CN106883878B - A kind of sweating and the method for producing explosive insensitiveness wax - Google Patents
A kind of sweating and the method for producing explosive insensitiveness wax Download PDFInfo
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- CN106883878B CN106883878B CN201510928616.XA CN201510928616A CN106883878B CN 106883878 B CN106883878 B CN 106883878B CN 201510928616 A CN201510928616 A CN 201510928616A CN 106883878 B CN106883878 B CN 106883878B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/005—Desensitisers, phlegmatisers
Abstract
The invention discloses a kind of sweating and the methods for producing explosive insensitiveness wax.This method is on the basis of common sweating de-oiling technique, the oil of liquid is carried out to force separation wax and oil by wax layer using air-flow in sweating effort, pressure is applied to wax layer by placing solid mass in wax layer simultaneously, to accelerate the separating rate of wax and oil and ensure airflow through wax layer, so that this solvent-free de-oiling method of sweating de-oiling be allow to produce explosive insensitiveness wax product.The method of the present invention has many advantages, such as that investment of production equipment is low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution.
Description
Technical field
The invention belongs to Wax special production technical fields, more particularly to a kind of sweating and the side of production explosive insensitiveness wax
Method.
Background technique
Explosive is the substance that rapidly can be burnt or decompose, can be in very short time under certain outside energy effect
Interior vigorous combustion (exploding) generates a large amount of heat and gas, carries out stable detonation formula to the external world and does work.Explosive it is extensive
Important facilitation is played using the material progress to human society.
Main explosive used is TNT during World War II, and currently used explosive is heisuojin (RDX, ring three
Three ammonium nitrate of methine) and octogen (HMX, cyclotetramethyltetranitrosamine).With the development of science and technology, various explosives towards
Development in terms of high-power, high security.
Under given conditions, the safety that the various sensitivity of explosive and powder charge use has close relationship, certain
Various sensitivity are lower in range, and safety in utilization is better.It may be expressed as: heat sensitivity, flame according to different detonation momentum sensitivity
Sensitivity, mechanical sensitivity (including impact sensitivity, friction sensitivity), shock sensitivity, detonation sensitivity etc..
Some explosives, such as RDX and HMX high explosive, their other explosion properties are very well or special with certain
The performance needed, only safety is poor, cannot meet the requirement of high-power and high security simultaneously, it is necessary to consider sensitivity
Give insensitiveness or insensitiveness processing with different methods.Explosive phlegmatizer refers to the substance to reduce explosive sensitivity.
The deterrent for being usually used in reducing explosive mechanical sensitivity has wax class, high polymer etc..Wax as explosive deterrent in state
Inside and outside to have continued to use over half a century, its efficient insensitive action has been recognized by people.Explosive is with insensitiveness wax to explosive
Insensitiveness has highly important effect, be to ensure that explosive in storage, transport, the entire life cycle that uses safety it is important
Factor.The insensitiveness wax of some special dynamites requires fusing point between 70 DEG C~80 DEG C, oil content 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 not able to satisfy certain dedicated usually between 0.8%~2.0%
The requirement of explosive insensitiveness wax.
The general name of the pertroleum wax all kinds of wax products obtained that are crude oil after refining processing from wax-containing distillate, including liquid
Body paraffin, soap manufacturing paraffin, paraffin and microwax.Paraffin be in crude oil lube cut through dewaxing, de-oiling, purification and molding
Production, typically contain C20~C50The components such as n-alkane, a small amount of isoparaffin and cycloalkane, usual fusing point is 50 DEG C~
74℃。
Dewaxing is that the process for the slack wax that oil content is 10~30% or so, dewaxing technique are produced by raw material of lube cut
Mainly there are squeezing dewaxing and solvent dewaxing.De-oiling is that the process of the base oil wax below of oil content 2% is produced using slack wax as raw material,
De-oiling technique mainly has solvent deoiling and sweating de-oiling.Base oil wax is again through clay-filtered or hydrofinishing and molding, packaging etc.
Commodity oil wax can be obtained in step.
Solvent deoiling method is according to wax and oil in selective solvent (acetone, benzene and toluene mixture；Or acetone, toluene；
Or methyl ethyl ketone, toluene) in the property of different solubility separated.Solvent deoiling technique with production process, receive by continuous, wax
Rate is high, finished product wax oil content can very low, lower production costs the advantages that, be the mainstream of current large-scale production petroleum paraffin product
De-oiling technique.But solvent deoiling technique investment of production equipment is big；It needs largely to use solvent in production process, recycling design needs
Consume a large amount of energy；Contain benzene homologues in solvent, environment can be impacted；Solvent is inflammable, be easy to cause production accident.
Sweating de-oiling method is separated using wax and oil property with different melting points.Point of various hydro carbons in pertroleum wax
Son amount Bu Tong can all make its fusing point different with structure.When being all n-alkane structure, the biggish n-alkane of molecular weight melts
Point is higher, and the fusing point of the lesser n-alkane of molecular weight is lower；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane is wanted
Lower than n-alkane, and isomery degree more high-melting-point is lower, or even is at normal temperature just in liquid condition, i.e., usually said
Oil.
Common sweating de-oiling technique mainly comprises the steps that (1) preparation: pad water is full of sweatbox with water
Ware plate lower space；Charging, raw material are heated to being packed into sweatbox when fusing point or more is in a liquid state；(2) it crystallizes: by raw material with little
10~20 DEG C of its fusing point or less are progressively cooled in the rate of temperature fall of 4 DEG C/h.In cooling procedure, various components are by fusing point by height
It is successively crystallized to low sequence and forms solid；(3) it sweating: after wax layer temperature reaches preset cooling final temperature, bleeds off
Pad water；Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components by fusing point by as low as
High sequence, which is successively fused into liquid and flows out the wax layer residue (on wax) finally obtained (under wax), to be exactly high-melting-point, low contains
The wax of oil；Continue to increase temperature after sweating effort, be taken out on wax with fusing, as crude product；(4) refine: crude product is molten
Be warming up to predetermined temperature after change, carclazyte is added and constant temperature stir to the predetermined time after filter, then formed, pack i.e. for the purpose of produce
Product.
Common sweating de-oiling technique can produce fusing point in 40 DEG C~60 DEG C of soap manufacturing paraffin and low melt point paraffin, be not suitable for giving birth to
Produce explosive insensitiveness wax product of the fusing point at 70 DEG C~80 DEG C.Have experiments have shown that, common sweating de-oiling technique production fusing point is 70
DEG C or so high melting point paraffin product when, even if using sweating sessions and the method that improves sweating final temperature is extended, after sweating
Oil content on phase wax 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 explosive insensitiveness wax product of the fusing point at 70 DEG C~80 DEG C, and especially oil-containing figureofmerit cannot meet explosive
With the technical requirement of insensitiveness wax.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is lower, the production cycle is longer, but
Be sweating de-oiling technique have small investment, production process is simple, operating cost is low, production process is safe, it is energy saving and to environment without
The advantages that pollution, still has part of the manufacturer producing soap manufacturing paraffin product using this method at present.
For many years, sweating de-oiling method has obtained some development in production equipment and process aspect, as CN89214332(is vertical
Formula square multipul sections spacer diaphoresis tank), CN94223980.6(ware type sudorific device), CN98233254.8(Paraffin sweating pot),
CN200920033500.X(novel paraffin sweating tank), a kind of Efficient paraffin sweatbox of CN201210508905.0(),
CN201320127680.4(tubular type paraffin deoiler) etc., it is improved in sweating de-oiling production equipment；CN91206202
(a kind of high-efficient sweat pot for paraffin wax) improves in sweating de-oiling technique, but these improvement cannot still produce fusing point 70 DEG C~
80 DEG C of explosive insensitiveness wax product.
Sweating de-oiling technique is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product,
In the today for advocating green low-carbon, environmental protection and energy saving, the demand of explosive insensitiveness wax product is produced more using sweating de-oiling technique
Urgently.
Summary of the invention
In view of the deficiencies of the prior art, a kind of method that the present invention provides sweating and produces explosive insensitiveness wax, specifically
Say on the basis of common sweating de-oiling technique, carried using air-flow by wax layer in sweating effort using sweatbox
The oil of liquid applies wax layer by way of placing solid mass in wax layer in sweating effort with forcing separation wax and oil out
Pressurization to accelerate the separating rate of wax and oil and ensure airflow through wax layer, makes this solvent-free de-oiling method of sweating de-oiling can by force
To produce explosive insensitiveness wax product.Explosive can also be produced by the way of sweating product and the allotment of general goods paraffin to use
Insensitiveness wax product is to reduce production cost.
A kind of sweating of the invention and the method for producing explosive insensitiveness wax, including the following contents:
(1) charge: the paraffin for being 60 DEG C~74 DEG C using fusing point is packed into sweatbox after heating fusing as raw material；
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization: wax layer is cooled down with 1.0 DEG C/h~3.0 DEG C/h rate
To proper temperature, high temperature constant temperature is for a period of time；It is cooled again with 0.5 DEG C/h~2.5 DEG C/h rate to below raw material fusing point 5
DEG C~20 DEG C of cooling final temperature, and cryogenic thermostat is for a period of time；
(3) heating-constant temperature sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate；Wax layer reaches predetermined temperature and constant temperature
Stop sweating after a period of time；Wax layer is forced air flow through in sweating effort；
(4) refine: on wax after refining be explosive insensitiveness wax product or be used as explosive insensitiveness wax product reconciliation group
Point.
In method of the invention, the oil content (in mass) of the sweating raw material paraffin grade wax is generally less than
2.0%；Fusing point is generally 60 DEG C~74 DEG C, preferably 64 DEG C~70 DEG C.
In method of the invention, in step (3) sweating effort, preferably by placing solid mass on wax layer surface with right
The pressure of wax layer application 0.5kPa or more.(e.g., solid mass surfacing, overall dimensions are slightly less than sweatbox inner wall size
The gap of solid mass edge and sweatbox inner wall is generally 0.01~50mm, preferably 0.1~20mm), inside has and passes through up and down
The gap worn.The density of solid mass generally requires to be greater than 4 g/cm3, can be the materials such as nonmetallic, metal and alloy, preferably
Density is 6~12 g/cm3Metal and alloy, such as zinc, iron, copper, lead and its alloy chemical property it is more stable low price gold
Belong to material.
In the present invention, solid mass is placed to apply pressure to wax layer on wax layer surface one of in the following ways: (1) being existed
It is added at one time the solid mass that can produce 0.5kPa or more pressure in sweating effort, is preferably added at one time when sweating starts
It can produce the solid mass of 1.4~20.0kPa pressure；(2) (preferably 2~3 times) are added several times in sweating effort, i.e., every
The solid mass that can produce 0.5kPa or more pressure is added in 0.1~20.0 h, being preferably added in every 0.1~10.0 h can produce
The solid mass of raw 1.4~10.0kPa pressure.
In method of the invention, the sweatbox is sweating ware, and wax layer pressurizing device added above and/or
Increase vacuum plant below wax layer.In step (3) sweating effort, the wax layer that forces air flow through is used above wax layer
Increase air pressure and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize.The pressure difference is general
For 10~500 kPa, preferably 20~200 kPa, to force air flow through wax layer.
In method of the invention, in the temperature-fall period of step (2) crystallization, the rate of temperature fall before high-temperature constant temperature section
It is preferred that 1.5 DEG C/h~2.5 DEG C/h.The proper temperature of the high-temperature constant temperature section of the temperature-fall period is -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.The time of the high-temperature constant temperature section for the process that cools is 0
~4.0 hours, preferably 0.1~4.0 hour, more preferably 1.0~4.0 hours.
In method of the invention, rate of temperature fall of the temperature-fall period of step (2) crystallization after high-temperature constant temperature section is excellent
Select 1.0 DEG C/h~2.0 DEG C/h.The cooling final temperature is preferably 8 DEG C~15 DEG C of source commodity paraffin melting point or less.It is described
Cool to final temperature, increase the cryogenic thermostat stage so that solid crystal is more abundant, the time in cryogenic thermostat stage
It is 0~3.0 hour, preferably 0.1~3.0 hour, more preferably 1.0~3.0 hours.
In method of the invention, heating rate preferably 1.0 DEG C/h~2.0 DEG C/h of the sweating effort of the step (3).Institute
The predetermined temperature (i.e. final temperature) for stating heating is lower than 1 DEG C~10 DEG C of fusing point of the i.e. explosive insensitiveness wax of purpose product.
In method of the invention, after the sweating of the step (3) is warming up to the predetermined temperature for producing product, increase constant temperature rank
Section can be such that wax separates with oil more sufficiently, and time in constant temperature stage is 0~5.0 hour, and preferably 0.1~5.0 hour, most preferably
It is 1.0~5.0 hours.
In method of the invention, the heating rate and cooling rate of said wax layer can pass through air bath, water-bath, oil bath
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer heating is controlled using water-bath or oil bath mode
When rate and rate of temperature fall, collet can be increased outside sweating ware, collet is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function, the substances such as water or conduction oil are added as circulatory mediator in the circulatory system；Coil pipe is soaked after charging
Not and be fixed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In method of the invention, the wax layer that forces air flow through of the step (3) can be real in sweating effort any stage
It applies, preferably implements at sweating initial stage.
In method of the invention, the wax layer that forces air flow through of the step (3) is utilized in increase air pressure above wax layer
Realize, can such as apply 20~150 kPa(gauge pressures above wax layer) air pressure, and wax layer lower section remain normal pressure.
In method of the invention, the wax layer that forces air flow through of the step (3) is utilized in reduction air pressure below wax layer
Realize, such as can the air pressure above wax layer keep normal pressure, and below wax layer maintain -20~-80 kPa(gauge pressures) air pressure.
In method of the invention, step (4) products therefrom may be used as explosive insensitiveness wax blend component, can with it is common
Paraffin grade wax is deployed to reduce cost.Therefore, method of the invention can also include step (5): acquired blend component and quotient
The allotment of product paraffin, molding obtain explosive insensitiveness wax product after packing；The fusing point of allotment paraffin grade wax is generally 64
DEG C~74 DEG C, oil content be 0.5%~2.0%；The allotment ratio of blend component and paraffin grade wax be 10%~99.9%:0.1%~
90%, preferably 10%~90%:10%~90%.The fusing point of preferred allotment paraffin grade wax is 68 DEG C~72 DEG C, oil content is
0.5%~1.0%.
Sweating de-oiling method is to be separated using wax and oil property with different melting points to produce pertroleum wax, for petroleum
Wax sweating process studies have shown that in sweating effort, oil is gradually discharged along crystalline portion, be similar to liquid in capillary
The case where middle flowing.But the high melting point paraffin product for fusing point at 70 DEG C or so, due to isoparaffin and cycloalkanes in raw material
The substances such as hydrocarbon increase, and chemical composition is complicated, cause crystals upon crystallization structure more fine and compact, are formed to the discharge of oil huge
Flow resistance power is filtered, this is resulted in only, and wax is difficult to be kept completely separate with oil in the common sweating effort of gravity natural separation.Therefore common
Sweating de-oiling technique cannot produce fusing point in 70 DEG C~80 DEG C, the oil content insensitiveness wax product of the explosive less than 0.5%.
The present invention in order to make sweating de-oiling it is this it is solvent-free production paraffin method be suitable for production fusing point 70 DEG C~80
DEG C, the oil content insensitiveness wax product of the explosive less than 0.5%, it is difficult for wax and oil by the further investigation to common sweating effort
To separate reason, wax layer is forced air flow through by using in sweating effort, while increasing height further preferably in crystallization process
The processes such as warm constant temperature stage and cryogenic thermostat stage and the constant temperature stage of sweating effort；And by wax layer in sweating effort
The mode that solid mass is placed on surface applies pressure to wax layer, these measures significantly reduce the oil content of product, Ke Yiman
The technical requirements of sufficient explosive insensitiveness wax product.
It is difficult to the reason of separating for wax in sweating effort and oil, by using air-flow to take by wax layer in sweating effort
The method for taking fluid oil out of forces oil to enhance separating effect with the separation of wax and accelerate separating rate；It was cooling
Increasing the high temperature constant temperature stage in journey can make the crystallization of pertroleum wax bigger, be conducive to discharge oily in heating sweating effort.For
Pertroleum wax crystallization process studies have shown that the chemical composition of pertroleum wax is to determine the main factor of crystal habit, it is cooling simultaneously
The condition of process also will affect crystal habit, especially near fusing point at a temperature of influence of the cooling condition to crystal habit
It is most obvious.When being cooled near fusing point, the n-alkane of larger molecular weight has formed crystallization and has been precipitated pertroleum wax, this partially crystallizable
Body can be used as the nucleus for being subsequently formed crystallization, increases the high temperature constant temperature stage at this time, nucleus can be enable sufficiently to increase, and be formed
Larger sized crystal, although this larger sized crystal is coarse not as good as the crystallization of low melt point paraffin, this increase
Crystal structure to the sweating stage discharge oil be also it is highly beneficial.During common sweating process, with the gradually discharge of oil,
Wax layer can generate the contraction of vertical direction and the contraction of horizontal direction, when above and below wax layer formed pressure difference to force air flow through
When wax layer, it some times happens that air-flow flows through through gap between wax layer and ware plate and the phenomenon that without wax layer.In the method for the present invention, lead to
Cross and apply the means of pressure to wax layer in the mode that solid mass is placed on wax layer surface, the oil coated in extrudable wax crystallization to
Accelerate the separating rate of wax and oil, it is often more important that wax layer can be made only to generate the contraction of vertical direction without generation level side
To contraction, increase the resistance between wax layer and baffle and ware plate；Simultaneously because have perforative gap up and down inside solid mass,
It may insure that air-flow is fuel-displaced to carry by wax layer.The cryogenic thermostat stage for being aided with crystallization process again keeps solid crystal more abundant,
And the constant temperature stage of sweating effort, to separate wax with oil the methods of more abundant, and sweating de-oiling technique is allow to produce explosive with blunt
Feel wax product.
By select fusing point for 64 DEG C~74 DEG C, oil content be 0.5%~2.0%, preferably 68 DEG C of fusing point~72 DEG C, oil-containing
Amount is deployed for 0.5%~1.0% paraffin grade wax and sweating product, then can reduce production cost.
The invention has the advantages that by using air-flow to force in sweating effort by the method that wax layer carries out fluid oil
The separation of wax and oil, enhances separating effect and accelerates separating rate；Simultaneously by being placed in wax layer in sweating effort
Solid mass is to accelerate the separating rate of wax and oil and ensure airflow through wax layer, so that it is fried to produce sweating de-oiling technique
Medicinal insensitiveness wax product.Method of the invention is low with plant investment, production process is simple and operating cost is low, safety, energy conservation
And the advantages that solvent-free pollution environment.
Specific embodiment
Sweating ware top connects dismountable sealing device and connect with pressurized buffer tank and compressor, and/or in sweating
Ware lower part connects pressure-reducing cushioning tank and vacuum pump；Sweating ware is packed into after paraffin raw material heating fusing；Wax layer ascending, descending is controlled with water-bath
Warm speed；Wax layer temperature be down to raw material melting temperature nearby and constant temperature for a period of time；Continue to be cooled to preset temperature and constant temperature one
The section time；In sweating effort, start compressor in wax layer positive pressure formed above, and/or starting vacuum pump with wax layer with
Lower formation negative pressure, to force air flow through wax layer；Solid pressure preferably is gradually increased on wax layer surface in sweating effort；Wax
Layer temperature reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；On wax through purification, (with paraffin grade wax allotment) at
It is explosive insensitiveness wax product after type, packaging.
The method for illustrating sweating of the present invention below by way of specific embodiment and producing explosive insensitiveness wax.
Embodiment 1
The present embodiment includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter
The processes such as temperature-constant temperature sweating, (4) product purification, (5) product preparing.
(1) preparation
The sealing system of sweating ware (square that inner wall is 1m × 1m) is connected with pressurized buffer tank and compressor；?
Sweating ware lower part installation pressure-reducing cushioning tank simultaneously connects vacuum pump；Sweating ware collet and removable coil pipe are connect with the circulatory system,
Using water as medium；The heating function for starting the circulatory system, makes recirculated water be warming up to 70 DEG C.Water is padded below sweating ware ware plate.
With 66#Semi-refined wax (Jinan petro-chemical corporation, 66.35 DEG C of fusing point, oil content 0.76%) is raw material, is added after heating fusing
Enter sweating ware.Coil pipe is immersed in raw material wax layer and is fixed.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, so that wax layer temperature is dropped to 67.0 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
56.0 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.
(3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (I) is to receive under wax；Connect the top seal of sweating ware
Device；Starting compressor simultaneously keeps pressurized buffer tank internal pressure strong stability in 110~130kPa(gauge pressure), sweating ware ware plate lower section is protected
Hold normal pressure；Start circulation system function, so that wax layer temperature is increased to 62.0 DEG C with the heating rate of 1.5 DEG C/h.
Stop compressor.Remove sealing device.It opens vacuum pump and keeps surge tank internal pressure strong stability in -40~-60 kPa
(gauge pressure), wax layer top air pressure keep normal pressure；Continue that wax layer temperature is made to be increased to 68.0 DEG C and perseverance with the heating rate of 1.5 DEG C/h
Temperature 4.0 hours so that the wax in wax layer is sufficiently separated with oil.
Stop vacuum pump, terminates sweating degreasing process.
The outlet of sweating ware is changed to connection crude product storage tank (I) to receive on wax.Continue increase circulating water temperature to 85 DEG C, with
Fusing is taken out on wax, as crude product (I).
(4) product purification
Crude product (I) is explosive after clay-filtered, molding, packaging with insensitiveness wax product (I).
Explosive insensitiveness wax product (I) property: 72.75 DEG C of fusing point；Oil content 0.35%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.The yield of explosive insensitiveness wax product (I) is 19.8%(relative to raw material 66#Half
Refine wax).
(5) product preparing
Explosive with insensitiveness wax (I) and No. 70 semi-refined waxs (Dalian Petrochemical Industry Company, 70.35 DEG C of fusing point；Oil content 0.81%) by weight
Amount is heated to 90 DEG C and melts and be uniformly mixed, be explosive insensitiveness wax after forming, packing than being that the ratio of 80%:20% weighs
Product (II).
Explosive insensitiveness wax product (II) property: 72.68 DEG C of fusing point；Oil content 0.45%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.
Embodiment 2
The present embodiment includes: (1) preparation, (2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization (3) liter
The processes such as temperature-constant temperature sweating, (4) product purification, (5) product preparing.
(1) preparation
It is several to prepare stainless steel plate, every piece of stainless steel plate overall dimensions are the m of 0.98 m × 0.98m × 0.02, and stainless
The through hole (away from drilling, hole center spacing 0.04m is played at edge 0.01m) that equally distributed 0.0015 m of φ is bored on steel plate is (every
The pressure about 1.5kPa that block stainless steel plate generates), it is spare.
The sealing system of sweating ware (with embodiment 1) is connected with pressurized buffer tank and compressor；In sweating ware lower part
Installation pressure-reducing cushioning tank simultaneously connects vacuum pump；Sweating ware collet and removable coil pipe are connect with the circulatory system, using water as medium；
The heating function for starting the circulatory system, makes recirculated water be warming up to 70 DEG C.Water is padded below sweating ware ware plate.
With 66#Semi-refined wax (with embodiment 1) is raw material, and sweating ware is added after heating fusing.Coil pipe is immersed in paraffin
It is in layer and fixed.
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, so that wax layer temperature is dropped to 67.0 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
56.0 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.
(3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (II) is to receive under wax.On wax layer surface, level is put
Set first piece of aforementioned stainless steel plate.Connect sweating ware sealing device for upper portion of annular.Starting compressor simultaneously keeps pressure in pressurized buffer tank
Stablize in 110~130kPa(gauge pressure), sweating ware ware plate lower section keeps normal pressure.Start circulation system function, with 1.5 DEG C/h
Heating rate so that wax layer temperature is increased to 62.0 DEG C.
Stop compressor.Remove sealing device.Second piece of aforementioned stainless steel plate is placed on wax layer surface.Starting vacuum pump is simultaneously protected
Surge tank internal pressure strong stability is held in -40~-60 kPa(gauge pressures), wax layer top air pressure keeps normal pressure.Continue with the liter of 1.5 DEG C/h
Warm rate makes wax layer temperature be increased to 68.0 DEG C.The aforementioned stainless steel plate of third block is placed on wax layer surface, is continued constant temperature 4.0 hours
So that the wax in wax layer is sufficiently separated with oil.Stop vacuum pump, terminates sweating degreasing process.
The outlet of sweating ware is changed to connection crude product storage tank (II) to receive on wax.Continue increase circulating water temperature to 85 DEG C,
It is taken out on wax with fusing, as crude product (II).
(4) product purification
Crude product (II) is explosive after clay-filtered, molding, packaging with insensitiveness wax product (III).
Explosive insensitiveness wax product (III) property: 72.68 DEG C of fusing point；Oil content 0.21%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.The yield of explosive insensitiveness wax product (III) is 25.2%(relative to raw material 66#Half
Refine wax).
(5) product preparing
Explosive is weighed with No. 70 semi-refined waxs (with embodiment 1) by weight for the ratio of 60%:40% with insensitiveness wax (III), is added
Heat is melted and is uniformly mixed to 90 DEG C, is explosive insensitiveness wax product (IV) after forming, packing.
Explosive insensitiveness wax product (IV) property: 71.86 DEG C of fusing point；Oil content 0.46%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.
The production method that can be seen that sweating of the present invention and explosive insensitiveness wax by embodiment 1-2 is pressurizeed by increasing
And/or the improvement to sweatbox such as vacuum facility；By placing solid mass in wax layer, and it is strong in heating sweating effort
Improvement of the air-flow processed by wax layer, the constant temperature stage for increasing cooling and temperature-rise period etc. to sweating process；Enhance wax and oil
Separating effect simultaneously accelerates separating rate, so that sweating de-oiling technique be allow to produce fusing point between 70 DEG C~80 DEG C, oil-containing
Amount is less than 0.5%, the insensitiveness wax product of the explosive without mechanical admixture.It can be reduced and be produced by the allotment with general goods paraffin
This.
Claims (24)
1. a kind of sweating and the method for producing explosive insensitiveness wax, including the following contents:
(1) charge: the paraffin for being 60 DEG C~74 DEG C using fusing point is packed into sweatbox after heating fusing as raw material；
(2) wax layer cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization: is cooled to by original with 1.0 DEG C/h~3.0 DEG C/h rate
Expect -1.0 DEG C of paraffin melting point~+2.0 DEG C of fusing point proper temperature, high temperature constant temperature is for a period of time；Again with 0.5 DEG C/h~2.5 DEG C/h
Rate cool to 5 DEG C below raw material fusing point~20 DEG C of cooling final temperature, and cryogenic thermostat is for a period of time；
(3) heating-constant temperature sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate；Wax layer reaches predetermined temperature and one section of constant temperature
Stop sweating after time, the predetermined temperature is lower than 1 DEG C~10 DEG C of fusing point of explosive insensitiveness wax；It is forced in sweating effort
Air-flow places solid mass by wax layer, and on wax layer surface to apply the pressure of 0.5kPa or more, the solid to wax layer
There is perforative hole up and down inside weight；
(4) refine: on wax after refining be explosive insensitiveness wax product or be used as explosive insensitiveness wax product blend component.
2. according to the method for claim 1, which is characterized in that the solid mass surfacing, overall dimensions are smaller
In sweatbox inner wall size.
3. according to the method for claim 1, which is characterized in that the density of the solid mass is greater than 4g/cm3。
4. according to the method for claim 3, which is characterized in that the density of the solid mass is 6~12g/cm3。
5. according to the method for claim 1, which is characterized in that described to place solid mass using following on wax layer surface
Mode: the solid mass that can produce 0.5kPa or more pressure is added at one time in sweating effort.
6. according to the method for claim 5, which is characterized in that be added at one time when sweating starts and can produce 1.4~
The solid mass of 20.0kPa pressure.
7. according to the method for claim 1, which is characterized in that described to place solid mass using following on wax layer surface
Mode: being added several times in sweating effort, i.e., the solid weight that can produce 0.5kPa or more pressure is added in every 0.1~20.0 h
Object.
8. according to the method for claim 7, which is characterized in that being added in every 0.1~10.0 h can produce 1.4~10.0
The solid mass of kPa pressure.
9. according to the method for claim 1, which is characterized in that force air flow through wax layer use described in step (3)
Increase air pressure above wax layer and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize, the pressure
Poor by force is 10~500 kPa.
10. according to the method for claim 9, which is characterized in that the pressure difference is 20~200 kPa.
11. according to the method for claim 1, which is characterized in that the melting point of paraffin wax is 64 DEG C~70 DEG C, oil content
Less than 2.0%.
12. according to the method for claim 1, which is characterized in that temperature-fall period is before high-temperature constant temperature section in step (2)
Rate of temperature fall is 1.5 DEG C/h~2.5 DEG C/h, and the rate of temperature fall after high-temperature constant temperature section is 1.0 DEG C/h~2.0 DEG C/h.
13. according to the method for claim 1, which is characterized in that proper temperature described in step (2) is molten for starting paraffin
Point~+1.0 DEG C of fusing point.
14. according to the method for claim 1, which is characterized in that the time of the high-temperature constant temperature section of temperature-fall period in step (2)
It is 0.1~4.0 hour, the time in cryogenic thermostat stage is 0.1~3.0 hour.
15. according to the method for claim 1, which is characterized in that cooling final temperature described in step (2) is raw material stone
8 DEG C~15 DEG C below the fusing point of wax.
16. according to the method for claim 1, which is characterized in that the heating rate of sweating effort described in step (3) is
1.0 DEG C/h~2.0 DEG C/h.
17. according to the method for claim 1, which is characterized in that the time of constant temperature described in step (3) is 0.1~5.0 small
When.
18. according to the method for claim 9, which is characterized in that forcing air flow through wax layer described in step (3) is to adopt
Increase what air pressure was realized above wax layer: applying the gauge pressure pressure of 20~150 kPa above wax layer, and kept below wax layer
For normal pressure.
19. according to the method for claim 9, which is characterized in that forcing air flow through wax layer described in step (3) is to adopt
Reduce what air pressure was realized below wax layer: air pressure keeps normal pressure above wax layer, and -20~-80 are maintained below wax layer
The gauge pressure pressure of kPa.
20. according to the method for claim 1, which is characterized in that force air flow through wax layer described in step (3) and rising
Warm sweating initial stage implements.
21. according to the method for claim 1, which is characterized in that be used as explosive insensitiveness in step (4) on wax after refining
Wax product blend component.
22. according to the method for claim 21, which is characterized in that further include step (5): acquired blend component and commodity
Paraffin allotment, molding obtain explosive insensitiveness wax product after packing；The fusing point of the allotment paraffin grade wax is 64 DEG C~74
DEG C, oil content be 0.5%~2.0%；The allotment ratio of blend component and paraffin grade wax is 10%~99.9%:0.1%~90%.
23. according to the method for claim 22, which is characterized in that the fusing point of the described allotment paraffin grade wax is 68 DEG C~
72 DEG C, oil content be 0.5%~1.0%.
24. according to the method for claim 1, which is characterized in that the sweatbox is sweating ware.
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| CN201510928616.XA CN106883878B (en) | 2015-12-15 | 2015-12-15 | A kind of sweating and the method for producing 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 |
| CN1760278A (en) * | 2004-10-12 | 2006-04-19 | 中国石油天然气股份有限公司 | Wax-for preventing rubber |
| CN101649119A (en) * | 2009-03-20 | 2010-02-17 | 上海绿菱特种蜡制品厂 | Novel rubber protective wax |
-
2015
- 2015-12-15 CN CN201510928616.XA patent/CN106883878B/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 |
| CN1760278A (en) * | 2004-10-12 | 2006-04-19 | 中国石油天然气股份有限公司 | Wax-for preventing rubber |
| CN101649119A (en) * | 2009-03-20 | 2010-02-17 | 上海绿菱特种蜡制品厂 | Novel rubber protective wax |
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