooled to 0.5 DEG C/h~2.5 DEG C/h rate again, and low Warm constant temperature 0.1~3.0 hour;The proper temperature is -1.0 DEG C of dropping point~+2.0 DEG C of dropping point of raw material microwax;
(3) sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate;Wax layer reaches predetermined temperature and after constant temperature 0.1~5.0 hour Stop sweating;Wax layer is forced air flow through in sweating effort;The predetermined temperature is lower than purpose product dropping point 2 DEG C~10 ℃;
(4) it refines: being high dropping point crystallite wax product after purification, molding, packaging on wax.
2. according to the method for claim 1, which is characterized in that the decomposable substance for generating gas of the oil-soluble adds Enter 0.01%~15.00% that amount is raw material weight.
3. according to the method for claim 2, which is characterized in that the decomposable substance for generating gas of the oil-soluble adds Enter 0.03%~8.00% that amount is raw material weight.
4. according to the method for claim 1, which is characterized in that the organic azo compound is selected from the different heptan of azo two One group of substance that nitrile, azodiisobutyronitrile, azodicarbonamide and azo diisopropyl imidazoline hydrochloride are constituted;The sulfonyl hydrazines It closes object and is selected from one group of substance that benzene sulfonyl hydrazide, unifor, 4,4 '-bis oxides (benzene sulfonyl hydrazide) are constituted;Described is organic Nitroso compound is selected from dinitrosopentamethylene tetramine and/or N, N '-dimethyl N, N '-dinitroso phthalyl Amine;The organic peroxide is selected from dibenzoyl peroxide, dilauroyl peroxide, dicetyl peroxydicarbonate isopropyl ester and peroxide Change one group of substance of two dicyclohexyl carbonates composition.
5. according to the method for claim 1, which is characterized in that the decomposable substance for generating gas of the oil-soluble is that have Machine azo-compound and/or organic peroxide.
6. according to the method for claim 1, which is characterized in that proper temperature described in step (2) is raw material microwax Dropping point~+1.0 DEG C of dropping point.
7. according to the method for claim 1, which is characterized in that cooling final temperature described in step (2) is lower than raw material 8 DEG C~15 DEG C of microwax dropping point.
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 8, which is characterized in that force air flow through wax layer use described in step (3) Increase air pressure above wax layer to realize, apply the gauge of 0.2~2.0 atmospheric pressure above wax layer, and is protected below wax layer It holds as normal pressure.
10. according to the method for claim 8, which is characterized in that forcing air flow through wax layer described in step (3) is to adopt Reduce what air pressure was realized below wax layer: air pressure keeps normal pressure above wax layer, and -0.2~-0.8 is maintained below wax layer The gauge of a atmospheric pressure.
11. 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.
12. according to the method for claim 8, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.
13. according to the method for claim 1, which is characterized in that the sweatbox is sweating ware.
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GB687235A (en) * 1950-03-24 1953-02-11 Bataafsche Petroleum Improvements in and relating to the treatment of paraffin wax
CN1144864C (en) * 2000-07-24 2004-04-07 中国石油化工股份有限公司 Production process of high-smelting point petroleum wax
CN1250650C (en) * 2003-06-11 2006-04-12 上海泰尔精蜡有限公司 Micro-mixed crystal anti-ozonant wax and its preparing process and application
CN1296461C (en) * 2004-01-19 2007-01-24 中国石油化工股份有限公司 Method for directly producing paraffin or micro crystal wax
CN105542856B (en) * 2015-12-31 2017-03-29 中科合成油技术有限公司 A kind of method that processing Fischer-Tropsch wax produces series of products

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