CN105754659B - A kind of preparation method of high melting point paraffin - Google Patents

A kind of preparation method of high melting point paraffin Download PDF

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Publication number
CN105754659B
CN105754659B CN201410786124.7A CN201410786124A CN105754659B CN 105754659 B CN105754659 B CN 105754659B CN 201410786124 A CN201410786124 A CN 201410786124A CN 105754659 B CN105754659 B CN 105754659B
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wax
wax layer
sweating
accordance
solid particle
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CN105754659A (en
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孙剑锋
张造根
王士新
张志银
张晓晖
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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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Abstract

The invention discloses a kind of preparation method of high melting point paraffin.This method is uniformly paved with metallic particles before heating sweating effort on wax layer surface, and forces air flow through wax layer in heating sweating effort, carries out the oil in liquid, accelerates the separating rate of wax and oil, and enhances the separating effect of wax and oil.The present invention is on the basis of common sweating method, and the process of wax and oil separation is forced in increase, this solvent-free de-oiling method of sweating is produced high melting point paraffin product.The inventive method has the advantages that plant investment is low, production process is simple and operating cost is low, solvent-free pollution.

Description

A kind of preparation method of high melting point paraffin
Technical field
The invention belongs to pertroleum wax production technical field, more particularly to a kind of preparation method of high melting point paraffin.
Background technology
The general name of the pertroleum wax obtained all kinds of wax products that are crude oil after refining processing from wax-containing distillate, including liquid Body paraffin, paraffin and microwax.Paraffin is that lube cut is produced through steps such as dewaxing, de-oiling, refined and shapings in crude oil, Typically contain C20~C30The component such as n-alkane, a small amount of isoparaffin and cycloalkane, usual fusing point is 50 DEG C~74 DEG C.
Dewaxing is the process that the slack wax that oil content is 10~30% or so is prepared by raw material of lube cut, dewaxing technique Mainly there is squeezing to dewax and solvent dewaxing.De-oiling is the process that scale wax of the oil content below 2% is prepared by raw material of slack wax, is taken off Oily technique mainly has sweating de-oiling and solvent deoiling.Scale wax again through clay-filtered or hydrofinishing and shaping, packaging and other steps, Both paraffin grade wax product had been can obtain.
Solvent deoiling process is in selective solvent(Acetone, benzene and toluene mixture;Or acetone, toluene;Or MEK, Toluene)Solution in freeze, the methods production paraffin wax products separated according to the difference of wax and oil solubility.Solvent deoiling Technique has the advantages that production is continuous, wax high income, finished product wax oil content can very low, production cost it is relatively low, be big rule at present Mould produces the main flow de-oiling technique of paraffin wax product.But solvent deoiling investment of production equipment is big;Need largely to use in production process Solvent, recycling design needs to consume substantial amounts of energy;Contain benzene homologues in solvent, environment can be impacted;Solvent is inflammable, holds Easily cause production accident.
Sweating de-oiling method is separated using the wax property different with oily fusing point.Point of various components in pertroleum wax Son amount Bu Tong can all make its fusing point different with structure.When being all n-alkane structure, the larger n-alkane of molecular weight it is molten Point is higher, and the fusing point of the less n-alkane of molecular weight is relatively low;When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will Less than n-alkane, and isomery degree more high-melting-point is lower, or even is in just liquid condition at normal temperatures, i.e., usually said Oil.Sweating de-oiling method in process of production without using only needed in solvent, and production process by raw material be heated to fusing point with On temperature.
Common sweating degreasing process is mainly included the following steps that:(1)Preparation:Water is padded, sweatbox is full of with water Ware plate lower space;(2)Charging:Load sweatbox when raw material is heated to more than fusing point being in a liquid state;(3)Decrease temperature crystalline:By original Material progressively cools to below its fusing point 10~20 DEG C to be not more than 4 DEG C/h rate of temperature fall.In cooling procedure, various components are pressed The order of fusing point from high to low crystallizes to form solid successively;(4)Heat up sweating:When wax layer temperature reaches that default cooling terminates temperature After degree, pad water is bled off;Raw material is slowly heated to default sweating final temperature again.It is various in heating sweating effort Component is successively fused into liquid by the order of fusing point from low to high and flowed out(Under wax), the wax layer residue finally obtained(On wax) It is exactly high-melting-point, the wax of low oil-containing;(5)Crude product is collected:Heating sweating effort terminates follow-up high-temperature of continuing rising, to melt taking-up On wax, as crude product;(6)Product purification, shaping, packaging:Subtractive process is generally using clay-filtered:After crude product is melted Predetermined temperature is warming up to, carclazyte is added and constant temperature stirs to the scheduled time filtering;It is again purpose product through shaping, packaging.
To common sweating de-oiling method, although wax and oily two classes component are respectively at solid and liquid in heating sweating effort Body state, but also be difficult to be kept completely separate.To make the oil content of final products meet the requirements, generally using extension sweating sessions simultaneously The method for improving sweating final temperature.Extension sweating sessions can cause the production cycle long;Part can be made by improving sweating final temperature Wax is removed with oil, causes product yield to decline.
Common sweating de-oiling technique can produce soap wax and low melt point paraffin of the fusing point at 40 DEG C~60 DEG C, be not suitable for production High melting point paraffin product of the fusing point at 70 DEG C or so.There is experiment to show, common sweating de-oiling technique productions fusing point is at 70 DEG C or so High melting point paraffin product when, even if using extension sweating sessions and the method that improves sweating final temperature, on sweating later stage wax Oil content it is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, so common sweating de-oiling technique is not Suitable for producing fusing point meets semi-refined or full refining product standard high melting point paraffin product, especially oil-containing at 70 DEG C or so Figureofmerit can not meet technical requirement.Only part producer uses sweating de-oiling technique productions soap wax and low melting point at present Paraffin wax product.
For many years, sweating de-oiling technique has obtained some development, such as CN89214332 in production equipment and process aspect(It is vertical Formula square multipul sections spacer diaphoresis tank)、CN98233254.8(Paraffin sweating pot)、CN201320127680.4(Tubular type paraffin de-oiling Device)Deng being improved in sweating de-oiling production equipment;CN91206202(A kind of high-efficient sweat pot for paraffin wax)In sweating de-oiling Improved in technique.But these improvement, which can not still be produced, meets semi-refined or full refining product standard high melting point paraffin production Product.
Compared with solvent deoiling technique, sweating de-oiling technique has that small investment, production process are simple and operating cost is low Advantage;Importantly, sweating de-oiling technique is currently known for the unique solvent-free de- of commercial scale paraffin wax product Oily method.In promotion green low-carbon, today of environmental protection and energy saving, using the demand of sweating de-oiling technique productions high melting point paraffin product It is more urgent.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of production method of high melting point paraffin, specifically uses Sweatbox, on the basis of common sweating method, solid particle is uniformly paved with before heating sweating effort on wax layer surface, and Wax layer is forced air flow through in heating sweating effort, the oil in liquid is carried out, the separating effect of wax and oil is enhanced, from And can be using this solvent-free de-oiling method production high melting point paraffin product of sweating de-oiling.The inventive method has plant investment Low, production process is simple and operating cost is low, solvent-free pollution the advantages of.
A kind of preparation method of high melting point paraffin of the present invention, including herein below:
(1)Water is padded in sweatbox;
(2)Using slack wax of the oil content less than 30% as raw material, load sweatbox after heating fusing;
(3)10 DEG C~20 DEG C are cooled to below slack wax fusing point with 1.0 DEG C/h~4.0 DEG C/h speed;
(4)The pad water in sweatbox is discharged, is then heated up with 0.5 DEG C/h~3.0 DEG C/h speed;In temperature-rise period Force air flow through wax layer;Wax layer, which reaches, stops sweating after predetermined temperature;
(5)Collect on wax;
(6)After refined, shaping it is purpose product on wax.
In high melting point paraffin preparation method of the present invention, the oil content of described slack wax is less than 30%, its fusing point model in mass Enclose generally 55 DEG C~70 DEG C.Slack wax raw material can be the line that subtracts three or the line distillate that subtracts four through the obtained slack wax of dewaxing.
In high melting point paraffin preparation method of the present invention, preferably in step(3)After middle raw material decrease temperature crystalline and in step (4)Before heating sweating effort(Now wax layer is in solid state), 10~100 mesh, preferably 20 are uniformly paved with the surface of wax layer The solid particle of~50 mesh.The material density of solid particle is generally higher than 4 g/cm3, can be nonmetallic, metal and alloy etc. Material, preferably material density are 6~12 g/cm3Metal and alloying pellet, such as zinc, iron, copper, lead and its alloy are chemically The more stable low price metal material of matter.The solid particle of two or more unlike material density can be selected, it is various Solid particle can ratio mixing close by weight.In two or more solid particles, two kinds of adjacent solid particles of density The density contrast of material is 1~5 g/cm3.Density described herein refers to the density for constituting the material of solid particle, and non-solid The heap density of particle.Sweating effort can reclaim solid particle and clean to reuse after terminating.
In high melting point paraffin preparation method of the present invention, described sweatbox is generally sweating ware, and increases more than wax layer Plus dismountable sealing system and pressue device and/or increase vacuum plant below wax layer.It is to adopt to force air flow through wax layer Apply pressure above wax layer(Air pressure)And/or pressure is reduced below wax layer(Air pressure), make to form pressure differential above and below wax layer Realize.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force air-flow Pass through wax layer.
In high melting point paraffin preparation method of the present invention, step(3)Described in cool speed preferably 1.5 DEG C/h~2.5 DEG C/ h。
In high melting point paraffin preparation method of the present invention, 12 DEG C~15 below the preferred slack wax fusing point of described cooling final temperature ℃。
High melting point paraffin preparation method of the present invention, described heating rate preferably 1.0 DEG C/h~2.0 DEG C/h.What is heated up is pre- Constant temperature degree(That is final temperature)For less than 2 DEG C~10 DEG C of purpose product fusing point.
In the method for the present 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., can be when controlling heating rate and rate of temperature fall using modes such as water-bath or oil baths Increase chuck outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system have program cool/heat work( Can, the circulatory system adds the material such as water or oil and is used as circulatory mediator;Coil pipe is immersed in wax layer after charging, can make wax layer liter/ Temperature-fall period faster, wax layer more uniform temperature.
In the high melting point paraffin preparation method of the present invention, the described wax layer that forces air flow through can be in heating sweating effort Any stage is implemented, and preferably implements initial stage in heating sweating.
In the high melting point paraffin preparation method of the present invention, the described wax layer that forces air flow through is utilized in increasing above wax layer What plus-pressure was realized, the pressure preferably applied above wax layer(Air pressure)For 0.2~2.0 atmospheric pressure(Gauge pressure), and below wax layer Remain normal pressure.
In the high melting point paraffin preparation method of the present invention, the described wax layer that forces air flow through is utilized in drop below wax layer What low-pressure was realized, preferably remain normal pressure above wax layer, and the pressure below wax layer(Air pressure)It is maintained -0.2~-0.8 Individual atmospheric pressure(Gauge pressure).
In the high melting point paraffin preparation method of the present invention, in addition to herein below:In step(4)Or(5)Middle collection part Product under wax, and by carry out circulation sweating, the lower slightly high melting point paraffin product of fusing point can be produced.
Sweating de-oiling method is to separate to produce paraffin wax product using the wax property progress different with oily fusing point, but for High melting point paraffin product of the fusing point at 70 DEG C or so, because chemical composition is more complicated, causes crystals upon crystallization structure more refinement Small densification, the discharge to fluid oil forms huge filter flow resistance power, and this results in the common sweating for only leaning on gravity natural separation Wax and oil are difficult to be kept completely separate in journey.Therefore can not to produce fusing point semi-refined in 70 DEG C or so meet for common sweating de-oiling technique Or the high melting point paraffin product of full refining product standard.
The present invention is in order that the method for this solvent-free production paraffin of sweating de-oiling is applied to prepare fusing point at 70 DEG C or so High melting point paraffin product, by the further investigation to common sweating effort, be difficult to separate reason for wax and oil, by rising Using the method that wax layer carries out fluid oil is forced air flow through in warm sweating effort, the separating effect of wax and oil is enhanced;Together When further preferably after the process of cooling terminates(I.e. before heating sweating effort), now wax layer is in solid state, in wax layer table The method that face is uniformly paved with solid particle is improved.In heating sweating effort, as wax layer temperature is raised, wax layer softens, Because the density of solid particle is big, it by with slower velocity sedimentation, runs through in wax layer above and below formation under gravity Thin channel, reduces filter flow resistance power, is conducive to the quick discharge of oil.The sedimentation speed of the solid particle of different densities and particle diameter Degree is different, can ensure that the different height in wax layer in the overall process of sweating de-oiling has more using the solid particle of mixing Discharge fluid oil passage.Wax layer is forced air flow through simultaneously, the oil of liquid is carried out, so as to enhance the separation of wax and oil Effect, allows sweating de-oiling technique to produce high melting point paraffin product.
It is an advantage of the invention that:By carrying out fluid oil using forcing air flow through wax layer in heating sweating effort Method, accelerates the separating rate of wax and oil, enhances the separating effect of wax and oil;Formed simultaneously during solid particles sediment Up and down run through wax layer tiny duct, be more favorable to fluid oil and quickly discharge.So that this solvent-free life of sweating de-oiling Production. art can produce high melting point paraffin product.The inventive method plant investment is low, production process is simple and operating cost is low, nothing Solvent contamination environment.
Embodiment
Sweating ware top connects dismountable sealing device and is connected with surge tank and compressor, and/or under sweating ware Portion connects surge tank and vavuum pump;Increase chuck outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system With program refrigerating/heating function;Using slack wax as raw material, load sweating ware after heating fusing, coil pipe is submerged in the feed simultaneously It is fixed;Wax layer heating-cooling speed is controlled with water-bath;Before heating sweating effort, preferably mixing is uniformly paved with wax layer surface Solid particle;Use above wax layer formation malleation in heating sweating effort and/or in wax layer negative pressure formed below to force Air-flow is carried out in fluid oil by wax layer, and wax layer temperature, which reaches, stops sweating after preset temperature.
1-3 illustrates the preparation method of high melting point paraffin of the present invention by the following examples.
Embodiment 1
The present embodiment includes:(1)Preparation,(2)Charging,(3)Decrease temperature crystalline,(4)Heating sweating,(5)Crude product is received Collection,(6)The process such as product purification and shaping, packaging.
(1)Preparation
The sealing system on sweating ware top and surge tank and compressor are connected.
Pad water below sweating ware ware plate.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with water For medium;Start circulation system function, heat cycles water is to 65 DEG C.
(2)Charging
With the Daqing crude oil line slack wax that subtracts four(The line slack wax property that subtracts four:Initial boiling point:410 DEG C, 90% distillate a little:520℃;Fusing point 58.5℃;Oil content 26.9%)For raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and fixed.
(3)Decrease temperature crystalline
Start the refrigerating function of the circulatory system, wax layer temperature drop is made wax to 45.0 DEG C with 2.0 DEG C/h rate of temperature fall Layer crystallization;Close the refrigerating function of the circulatory system.
(4)Heat up sweating
Discharge sweating ware pad water.
Connect sweating ware sealing device for upper portion of annular;Storage tank under sweating ware outlet connection wax;Start compressor and keep surge tank Interior pressure stability is in 1.3~1.5 atmospheric pressure(Gauge pressure), sweating ware ware plate lower section keeps normal pressure;Start circulation system work( Can, wax layer temperature is increased to 70.0 DEG C with 2.0 DEG C/h heating rate.
Stop compressor, terminate sweating degreasing process.
(5)Crude product is collected
The outlet of sweating ware is changed to connection crude product storage tank to receive on wax;Continue elevation system temperature to 90 DEG C, to melt Take out on wax, as high melting point paraffin crude product.
(6)Product purification and shaping, packaging
Crude product is high melting point paraffin product after clay-filtered, shaping, packaging(Ⅰ).
High melting point paraffin product(Ⅰ)Property:
Fusing point:72.3 DEG C, oil content:0.78%.Meet the associated specifications of commodity 72# fully refined paraffin wax.
72# fully refined paraffin wax total yield of products is 10.8%(Relative to slack wax raw material).
Embodiment 2
The present embodiment includes:(1)Preparation,(2)Charging,(3)Decrease temperature crystalline,(4)Heating sweating,(5)Crude product is received Collection and metallic particles reclaim,(6)The process such as product purification and shaping, packaging.
(1)Preparation
The lead particle and zinc particle of the mesh of 20 mesh~40 are screened out, by weight being 1:1 is well mixed.
The sealing system on sweating ware top and surge tank and compressor are connected.
Sweating ware ware plate bottom pad water;Double-deck Medium speed filter paper is spread in sweating ware bottom.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, with water For medium;Start circulation system function, heat cycles water is to 65 DEG C.
(2)Charging
With the Daqing crude oil line slack wax that subtracts four(Property be the same as Example 1)For raw material, add bottom after heating fusing and complete filter paper Sweating ware.Coil pipe is immersed in raw material wax layer and fixed.
(3)Decrease temperature crystalline
Start the refrigerating function of the circulatory system, wax layer temperature drop is made wax to 45.0 DEG C with 2.0 DEG C/h rate of temperature fall Layer crystallization;Close the refrigerating function of the circulatory system.
(4)Heat up sweating
Foregoing lead, zinc hybrid particles are uniformly paved with wax layer surface;
Discharge sweating ware pad water.
Connect sweating ware sealing device for upper portion of annular;Under one wax of sweating ware outlet connection(Effluent under Part I wax, similarly hereinafter) Storage tank;Start compressor and keep buffering pressure inside the tank stable in 1.3~1.5 atmospheric pressure(Gauge pressure), sweating ware ware plate lower section Keep normal pressure;Start circulation system function, wax layer temperature is increased to 60.0 DEG C with 2.0 DEG C/h heating rate.
Storage tank under the sweating ware outlet wax of changing-over two;Keep buffering pressure inside the tank stable in 1.3~1.5 atmospheric pressure(Table Pressure), sweating ware ware plate lower section keeps normal pressure;Wax layer temperature is set to be increased to 65.0 DEG C with 2.0 DEG C/h heating rate.
Storage tank under the sweating ware outlet wax of changing-over three;Keep buffering pressure inside the tank stable in 1.3~1.5 atmospheric pressure(Table Pressure), sweating ware ware plate lower section keeps normal pressure;Wax layer temperature is set to be increased to 70.0 DEG C with 1.0 DEG C/h heating rate.
Stop compressor, terminate sweating degreasing process.
(5)Crude product is collected and mixed metal particles are reclaimed
The outlet of sweating ware is changed to connection crude product storage tank to receive on wax;Continue elevation system temperature to 90 DEG C, to melt Take out on wax, as high melting point paraffin crude product.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
(6)Product purification and shaping, packaging
Crude product is high melting point paraffin product after clay-filtered, shaping, packaging(Ⅱ).
High melting point paraffin product(Ⅱ)Property:
Fusing point:72.8 DEG C, oil content:0.53%.Meet the associated specifications of commodity 72# fully refined paraffin wax.
72# fully refined paraffin wax total yield of products is 12.6%(Relative to slack wax raw material).
Embodiment 3
The present embodiment includes:(1)Preparation,(2)Charging,(3)Decrease temperature crystalline,(4)Heating sweating,(5)Crude product is received Collection and mixed metal particles reclaim,(6)The process such as product purification and shaping, packaging.
(1)Preparation
By under two waxes in embodiment 2(59.5 DEG C of fusing point;Oil content 22.4%)Under three waxes(66.4 DEG C of fusing point;Oil-containing Amount 12.1%)Mix and through clay-filtered, mixture as the present embodiment raw material.
Surge tank is installed in sweating ware bottom and vavuum pump is connected.
The copper particle and iron particle of the mesh of 30 mesh~50 are screened out, by weight being 1:1 is well mixed.
The sweating ware of jacketed is connected with removable coil pipe with the circulatory system with program refrigerating/heating function, starts Circulation system function, heat cycles water is to 70 DEG C.
Sweating ware ware plate bottom pad water;Double-deck Medium speed filter paper is spread in sweating ware bottom.
(2)Charging
With mixture material under foregoing two refined waxes and under three waxes, add bottom after heating fusing and complete the sweating of filter paper Ware.Coil pipe is placed in raw material wax layer and fixed;Coil pipe, chuck and the circulatory system are connected.
(3)Decrease temperature crystalline
Using water as heat-conducting medium, start the refrigerating function of the circulatory system, at a temperature of making wax layer with 2.0 DEG C/h rate of temperature fall It is down to 50.0 DEG C.
Foregoing copper, iron hybrid particles are uniformly paved with wax layer surface;Close the refrigerating function of the circulatory system.
(4)Heat up sweating
Discharge sweating ware pad water.
Storage tank under sweating ware outlet connection wax;Start vavuum pump and keep buffering pressure inside the tank stable at -0.4~-0.6 Atmospheric pressure(Gauge pressure), wax layer top keeps normal pressure;Start circulation system function, wax layer is made with 1.5 DEG C/h heating rate Temperature is increased to 68.0 DEG C of progress sweating de-oilings.
Stop vavuum pump, terminate sweating effort.
(5)Crude product is collected and metallic particles is reclaimed
The outlet of sweating ware is changed to connection crude product storage tank to receive on wax;Continue to raise circulatory system temperature to 90 DEG C, with Fusing is taken out on wax, as purpose product crude product.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
(6)Product purification and shaping, packaging
Crude product is high melting point paraffin product after clay-filtered, shaping and packaging(Ⅲ).
High melting point paraffin product(Ⅲ)Property:
Fusing point:70.3 DEG C, oil content:0.90%.Meet the associated specifications of commodity 70# semi-refined paraffin waxs.
The product yield of 70# semi-refined paraffin waxs is 3.7%(Relative to crude oil slack wax).
The production method of high melting point paraffin of the present invention is can be seen that by embodiment 1-3, is spread by using on wax layer surface Metallic particles forces air-flow to lead to run through the tiny duct of wax layer above and below being formed in sweating effort in heating sweating effort The method for crossing wax layer, enhances the separating effect of wax and oil, the method that can use this solvent-free production paraffin of sweating de-oiling Prepare high melting point paraffin product.

Claims (19)

1. a kind of preparation method of high melting point paraffin, including herein below:
(1)Water is padded in sweatbox;
(2)30%, slack wax that fusing point is 55 DEG C~70 DEG C is less than as raw material using oil content, loads sweatbox after heating fusing;
(3)10 DEG C~20 DEG C are cooled to below slack wax fusing point with 1.0 DEG C/h~4.0 DEG C/h speed;
(4)The pad water in sweatbox is discharged, is then heated up with 0.5 DEG C/h~3.0 DEG C/h speed;Forced in temperature-rise period Air-flow passes through wax layer;Wax layer, which reaches, stops sweating after predetermined temperature;
(5)Collect on wax;
(6)After refined, shaping it is purpose product on wax;
Wherein, in step(3)After middle raw material slack wax decrease temperature crystalline and in step(4)Before middle heating sweating effort, in wax layer table Face is uniformly paved with the solid particle of 10~100 mesh.
2. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer Fang Zeng great air pressure and/or air pressure is reduced below wax layer, make to form what pressure differential was realized above and below wax layer, described pressure differential is 0.1~5.0 atmospheric pressure.
3. in accordance with the method for claim 1, it is characterised in that the mesh number of the solid particle is 20~50 mesh.
4. according to the method described in claim 1 or 3, it is characterised in that the material density of the solid particle is more than 4 g/cm3
5. in accordance with the method for claim 1, it is characterised in that methods described also includes herein below:Sweating effort terminates Solid particle is reclaimed afterwards and cleans to reuse.
6. in accordance with the method for claim 4, it is characterised in that the material of the solid particle be zinc, iron, copper, lead and its One or more in alloy.
7. in accordance with the method for claim 4, it is characterised in that described solid particle selects two or more unlike materials The solid particle of density.
8. in accordance with the method for claim 7, it is characterised in that two kinds of adjacent solids of two or more solid particle Midst densities The density contrast of particle is 1~5 g/cm3
9. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
10. in accordance with the method for claim 1, it is characterised in that cooling final temperature is 12 DEG C~15 below slack wax fusing point ℃。
11. in accordance with the method for claim 1, it is characterised in that described forces air flow through wax layer in heating sweating Journey any stage is implemented.
12. in accordance with the method for claim 1, it is characterised in that described rate of temperature fall is 1.5 DEG C/h~2.5 DEG C/h.
13. in accordance with the method for claim 1, it is characterised in that described heating rate 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 step(4)The predetermined temperature of middle heating is less than purpose production 2 DEG C~10 DEG C of the fusing point of product.
15. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer Top increase air pressure realizes that the gauge applied above wax layer is 0.2~2.0 atmospheric pressure, and is remained below wax layer Normal pressure.
16. in accordance with the method for claim 2, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer Lower section reduction air pressure is realized, normal pressure is kept above wax layer, and the gauge below wax layer is maintained -0.2~-0.8 Atmospheric pressure.
17. in accordance with the method for claim 2, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
18. in accordance with the method for claim 4, it is characterised in that the material density of the solid particle is 6~12 g/cm3
19. in accordance with the method for claim 11, it is characterised in that described forces air flow through wax layer in heating reality at initial stage Apply.
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