CN105778868B - A kind of preparation method of wax class phase-change material - Google Patents
A kind of preparation method of wax class phase-change material Download PDFInfo
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- CN105778868B CN105778868B CN201410786309.8A CN201410786309A CN105778868B CN 105778868 B CN105778868 B CN 105778868B CN 201410786309 A CN201410786309 A CN 201410786309A CN 105778868 B CN105778868 B CN 105778868B
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Abstract
The invention discloses a kind of preparation methods of wax class phase-change material.This method is uniformly paved with metallic particles on wax layer surface before the sweating effort that heats up, and wax layer is forced air flow through in heating sweating effort, liquid composition is carried out, the separating rate of solids fraction and liquid composition is accelerated, and enhances the separating effect of solids fraction and liquid composition.The present invention increases the process for forcing solids fraction and liquid composition separation, this solvent-free de-oiling method of sweating is allow to produce wax class phase-change material product on the basis of common sweating method.The method of the present invention has many advantages, such as that plant investment is low, production process is simple and operating cost is low, solvent-free pollution.
Description
Technical field
The invention belongs to special wax production technical fields, more particularly to a kind of preparation method of wax class phase-change material.
Background technique
Temperature change is not in fusing or process of setting for phase-change material (Phase Change Material, abbreviation PCM)
Greatly, the latent heat for absorbing or discharging but in the temperature range of very little is quite big, this characteristic make its constant temperature, in terms of
It is widely used.Generally phase-change material is required to have phase transition temperature appropriate and biggish latent heat of phase change.Twentieth century 80 years
Just phase-change material was applied to aerospace field and obtained good application effect by the U.S. generation, was then widely used in military affairs
Field.Late nineteen eighties, phase-change material start to be applied to civilian aspect, and some products are in US and European market sale.
According to the difference of phase transition temperature, phase-change material can be generally divided into high temperature phase change material (pcm), medium temperature phase-change material and low
Warm phase-change material.According to the difference of chemical composition, generally phase-change material can be divided into inorganic phase-changing material and organic phase change material.
According to the difference of material phase-state change during energy storage, phase-change material can be generally divided into solid-gas phase-change material, liquid-gas phase
Become material, solid-liquid phase-change material, solid-solid phase change material.Gu the most commonly used is consolidate-liquid ,-two kinds admittedly in constant temperature, thermal energy storage process
Phase-change material.Wax class phase-change material be it is common it is organic in, low temperature solid-liquid phase change material.
Pertroleum wax is crude oil by all kinds of wax products obtained after the processing of the processes such as dewaxing, de-oiling, purification and molding
General name, including atoleine, paraffin and microwax.Pertroleum wax is containing components such as n-alkane, isoparaffin and cycloalkane
Mixture.
Compared with isoparaffin and cycloalkane, the latent heat of phase change of n-alkane is big.With the increase of n-alkane chain length,
Its fusing point increases, and the fusing point of common n-alkane is -20~100 DEG C.Since the fusing point of pertroleum wax is the various components of its composition
Concentrated expression, thus can consider that the fusing point of pertroleum wax is any adjustable within the scope of -20~100 DEG C, this is exactly that pertroleum wax is used
Make the sharpest edges of phase-change material.The temperature region is also the range most often contacted in people's daily life simultaneously, and petroleum
Wax chemical property is stable, non-corrosive, free from environmental pollution, thus pertroleum wax is used as phase-change material with unrivaled advantage.
But general goods pertroleum wax contains the components such as isoparaffin and cycloalkane, and carbon number distribution is wider, when being directly used as phase-change material
Latent heat is smaller, and phase transformation section is wider.
Pertroleum wax purified must just can serve as phase-change material to improve normal paraffin content and reduce carbon number distribution width.
Common pertroleum wax separation manufacturing process mainly has distillation, sweating de-oiling, solvent deoiling etc. in terms of pertroleum wax production technology.
Distillation is to achieve the purpose that separating-purifying using the boiling point difference of different molecular weight hydro carbons, and the boiling range for reducing distillation can
It the width of product carbon distribution is effectively reduced, but is influenced less on normal paraffin content is improved, simultaneously because distillation process needs
Pertroleum wax is heated to boiling point or more, consumes a large amount of energy.
Solvent deoiling method is to reach separating-purifying using n-alkane and the different solubility of isoparaffin in a solvent
Purpose, can effectively improve the normal paraffin content in product, but the influence to carbon distribution width is little, while solvent deoiling
Investment of production equipment is big；It needs largely to use solvent in production process, recycling design needs to consume a large amount of energy；Contain in solvent
There are benzene homologues, environment can be impacted；Solvent is inflammable, be easy to cause production accident.
Sweating de-oiling method carries out separating-purifying using hydrocarbon components various in wax property with different melting points.Pertroleum wax
In molecular weight and the structure of various components Bu Tong can all make its fusing point different.When being all n-alkane, molecular weight is biggish just
The fusing point of structure alkane is higher, and the fusing point of the lesser n-alkane of molecular weight is lower；When molecular weight is identical, isoparaffin and cycloalkanes
The fusing point of hydrocarbon will be lower than n-alkane, and isomery degree more high-melting-point is lower.So sweating de-oiling can reduce product carbon point
The width of cloth can improve normal paraffin content again.
Compared with distillation separation method, since the melting temperature of various hydro carbons is far below boiling temperature, so sweating separates
The energy consumption of process is far below distillation separation；Compared with solvent fractionation method, sweating separation process does not use solvent, so sweating point
From process on environment without influence.And diaphoresis can reduce product carbon distribution width can improve normal paraffin content, institute again
With for preparing wax class phase-change material, sweating de-oiling separation process is all advantageous in production process and two aspect of properties of product.
Common sweating degreasing process mainly comprises the steps that (1) preparation: pad water is full of sweatbox with water
Ware plate lower space；(2) charge: raw material is heated to being packed into sweatbox when fusing point or more is in a liquid state；(3) decrease temperature crystalline: will be former
Material progressively cools to 10~20 DEG C of its fusing point or less with the rate of temperature fall no more than 4 DEG C/h.In cooling procedure, fusing point is highest
Component first is come out with thick fibrous crystal morphological crystal, as wax layer temperature continues to reduce, other components by fusing point by height to
Low sequence successively crystallizes and forms solid；(4) heat up sweating: after wax layer temperature reaches preset cooling final temperature, putting
Fall to pad water；Raw material is slowly heated to preset sweating final temperature again.In heating sweating effort, various components press fusing point
It is exactly Gao Rong that sequence from low to high, which is successively fused into liquid and flows out the wax layer residue (on wax) finally obtained (under wax),
The wax of point, low oil-containing；(5) crude product is collected: being continued to increase temperature after heating sweating effort, be taken out on wax with fusing, i.e.,
For crude product；(6) product purification, molding, packaging: subtractive process generallys use clay-filtered: being warming up to after crude product is melted
Predetermined temperature is added carclazyte and simultaneously filters after constant temperature was stirred to the predetermined time；It formed, packed i.e. as purpose product again.
To common sweating de-oiling method, solids fraction (wax of higher melt) and liquid composition in heating sweating effort
(oil and the wax compared with low melting point) although two class components are respectively at two kinds of phases of solid and liquid, but are also difficult to be kept completely separate.
To make the oil content of final products meet the requirements, the method for generalling use extension sweating sessions and improving sweating final temperature, but
It will lead to production cycle length in this way and product yield decline.
Common sweating de-oiling technique can produce fusing point in 40 DEG C~60 DEG C of soap wax and low melt point paraffin, be not suitable for producing
Wax product of the fusing point at 70 DEG C or more.Have experiments have shown that, common sweating de-oiling technique production fusing point in 70 DEG C or more of product,
The carbon dispersion of distribution and normal paraffin content on sweating later period wax is unrelated with yield, i.e., the carbon dispersion of distribution on wax is not with yield
Decline and decline, normal paraffin content is not also improved with the decline of yield, so common sweating separating technology is not suitable for preparing
Wax class phase-change material of the fusing point at 70 DEG C or more.Only part of the manufacturer uses sweating de-oiling technique production soap wax and low melting point at present
The common products such as paraffin.
For many years, sweating de-oiling technique has obtained some development in production equipment and process aspect, as CN89214332(is vertical
Formula square multipul sections spacer diaphoresis tank), CN98233254.8(Paraffin sweating pot), CN201320127680.4(tubular type paraffin de-oiling
Device) etc., it is improved in sweating de-oiling production equipment；A kind of high-efficient sweat pot for paraffin wax of CN91206202() in sweating de-oiling
It is improved in technique.But these improvement cannot still produce wax class phase-change material of the fusing point at 70 DEG C or more.
Compared with solvent deoiling technique, sweating de-oiling technique has small investment, production process are simple and operating cost is low etc.
Advantage；Importantly, sweating de-oiling technique is currently known for the unique solvent-free de- of commercial scale paraffin wax product
Oily method.Wax class in the today for advocating green low-carbon, environmental protection and energy saving, using sweating de-oiling technique production fusing point at 70 DEG C or more
The demand of phase-change material is more urgent.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of wax class phase-change material, specifically with
Paraffin grade wax is raw material, the proper temperature using sweatbox, on the basis of common sweating method, during cooling
Increase the high temperature constant temperature stage, and increases the constant temperature rank in cryogenic thermostat stage after cooling procedure and heating sweating effort
Section；The metallic particles of mixing is uniformly paved on wax layer surface after cooling procedure, and forces gas in heating sweating effort
Stream is carried out in liquid composition by wax layer, to accelerate the separating rate of solids fraction and liquid composition, and is enhanced
The separating effect of solids fraction and liquid composition allows this solvent-free de-oiling method of sweating de-oiling to produce fusing point at 70 DEG C
Above wax class phase-change material product.
A kind of preparation method of wax class phase-change material of the invention, including the following contents:
(1) water is padded in sweatbox；
(2) using paraffin grade wax as raw material, sweatbox is packed into after heating fusing；
(3) wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h rate, high temperature constant temperature is for a period of time；Again with
The rate of 0.5 DEG C/h~2.5 DEG C/h is cooled to 5 DEG C~20 DEG C of raw material fusing point or less of cooling final temperature, and cryogenic thermostat one
The section time；
(4) the pad water in sweatbox is discharged；Then with the heating of 0.5 DEG C/h~2.5 DEG C/h rate, wax layer reaches predetermined
Constant temperature for a period of time, then stops sweating after temperature；Wax layer is wherein forced air flow through in temperature-rise period；
(5) it collects on wax；
(6) wax class phase-change material product is obtained on wax after purification, molding, packaging.
In the preparation method of wax class phase-change material of the invention, the melting range of the paraffin grade wax is generally 60~74
DEG C, preferably fusing point range is 66~74 DEG C.
In the preparation method of wax class phase-change material of the invention, preferably after raw material decrease temperature crystalline and in heating sweating
Cheng Qian (wax layer is in solid state at this time) is crossed, is uniformly paved with 10~100 mesh, the preferably solid of 20~50 mesh on the surface of wax layer
Particle.The density of solid particle is generally higher than 4 g/cm3, can be the materials such as nonmetallic, metal and alloy, preferred density 6
~12 g/cm3Metal and alloying pellet, such as zinc, iron, copper, lead and its more stable low price metal of alloy chemical property
Material.It can choose the solid particle of two or more different densities, two kinds of adjacent solid particle materials of density
Density contrast is 1~5 g/cm3.Two or more solid particles can ratio mixing similar in parts by weight.Described herein is close
Degree refers to the density for constituting the material of solid particle, and if the density of metallic particles refers to the density of metal, and non-particulate heap is close
Degree.Solid particle can be recycled after sweating effort and is cleaned to reuse.
In the preparation method of wax class phase-change material of the invention, the sweatbox is generally sweating ware, and in wax layer
Dismountable sealing system added above and pressurizing device and/or increase vacuum plant below wax layer.The pressure air-flow
It is utilized in above wax layer to increase by wax layer and reduces pressure (air pressure) below pressure (air pressure) or wax layer, form wax layer up and down
What pressure difference was realized.The pressure difference is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to strong
Air-flow processed passes through wax layer.
Drop in the preparation method of wax class phase-change material of the invention, in the temperature-fall period before high-temperature constant temperature section
Warm rate preferably 1.5 DEG C/h~2.5 DEG C/h.
In the preparation method of wax class phase-change material of the invention, the proper temperature of the high-temperature constant temperature section of the temperature-fall period
It is -1.0 DEG C of starting paraffin fusing point~+2.0 DEG C of fusing point, preferably starting paraffin fusing point~+1.0 DEG C of fusing point.Cool process
High-temperature constant temperature section time be 0~4.0 hour, preferably 1.0~4.0 hours.
In the preparation method of wax class phase-change material of the invention, cooling of the temperature-fall period after high-temperature constant temperature section
Rate preferably 1.0 DEG C/h~2.0 DEG C/h.
In the preparation method of wax class phase-change material of the invention, the cooling final temperature is preferably starting paraffin fusing point
8 DEG C below~15 DEG C.
It in the preparation method of wax class phase-change material of the invention, is cooling to preset temperature, is increasing the constant temperature stage
So that solid crystal is more abundant.The time in the cryogenic thermostat stage for the process that cools be 0~3.0 hour, preferably 1.0~
3.0 hour.
In the preparation method of wax class phase-change material of the invention, the heating rate preferably 1.0 of the heating sweating effort
DEG C/h~2.0 DEG C/h.The predetermined temperature (i.e. final temperature) of the heating is lower than purpose product, that is, wax class phase-change material product
1 DEG C~10 DEG C of fusing point.
In the preparation method of wax class phase-change material of the invention, the heating sweating to the preset temperature for producing product
Afterwards, 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 hour, excellent
It is selected as 1.0~5.0 hours.
In method of the invention, the heating rate and rate of temperature fall 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 are controlled.Using the modes control such as water-bath or oil bath
When heating rate processed and rate of temperature fall, collet can be increased outside sweating ware, collet is connected with removable coil pipe and the circulatory system, follows
Loop system has program cooling/heating function, and the substances such as water or oil are added as circulatory mediator in the circulatory system；By coil pipe after charging
Be immersed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the preparation method of wax class phase-change material of the invention, the wax layer that forces air flow through can be in heating sweating
Process any stage is implemented, and preferably implements at heating sweating initial stage.
In the preparation method of wax class phase-change material of the invention, the wax layer that forces air flow through is utilized in wax layer
What Fang Zengjia air pressure was realized, the pressure that can such as apply above wax layer is 0.2~1.5 atmospheric pressure (gauge pressure), and below wax layer
Remain normal pressure.
In wax class phase-change material preparation method of the invention, the wax layer that forces air flow through is utilized in below wax layer
Reduce what pressure (air pressure) realized, preferably remain normal pressure above wax layer, and the pressure below wax layer be maintained -0.2~-
0.8 atmospheric pressure (gauge pressure).
Common sweating de-oiling method be separation production petroleum paraffin product is carried out using wax and oil property with different melting points, but
It is the petroleum paraffin product for fusing point at 70 DEG C or so, since the substances such as cycloalkane and isoparaffin increase in raw material, chemical group
At complexity, cause crystals upon crystallization structure more fine and compact, huge filter flow resistance power is formed to the discharge of liquid composition, this is just
Solids fraction in the common sweating effort for only leaning on gravity natural separation is caused to be difficult to be kept completely separate with liquid composition.Therefore common hair
Sweat de-oiling technique cannot produce wax class phase-change material product of the fusing point at 70 DEG C or more.
The present invention produces to allow the method for this solvent-free production pertroleum wax of sweating de-oiling to prepare wax class phase-change material
Product, by wax class phase-change material performance and the relationship of its chemical composition and the further investigation of common sweating effort, for common
It is to cause common petroleum wax product that cannot expire that carbon number distribution is wider in petroleum paraffin product chemical composition and normal paraffin content is lower
The reason of sufficient wax class phase-change material product technology requires reduces carbon number distribution width by using diaphoresis and improves N-alkanes simultaneously
Hydrocarbon content；It is difficult to separate reason with liquid composition for solids fraction in common sweating effort, by heating sweating effort
The method for carrying out liquid composition using wax layer is forced air flow through, while further preferably increasing high-temperature constant during cooling
Thermophase, and the side of solid particle is uniformly paved on wax layer surface (i.e. before heating sweating effort) after cooling process
Method improves；The cryogenic thermostat stage and the constant temperature stage after heating sweating to preset temperature for increasing the process that cools simultaneously
Etc. processes.These measures significantly reduce the width of product carbon distribution and improve normal paraffin content, enable the performance of product
Enough meet the technical requirements of wax class phase-change material.
For pertroleum wax sweating effort studies have shown that in sweating effort, liquid composition is gradually arranged along crystalline portion
Out, the case where being flowed in capillary similar to liquid.Due to the fusing point crystallization fine and compact in 70 DEG C or so of pertroleum wax
Structure can be such that the filter flow resistance power formed to liquid composition increased dramatically, this is resulted in only by the common of gravity natural separation process
Sweating method cannot produce wax class phase-change material product.
Increasing the high temperature constant temperature stage during cooling can make the crystallization of pertroleum wax bigger, be conducive to heating sweating
The discharge of liquid composition in journey.For pertroleum wax crystallization process studies have shown that its chemical composition is to determine crystal habit most
Main cause, while the condition of cooling procedure also will affect crystal habit, especially near fusing point at a temperature of cooling item
Influence of the part to crystal habit is most obvious.Fusing point in 70 DEG C or so of pertroleum wax when being cooled near fusing point, larger molecular weight
N-alkane formed crystallization and be precipitated, this partially crystallizable body can be used as the nucleus for being subsequently formed crystallization, increases high temperature at this time
The constant temperature stage can enable nucleus sufficiently to increase, and form larger sized crystal, although this larger sized crystal is not so good as
The crystallization of low melt point paraffin is coarse like that, but the crystal structure of this increase is also extremely to have to sweating stage discharge liquid composition
Benefit.
After cooling process wax layer surface be uniformly paved with solid particle simultaneously in heating sweating effort it is strong
Air-flow processed is also beneficial to the discharge of liquid composition in heating sweating effort by wax layer.It (is risen after cooling process
Before warm sweating effort), wax layer is in solid state at this time, is uniformly paved with solid particle on wax layer surface.In heating sweating effort
In, soften as wax layer temperature increases wax layer, metallic particles will be sunk since density is big with slower speed under the effect of gravity
Drop forms perforative thin channel up and down in wax layer, reduces filter flow resistance power, is conducive to the quick discharge of liquid composition.No
It is different with density and the sinking speed of the solid particle of partial size, it can be guaranteed in sweating overall process using mixed solid particle
There is the channel of more discharge liquid composition in the different height of wax layer.Wax layer is forced air flow through simultaneously, carries out liquid
Component is to enhance the separating effect of solids fraction and liquid composition.The cryogenic thermostat stage for being aided with cooling procedure again makes solid
It is the methods of more abundant that crystallization more abundant and sweating effort the constant temperature stage separates solids fraction with liquid composition, makes sweating
De-oiling technique can produce carbon number distribution narrow range and the high wax class phase-change material product of normal paraffin content.
The invention has the advantages that the method for carrying out liquid composition using wax layer is forced air flow through, accelerates solid-state group
Divide the separating rate with liquid composition.And by settling hybrid solid particle in heating sweating effort, the upper and lower of formation is passed through
The thin channel for wearing wax layer is more favorable to the quick discharge of oil.The separation for thus enhancing solids fraction and liquid composition is imitated
Fruit.So that sweating de-oiling technique can produce, carbon number distribution range is relatively narrow and the higher pertroleum wax of normal paraffin content produces
Product, these products may be used as wax class phase-change material.The method of the present invention plant investment is low, production process is simple and operating cost
Low, solvent-free pollution environment.
Specific embodiment
Sweating ware top connects dismountable sealing device and connect with surge tank and compressor, and/or under sweating ware
Portion connects surge tank and vacuum pump；Increase collet outside sweating ware, collet is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function；The paraffin for being suitable for using fusing point is packed into sweating ware after heating fusing, coil pipe is submerged as raw material
It is in the feed and fixed；It is simultaneously permanent near wax layer temperature to raw material melting temperature to reduce that cryogenic media is passed through in collet and coil pipe
Warm a period of time；Hybrid solid particle is uniformly paved on wax layer surface；Heat cycles medium improves wax layer temperature；Connection sealing dress
It sets and starts compressor in wax layer positive pressure formed above, and/or starting vacuum pump is in wax layer negative pressure formed below, to strong
Air-flow processed passes through wax layer；Wax layer temperature reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time.On wax through purification, at
It is wax class phase-change material product after type, packaging.
1-2 illustrates the preparation method of wax class phase-change material of the present invention by the following examples.
Embodiment 1
The present embodiment includes: (1) preparation, (2) charging, (3) cooling-high temperature constant temperature-cooling-cryogenic thermostat knot
Crystalline substance, (4) heating-constant temperature sweating, (5) crude product collect, (6) product purification and molding, packaging etc. processes.
(1) preparation
The sealing system on sweating ware top is connected with surge tank and compressor.Surge tank is installed simultaneously in sweating ware lower part
Connect vacuum pump.
Pad water in sweating ware ware plate lower part.
The collet of sweating ware is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with water
For heat-conducting medium.
The heating function for starting the circulatory system, makes water-cycling-media be warming up to 78 DEG C.
(2) it charges
With No. 72 semi-refined waxs (Dalian Petrochemical Industry Company's production, property are as follows: 72.50 DEG C of fusing point；Oil content 0.66%；N-alkanes
Hydrocarbon content 68.25%) it is raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and is fixed.
(3) 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 73.0 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 crystallization sufficiently increases；Drop to wax layer temperature again with the rate of temperature fall of 1.5 DEG C/h
62.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.
Close the refrigerating function of the circulatory system.
(4) heating-constant temperature sweating
Sweating ware is discharged and pads water.
Storage tank under sweating ware outlet connection wax；Connect sweating ware sealing device for upper portion of annular；Starting compressor simultaneously keeps surge tank
Interior pressure is stablized keeps normal pressure below 1.0~1.2 atmospheric pressure (gauge pressure), sweating ware ware plate；Start circulation system function
Can, so that wax layer temperature is increased to 72.0 DEG C with the heating rate of 1.5 DEG C/h.
Stop compressor.Remove sealing device.
It opens vacuum pump and buffering pressure inside the tank is kept to stablize and protected above -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer
Hold normal pressure；Wax layer temperature is set to be increased to 75.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.5 DEG C/h so that solid-state in wax layer
Component is sufficiently separated with liquid composition.
Stop vacuum pump, terminates sweating degreasing process.
(5) crude product is collected
Sweating ware exports changing-over crude product storage tank (I) to receive on wax；Continue the temperature of raising recirculated water to 90 DEG C, with molten
Change and take out on wax, as crude product.
(6) product purification and molding, packaging
Crude product is wax class phase-change material product (I) after clay-filtered, molding and packaging.
Wax class phase-change material product (I) property:
Fusing point (DSC method): 77.51 DEG C；Latent heat of phase change: 218.52J/g；Normal paraffin content 81.47%.
The yield of wax class phase-change material product (I) is 14.6%(relative to raw material 72# semi-refined wax).
Embodiment 2
The present embodiment includes: (1) preparation, (2) charging, (3) cooling-high temperature constant temperature-cooling-cryogenic thermostat knot
Crystalline substance, (4) heating-constant temperature sweating, (5) crude product is collected and metallic particles recycling, (6) product purification and molding, packaging waited
Journey.
(1) preparation
20 mesh~40 mesh lead particle and zinc particle are screened out, is uniformly mixed by weight for 1:1.
The sealing system on sweating ware top is connected with surge tank and compressor.Surge tank is installed simultaneously in sweating ware lower part
Connect vacuum pump.
Pad water in sweating ware ware plate lower part；The double-deck Medium speed filter paper is spread in sweating ware bottom.
The circulatory system of the sweating ware of jacketed with removable coil pipe and with program refrigerating/heating function is connected, with water
For heat-conducting medium.
The heating function for starting the circulatory system, makes water-cycling-media be warming up to 78 DEG C.
(2) it charges
With No. 72 semi-refined waxs (property is with embodiment 1) for raw material, the sweating ware that filter paper is completed in bottom is added after heating fusing.
Coil pipe is immersed in raw material wax layer and is fixed.
(3) 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 73.0 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 crystallization sufficiently increases；Drop to wax layer temperature again with the rate of temperature fall of 1.5 DEG C/h
62.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature, so that crystallization is more abundant.
Close the refrigerating function of the circulatory system.
(4) heating-constant temperature sweating
Lead above-mentioned, zinc hybrid particles are uniformly paved on wax layer surface.
Sweating ware is discharged and pads water.
Storage tank under sweating ware outlet connection wax；Connect sweating ware sealing device for upper portion of annular；Starting compressor simultaneously keeps surge tank
Interior pressure is stablized keeps normal pressure below 1.0~1.2 atmospheric pressure (gauge pressure), sweating ware ware plate；Start circulation system function
Can, so that wax layer temperature is increased to 72.0 DEG C with the heating rate of 1.5 DEG C/h.
Stop compressor.Remove sealing device.
It opens vacuum pump and buffering pressure inside the tank is kept to stablize and kept above -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer
Normal pressure；Wax layer temperature is set to be increased to 75.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.5 DEG C/h so that solid-state group in wax layer
Divide and is sufficiently separated with liquid composition.
Stop vacuum pump, terminates sweating degreasing process.
(5) crude product is collected and metallic particles recycles
Sweating ware exports changing-over crude product storage tank (II) to receive on wax；Continue increase recirculated water temperature to 90 DEG C, with
Fusing is taken out on wax, as crude product.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
(6) product purification and molding, packaging
Crude product is product (II) after clay-filtered, molding and packaging.
Wax class phase-change material product (II) property:
Fusing point (DSC method): 78.23 DEG C；Latent heat of phase change: 230.15J/g；Normal paraffin content 86.35%.
The yield of wax class phase-change material product (II) is 14.2%(relative to raw material 72# semi-refined wax).
The preparation method that can be seen that wax class phase-change material of the present invention by embodiment 1-2, by using on wax layer surface
Metallic particles is spread to form the tiny duct for running through wax layer up and down in sweating effort, and force air-flow in heating sweating effort
By the method for wax layer, the separating effect of solids fraction and liquid composition is enhanced, it is this solvent-free that sweating de-oiling can be used
Production paraffin method prepare fusing point 70 DEG C or more, latent heat of phase change 210J/g or more wax class phase-change material product.
Claims (19)
1. a kind of preparation method of wax class phase-change material, including the following contents:
(1) water is padded in sweatbox；
(2) using paraffin grade wax as raw material, sweatbox is packed into after heating fusing；The fusing point of the paraffin grade wax is 60~74 DEG C；
(3) wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h rate, high temperature constant temperature is for a period of time；Again with 0.5
DEG C/h~2.5 DEG C/h rate is cooled to 5 DEG C~20 DEG C of raw material fusing point or less of cooling final temperature, and at one section of cryogenic thermostat
Between；The proper temperature is -1.0 DEG C of starting paraffin fusing point~+2.0 DEG C of fusing point；
(4) the pad water in sweatbox is discharged；Then with the heating of 0.5 DEG C/h~2.5 DEG C/h rate, wax layer reaches predetermined temperature
Constant temperature for a period of time, then stops sweating afterwards；Wax layer is wherein forced air flow through in temperature-rise period；
(5) it collects on wax；
(6) wax class phase-change material product is obtained on wax after purification, molding, packaging；
Wherein, equal on the surface of wax layer in step (3) after raw material decrease temperature crystalline, and before step (4) heat up sweating effort
The even solid particle for being paved with 10~100 mesh.
2. according to the method for claim 1, which is characterized in that the fusing point of the paraffin grade wax is 66~74 DEG C.
3. according to the method for claim 1, which is characterized in that the proper temperature be starting paraffin fusing point~fusing point+
1.0℃。
4. according to the method for claim 1, which is characterized in that the mesh number of the solid particle is 20~50 mesh.
5. according to the method described in claim 1, which is characterized in that the density of the solid particle is greater than 4 g/cm3。
6. according to the method for claim 5, which is characterized in that the density of the solid particle is 6~12 g/cm3。
7. according to the method for claim 5, which is characterized in that the solid particle is selected from zinc, iron, copper, lead and its conjunction
One or more of gold.
8. according to the method for claim 7, which is characterized in that the solid particle selects two or more different densities
Solid particle, the density contrasts of two kinds of adjacent solid particle materials of density is 1~5 g/cm3。
9. according to the method for claim 1, which is characterized in that the wax layer that forces air flow through is utilized in wax layer
Air pressure is reduced below Fang Zengjia air pressure and/or wax layer, so that wax layer is formed what pressure difference was realized up and down, the pressure difference is 0.1
~5.0 atmospheric pressure.
10. according to the method for claim 9, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.
11. according to the method for claim 1, which is characterized in that temperature-fall period described in step (3) high-temperature constant temperature section it
Preceding rate of temperature fall be 1.5 DEG C/h~2.5 DEG C/h, and the rate of temperature fall after high-temperature constant temperature section be 1.0 DEG C/h~2.0 DEG C/
h。
12. according to the method for claim 1, which is characterized in that the time of high temperature constant temperature described in step (3) be 1.0~
4.0 hour.
13. according to the method for claim 1, which is characterized in that cooling final temperature described in step (3) is starting paraffin
8 DEG C~15 DEG C below fusing point.
14. according to the method for claim 1, which is characterized in that the time of cryogenic thermostat described in step (3) be 1.0~
3.0 hour.
15. according to the method for claim 1, which is characterized in that heating rate described in step (4) be 1.0 DEG C/h~
2.0℃/h。
16. according to the method for claim 1, which is characterized in that the predetermined temperature to heat up in step (4) is to produce lower than purpose
1 DEG C~10 DEG C of the fusing point of product.
17. according to the method for claim 1, which is characterized in that the time of constant temperature described in step (4) is 1.0~5.0 small
When.
18. according to the method for claim 9, which is characterized in that the wax layer that forces air flow through is utilized in wax layer
Top increases what air pressure was realized: applying the gauge of 0.2~1.5 atmospheric pressure above wax layer, and remains below wax layer
Normal pressure.
19. according to the method for claim 9, which is characterized in that the wax layer that forces air flow through is utilized in wax layer
Lower section reduces what pressure was realized: normal pressure is kept above wax layer, and the gauge below wax layer is maintained -0.2~-0.8
A atmospheric pressure.
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|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1189527A (en) * | 1997-01-27 | 1998-08-05 | 王福祥 | Quick sweating wax making tech. |
| CN1458242A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Waxy temperature sensing medium for automatic temperature regulating valve of showering |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
| CN103773427A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Method for preparing liquid wax |
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- 2014-12-18 CN CN201410786309.8A patent/CN105778868B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1189527A (en) * | 1997-01-27 | 1998-08-05 | 王福祥 | Quick sweating wax making tech. |
| CN1458242A (en) * | 2002-05-15 | 2003-11-26 | 中国石油化工股份有限公司 | Waxy temperature sensing medium for automatic temperature regulating valve of showering |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
| CN103773427A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Method for preparing liquid wax |
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