CN105754652B - A kind of preparation method of explosive insensitiveness wax - Google Patents
A kind of preparation method of explosive insensitiveness wax Download PDFInfo
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- CN105754652B CN105754652B CN201410786123.2A CN201410786123A CN105754652B CN 105754652 B CN105754652 B CN 105754652B CN 201410786123 A CN201410786123 A CN 201410786123A CN 105754652 B CN105754652 B CN 105754652B
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Abstract
The invention discloses a kind of preparation method of explosive insensitiveness wax.This method is uniformly paved with solid particle before heating sweating effort on wax layer surface, and carries out the oil of liquid by wax layer using air-flow in heating sweating effort, enhances separating effect and accelerates separating rate.The present invention is on the basis of common sweating method, and the process that fluid oil is separated with solid state wax is forced in increase, this solvent-free de-oiling method of sweating is produced explosive insensitiveness wax 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
Technical field
The invention belongs to Wax special production technical field, more particularly to a kind of preparation method of explosive insensitiveness wax.
Background technology
Explosive is the material that rapidly can be burnt or decompose, can be in very short time under certain outside energy effect
Interior vigorous combustion（Explode）Substantial amounts of heat and gas are produced, the detonation formula acting stablized to external world.During explosive charge
Play destruction, throwing, compression etc. to ambient substance.
Explosive comes from China, is one of Ancient Times in China four inventions.After 19th-century, foreign chemical industry is rapidly sent out
Exhibition, generates number with the explosive of all kinds of thousand notes and chemical composition.In late nineteenth century and the World War I, respectively
Explosive used in state is mainly TNT（Picric acid）.Because accidental explosion accident easily occurs for picric acid, in World War II by
TNT replaces.TNT is inexpensive, sensitivity is low, but detonation energy is low.Conventional high explosive is RDX at present（RDX, ring cyclonite
Three ammonium nitrates）And HMX（HMX, HMX）.
Explosive has been widely used in mining, oil exploitation, geological prospecting, machine-building, hydraulic and electric engineering since the generation
The all sectors of the national economy such as engineering, railway and highway construction；Explosive militarily can be used as explosive charge and military blasting.Explosive
Widely use important facilitation served to the material progress of human society.
With the development of science and technology, various explosives develop in terms of high-power, high security, different purposes,
Storage and traffic condition propose different requirements to the various performances of the explosive of different compositions.The quick change of modern war with
Development and battlefield surroundings go from bad to worse, and to weapons and ammunitions propose more stringent requirement.Ammunition will not only meet and penetrate
The requirement that Cheng Yuan, precision are high, power is big, and higher and higher want is proposed to the survival ability and security performance of modern weapons
Ask.
Ammunition is produced the phenomenon of self-destruction by environmental stimuli and occurred repeatedly in war.Counted according to relevant person, modern times war
In striving, the destruction about 60% of tank is due to, by external world's attack, to cause itself ammunition to explode and damage.And weapon bullet
The accident that medicine occurs in the duties processing procedures such as production, maintenance, transport due to safety issue is even more too numerous to mention.These are miserable
Pain lesson make it was recognized that, it is necessary to develop low rapid wear ammunition, develop desensitized explosive, the emphasis that explosive is studied is from attempting significantly
Degree improve energy transfer to ensure security performance on the premise of moderately improve energy direction on.
Under given conditions, the various sensitivity of explosive have close relationship with the security that powder charge is used, certain
In the range of various sensitivity it is lower, safety in utilization is better.It is represented by according to different detonation momentum sensitivity：Heat sensitivity, flame
Sensitivity, mechanical sensitivity (including impact sensitivity, friction sensitivity), shock sensitivity, detonation sensitivity etc..
Some explosives, such as RDX and HMX, their other explosion propertys very well or the performance with certain special requirement,
Simply security is poor, it is impossible to while meeting the use requirement of high-power and high security, it is necessary to consider sensitivity with different sides
Method gives insensitiveness or insensitiveness processing.Explosive phlegmatizer refers to the material for reducing explosive sensitivity.Deterrent can be coated on fried
Space in medicine particle surface, filling explosive, can reduce the friction between explosive, disperse external forces and absorb heat, so that
Make explosive insensitiveness.
Being usually used in reducing the deterrent of explosive mechanical sensitivity has wax class, high polymer etc..Wax is used as the deterrent of explosive, the country
Over half a century is continued to use outside, its efficient insensitive action is recognized by people.Although there is the research of a variety of deterrents
Report, but pertroleum wax be still it is most ripe, using most deterrents.Wax can both be used alone as deterrent, also may be used
Carry out desensitized explosive to constitute blended wax.
Explosive insensitiveness wax has highly important effect to the insensitiveness of explosive, be to ensure that explosive storing, transport, use
Entire life cycle in security key factor.Some special explosive insensitiveness waxes require fusing points between 70 DEG C~80 DEG C,
Oil content is less than 0.5%, without mechanical admixture.General goods oil content in paraffin wax of the fusing point between 70 DEG C~80 DEG C is generally 0.8%
Between~2.0, it is impossible to meet the requirement of the special insensitiveness wax of high explosive.
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 continuous production, wax high income, production cost are relatively low, is that the main flow of current large-scale production paraffin wax product takes off
Oily technique.But solvent deoiling investment of production equipment is big；Need largely to use solvent in production process, recycling design needs to consume big
The energy of amount；Contain benzene homologues in solvent, environment can be impacted；Solvent is inflammable, easily causes 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
Explosive insensitiveness wax product of the fusing point at 70 DEG C~80 DEG C.There is experiment to show, common sweating de-oiling technique productions fusing point is on 70 DEG C of left sides
During the high melting point paraffin product on the right side, even if using the method for extending sweating sessions and improving sweating final temperature, sweating later stage wax
On 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
It is not suitable for explosive insensitiveness wax product of the production fusing point at 70 DEG C~80 DEG C, especially oil-containing figureofmerit can not meet technical indicator and want
Ask.Only part producer uses sweating de-oiling technique productions soap wax and the paraffin wax product of low melting point at present.
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 can not still produce explosive insensitiveness wax product of the fusing point at 70 DEG C~80 DEG C.
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 explosive insensitiveness wax 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 preparation method of explosive insensitiveness wax, 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 explosive insensitiveness wax product of sweating de-oiling.
A kind of preparation method of explosive insensitiveness wax of the present invention, including herein below：
A, first paragraph sweating, including：
（A1）Water is padded in sweatbox；
（A2）Using slack wax of the oil content less than 30% as raw material, load sweatbox after heating fusing；
（A3）Temperature is terminated with the cooling that 1.0 DEG C/h~4.0 DEG C/h speed is cooled to 10 DEG C~20 DEG C below slack wax fusing point
Degree；
（A4）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
In force air flow through wax layer；Wax layer, which reaches, stops sweating after predetermined temperature；
（A5）Collect on wax；
（A6）After refined, shaping it is intermediate products on wax；With
B, second segment sweating, including：
（B1）Water is padded in sweatbox；
（B2）The intermediate products obtained using first paragraph sweating load sweatbox as raw material after heating fusing；
（B3）It is whole with the cooling that 1.0 DEG C/h~4.0 DEG C/h speed is cooled to 10 DEG C~20 DEG C below intermediate products fusing point
Only temperature；
（B4）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
In force air flow through wax layer；Wax layer, which reaches, stops sweating after predetermined temperature；
（B5）Collect on wax；
（B6）After refined, shaping, packaging it is explosive insensitiveness wax product on wax.
In the preparation method of the explosive insensitiveness wax of the present invention, step（A2）Described in raw material slack wax oil content（With matter
Gauge）Less than 30%, its melting range is generally 55 DEG C~70 DEG C.Slack wax raw material can be the line that subtracts three or the line distillate warp that subtracts four
The obtained slack wax of dewaxing.
In the waxed Preparation Method of explosive insensitiveness of the present invention, preferably in step（A3）With（B3）After middle raw material decrease temperature crystalline and
In step（A4）With（B4）Before heating sweating effort（Now wax layer is in solid state）, uniformly it is paved with 10 on the surface of wax layer~
The solid particle of 100 mesh, preferably 20~50 mesh.The material density of solid particle is generally higher than 4 g/cm3, can be it is nonmetallic,
The material such as metal and alloy, preferably material density are 6~12 g/cm3Metal and alloying pellet, such as zinc, iron, copper, lead and its
The more stable low price metal material of the chemical property such as alloy.Consolidating for two or more unlike material density can be selected
Body particle, various solid particles can ratio mixing close by weight.Two kinds of adjacent solid particle materials of density it is close
Degree difference is 1~5 g/cm3.Density described herein refer to constitute solid particle material density, rather than solid particle heap
Density.Sweating effort can reclaim solid particle and clean to reuse after terminating.
In the preparation method of the explosive insensitiveness wax of the present invention, described sweatbox is generally sweating ware, and wax layer with
It is upper to increase dismountable sealing system and pressue device and/or increase vacuum plant below wax layer.Described pressure air-flow leads to
Cross wax layer and be utilized in increase pressure above wax layer（Air pressure）And/or pressure is reduced below wax layer（Air pressure）, make above and below wax layer
Form what pressure differential was realized.Described pressure differential is generally 0.1~5.0 atmospheric pressure, and preferably 0.2~2.0 atmospheric pressure is used
To force air flow through wax layer.
In the waxed Preparation Method of explosive insensitiveness of the present invention, step（A3）With（B3）Described in cool preferably 1.5 DEG C of speed/
H~2.5 DEG C/h.
In the waxed Preparation Method of explosive insensitiveness of the present invention, step（A3）With（B3）Described cooling final temperature is preferably original
12 DEG C~15 DEG C are expected below fusing point.
In the waxed Preparation Method of explosive insensitiveness of the present invention, step（A4）With（B4）Described heating rate preferably 1.0 DEG C/h
~2.0 DEG C/h.Step（A4）The predetermined temperature of middle heating（That is final temperature）To be the fusing point 1 of intermediate products less than purpose product
DEG C~10 DEG C.Step（B4）The predetermined temperature of middle heating（That is final temperature）To be the fusing point of explosive insensitiveness wax less than purpose product
1 DEG C~10 DEG C.
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.
The waxed Preparation Method of explosive insensitiveness of the present invention, the described wax layer that forces air flow through can be in heating sweating effort times
The meaning stage implements, and preferably implements initial stage in heating sweating.
The waxed Preparation Method of explosive insensitiveness of the present invention, the described wax layer that forces air flow through is utilized in increase above wax layer
What air pressure was realized, the pressure that can such as apply above wax layer is 0.2~2.0 atmospheric pressure（Gauge pressure）, and remained below wax layer
Normal pressure.
The waxed Preparation Method of explosive insensitiveness of the present invention, the described wax layer that forces air flow through is utilized in reduction gas below wax layer
What pressure was realized, normal pressure preferably is remained above wax layer, and the pressure below wax layer is maintained -0.2~-0.8 atmospheric pressure（Table
Pressure）.
In the waxed Preparation Method of explosive insensitiveness of the present invention, described sweating includes process（A）With（B）Two sections of circulation sweating
Process.Wherein process（A）First paragraph sweating reduction raw material oil content and be enriched with purpose product, and process（B）Second segment
Sweating continues de-oiling production explosive insensitiveness wax product.
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 low containing fried at 70 DEG C~80 DEG C for common sweating de-oiling technique
Medicine insensitiveness wax product.
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 70 DEG C~80
DEG C explosive insensitiveness wax product, by the further investigation to common sweating effort, be difficult to separate reason for wax and oil, by
Using the method that wax layer carries out fluid oil is forced air flow through in heating sweating effort, the separating effect of wax and oil is enhanced；
Simultaneously further preferably after the process of cooling terminates（I.e. before heating sweating effort）, now wax layer is in solid state, in wax layer
The method that surface is uniformly paved with solid particle is improved.In heating sweating effort, as wax layer temperature is raised, wax layer becomes
Soft, because density of solid particles is big, it is under gravity by with slower velocity sedimentation, so as to be passed through above and below being formed in wax layer
The thin channel worn, reduces filter flow resistance power, and is conducive to the quick discharge of oil.The solid particle of different densities and particle diameter it is heavy
Reduction of speed degree is different, can ensure that the different height in wax layer in the overall process of sweating de-oiling has using the solid particle of mixing
The passage of more discharge fluid oil.Wax layer is caused air flow through simultaneously, the oil of liquid is carried out to force separation wax and oil, so that
Enhance the separating effect of wax and oil so that sweating de-oiling technique can be used in producing explosive insensitiveness wax 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；While solid（Metal）Particle infall process
The tiny duct for running through wax layer up and down of middle formation, is more favorable to fluid oil and quickly discharges.So that sweating de-oiling is this
Solvent-free production process can produce explosive insensitiveness wax product.The inventive method plant investment is low, production process simple and operation
Expense is low, solvent-free pollution 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；In the sweating effort of heating by wax layer top formed malleation and/or wax layer bottom formed negative pressure with
Force air flow through wax layer to carry out in fluid oil, wax layer temperature, which reaches, stops sweating after preset temperature.
1-2 illustrates the preparation method of explosive insensitiveness wax of the present invention by the following examples.
Embodiment 1
The present embodiment includes A：First paragraph sweating, and B：Second segment sweating two parts.
A：First paragraph sweating
This process includes：（A1）Preparation,（A2）Charging,（A3）Decrease temperature crystalline,（A4）Heating sweating,（A5）Centre production
Product collection,（A6）The process such as intermediate products are refined.
（A1）Preparation
The sealing system on sweating ware top and surge tank and compressor are connected.
Sweating ware ware plate bottom pad water.
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 the heating function of the circulatory system, water-cycling-media is warming up to 65 DEG C.
（A2）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.
（A3）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.
（A4）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 68.0 DEG C with 2.0 DEG C/h heating rate.
Stop compressor, terminate sweating degreasing process.
（A5）Intermediate products are collected
The outlet of sweating ware is changed to connection intermediate products storage tank to receive on wax；
Continue to raise circulating water temperature to 90 DEG C, taken out with melting on wax, as the thick intermediate products of explosive insensitiveness wax（Ⅰ）.
（A6）Intermediate products are refined
Thick intermediate products are explosive insensitiveness wax intermediate products through clay-filtered, shaping（Ⅰ）.
Explosive insensitiveness wax intermediate products（Ⅰ）Property：
Fusing point：71.2 DEG C, oil content：3.26%.
Explosive insensitiveness wax intermediate products（Ⅰ）Yield is 18.3%（Relative to slack wax raw material）.
B：Second segment sweating
This process includes：（B1）Preparation,（B2）Charging,（B3）Decrease temperature crystalline,（B4）Heating sweating,（B5）Crude product
Collect,（B6）The process such as product purification and shaping, packaging.
（B1）Preparation
Surge tank is installed and vavuum pump is connected in sweating ware bottom；The sweating ware of jacketed is with removable coil pipe and with program
The circulatory system of refrigerating/heating function is connected；Start the heating function of the circulatory system, water-cycling-media is warming up to 75 DEG C.
Sweating ware ware plate bottom pad water.
（B2）Charging
With the product of first paragraph sweating（Intermediate products after refined）For raw material, sweating ware is added after heating fusing.By disk
Pipe is placed in raw material wax layer and fixed；Coil pipe, chuck and the circulatory system are connected.
（B3）Decrease temperature crystalline
Start the refrigerating function of the circulatory system, wax layer temperature drop is made to 58.0 DEG C with 2.0 DEG C/h rate of temperature fall；Close
The refrigerating function of the circulatory system.
（B4）Heat up sweating
Discharge sweating ware pad water.
Storage tank under sweating ware outlet connection wax；Open vavuum pump and keep buffering pressure inside the tank stable at -0.5~-0.7
Atmospheric pressure（Gauge pressure）, wax layer top keeps normal pressure；Start the heating function of the circulatory system, wax is made with 1.5 DEG C/h heating rate
Layer temperature is increased to 71.0 DEG C.
Stop vavuum pump, terminate sweating degreasing process.
（B5）Crude product is collected：
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 explosive insensitiveness wax crude product（Ⅰ）.
（B6）Product purification, shaping and packaging：
Crude product is explosive insensitiveness wax product after clay-filtered, shaping and packaging（Ⅰ）.
Explosive insensitiveness wax product（Ⅰ）Property：
Fusing point：73.5 DEG C, oil content：0.44%th, mechanical admixture：Nothing.The correlation technique for meeting explosive insensitiveness wax product will
Ask.
Explosive insensitiveness wax product（Ⅰ）Yield be 7.16%（Relative to raw material slack wax）.
Embodiment 2
The present embodiment includes A：First paragraph sweating, and B：Second segment sweating two parts.
A：First paragraph sweating
This process includes：（A1）Preparation,（A2）Charging,（A3）Decrease temperature crystalline,（A4）Heating sweating,（A5）Centre production
Product are collected and metallic particles is reclaimed,（A6）The process such as intermediate products are refined.
（A 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 the heating function of the circulatory system, water-cycling-media is warming up to 65 DEG C.
（A2）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.
（A3）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.
（A4）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；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 68.0 DEG C with 2.0 DEG C/h heating rate.
Stop compressor, terminate sweating degreasing process.
（A5）Thick intermediate products are 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 the thick intermediate products of explosive insensitiveness wax（Ⅱ）.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
（A6）Intermediate products are refined
Thick intermediate products are explosive insensitiveness wax intermediate products through clay-filtered, shaping（Ⅱ）.
Explosive insensitiveness wax intermediate products（Ⅱ）Property：
Fusing point：71.8 DEG C, oil content：2.87%.
Explosive insensitiveness wax intermediate products yield is 17.8%（Relative to slack wax raw material）.
B：Second segment sweating
This process includes：（B1）Preparation,（B2）Charging,（B3）Decrease temperature crystalline,（B4）Heating sweating,（B5）Crude product
Collect and metallic particles reclaim,（B6）The process such as product purification and shaping, packaging.
（B1）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.
Sweating ware ware plate bottom pad water；Double-deck Medium speed filter paper is spread in sweating ware bottom.
Surge tank is installed and vavuum pump is connected in sweating ware bottom；The sweating ware of jacketed is with removable coil pipe and with program
The circulatory system of refrigerating/heating function is connected；Start the heating function of the circulatory system, water-cycling-media is warming up to 75 DEG C.
（B2）Charging
With the product of first paragraph sweating（Intermediate products after refined）For raw material, add bottom after heating fusing and complete filter paper
Sweating ware.Coil pipe is placed in raw material wax layer and fixed；Coil pipe, chuck and the circulatory system are connected.
（B3）Decrease temperature crystalline
Start the refrigerating function of the circulatory system, wax layer temperature drop is made wax to 58.0 DEG C with 2.0 DEG C/h rate of temperature fall
Layer crystallization.
Foregoing lead, zinc hybrid particles are uniformly paved with wax layer surface；Close the refrigerating function of the circulatory system.
（B4）Heat up sweating
Discharge sweating ware pad water.
Storage tank under sweating ware outlet connection wax；Open vavuum pump and keep buffering pressure inside the tank stable at -0.5~-0.7
Atmospheric pressure（Gauge pressure）, wax layer top keeps normal pressure；Start the heating function of the circulatory system, wax is made with 1.5 DEG C/h heating rate
Layer temperature is increased to 71.0 DEG C.
Stop vavuum pump, terminate sweating degreasing process.
（B5）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 to raise circulatory system temperature to 90 DEG C, with
Fusing is taken out on wax, as explosive insensitiveness wax crude product（Ⅱ）.
The mixed metal particles on filter paper are collected, cleans, dry in case reusing.
（B6）Product purification, shaping and packaging
Crude product（Ⅱ）It is explosive insensitiveness wax product after clay-filtered, shaping and packaging（Ⅱ）.
Explosive insensitiveness wax product（Ⅱ）Property：
Fusing point：74.7 DEG C, oil content：0.35%th, mechanical admixture：Nothing.The correlation technique for meeting explosive insensitiveness wax product will
Ask.
Explosive insensitiveness wax product（Ⅱ）Yield be 7.06%（Relative to raw material slack wax）.
The preparation method of explosive insensitiveness wax of the present invention is can be seen that by embodiment 1-2, 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 fusing point between 70 DEG C~80 DEG C, oil content be less than 0.5%, the special dynamite insensitiveness wax product without mechanical admixture.
Claims (17)
1. a kind of preparation method of explosive insensitiveness wax, including herein below：
A, first paragraph sweating, including：
（A1）Water is padded in sweatbox；
（A2）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；
（A3）10 DEG C~20 DEG C below slack wax fusing point of cooling final temperature is cooled to 1.0 DEG C/h~4.0 DEG C/h speed；
（A4）The pad water in sweatbox is discharged, is then heated up with 0.5 DEG C/h~3.0 DEG C/h speed；It is strong in temperature-rise period
Air-flow processed passes through wax layer；Wax layer, which reaches, stops sweating after predetermined temperature；
（A5）Collect on wax；
（A6）After refined, shaping it is intermediate products on wax；With
B, second segment sweating, including：
（B1）Water is padded in sweatbox；
（B2）The intermediate products obtained using first paragraph sweating load sweatbox as raw material after heating fusing；
（B3）Terminated with the cooling that 1.0 DEG C DEG C/h~4.0 DEG C/h speed is cooled to 10 DEG C~20 DEG C below intermediate products fusing point
Temperature；
（B4）The pad water in sweatbox is discharged, is then heated up with 0.5 DEG C/h~3.0 DEG C/h speed；It is strong in temperature-rise period
Air-flow processed passes through wax layer；Wax layer, which reaches, stops sweating after predetermined temperature；
（B5）Collect on wax；
（B6）After refined, shaping, packaging it is explosive insensitiveness wax product on wax；
Wherein, in step（A3）After middle raw material decrease temperature crystalline, and in step（A4）Before heating sweating effort, and in step（B3）
After decrease temperature crystalline, step（B4）Heat up before sweating effort, solid particle is uniformly paved with the surface of wax layer.
2. in accordance with the method for claim 1, it is characterised in that the mesh number of the solid particle is 10~100 mesh.
3. according to the method described in claim 1 or 2, it is characterised in that the material density of the solid particle is more than 4 g/cm3。
4. in accordance with the method for claim 3, it is characterised in that described solid particle is selected from zinc, iron, copper, lead and its conjunction
One or more in gold.
5. in accordance with the method for claim 4, it is characterised in that described solid particle selects two or more unlike materials
Solid particle, the density contrasts of two kinds of adjacent solid particle materials of density is 1~5 g/cm3。
6. 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.
7. in accordance with the method for claim 1, it is characterised in that step（A3）With（B3）Described in the speed that cools be 1.5
DEG C/h~2.5 DEG C/h.
8. in accordance with the method for claim 1, it is characterised in that step（A3）With（B3）Described cooling final temperature is original
12 DEG C~15 DEG C are expected below fusing point.
9. in accordance with the method for claim 1, it is characterised in that step（A4）With（B4）Described in heating rate be 1.0
DEG C/h~2.0 DEG C/h.
10. in accordance with the method for claim 1, it is characterised in that step（A4）The predetermined temperature of middle heating is less than centre
1 DEG C of the fusing point of product~10 DEG C, step（B4）The predetermined temperature of middle heating is 1 DEG C of the fusing point less than purpose product explosive insensitiveness wax
~10 DEG C.
11. in accordance with the method for claim 6, it is characterised in that the described wax layer that forces air flow through is utilized in wax layer
Top increase air pressure is realized：The gauge applied above wax layer is 0.2~2.0 atmospheric pressure, and is kept below wax layer
For normal pressure.
12. in accordance with the method for claim 6, 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 remained above wax layer, and the gauge below wax layer is maintained -0.2~-0.8
Individual atmospheric pressure.
13. 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.
14. according to the method described in claim 1 or 2, it is characterised in that the mesh number of the solid particle is 20~50 mesh.
15. in accordance with the method for claim 3, it is characterised in that the material density of the solid particle is 6~12 g/cm3。
16. in accordance with the method for claim 6, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
17. in accordance with the method for claim 13, it is characterised in that described forces air flow through wax layer at the beginning of the sweating that heats up
Phase implements.
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| CN201410786123.2A CN105754652B (en) | 2014-12-18 | 2014-12-18 | A kind of preparation method of explosive insensitiveness wax |
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Citations (3)
| 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. |
| CN103102917A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Two-stage hydrogenation method for producing low freezing point motor fuel |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100343165B1 (en) * | 1998-09-04 | 2002-08-22 | 삼성전자 주식회사 | Computer having the function of emergency call and emergency calling method using a computer |
-
2014
- 2014-12-18 CN CN201410786123.2A patent/CN105754652B/en active Active
Patent Citations (3)
| 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. |
| CN103102917A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Two-stage hydrogenation method for producing low freezing point motor fuel |
Non-Patent Citations (1)
| Title |
|---|
| 发汗技术在相变石蜡开发中的应用;魏荣敏等;《石化技术》;20131231;第20卷(第4期);第21-24页 * |
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