CN106883082B - A method of producing explosive insensitiveness wax - Google Patents
A method of producing explosive insensitiveness wax Download PDFInfo
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- CN106883082B CN106883082B CN201510928607.0A CN201510928607A CN106883082B CN 106883082 B CN106883082 B CN 106883082B CN 201510928607 A CN201510928607 A CN 201510928607A CN 106883082 B CN106883082 B CN 106883082B
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- 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
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Abstract
The invention discloses a kind of methods for producing explosive insensitiveness wax.This method is on the basis of common sweating process, the oil of liquid is carried out to force separation wax and oil by wax layer using air-flow in sweating effort, generation gas is decomposed using inorganic salts simultaneously, and short space is formed in wax layer, it is also beneficial to the quick discharge of oil, so that this solvent-free de-oiling method of sweating 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 method for producing explosive insensitiveness wax.
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.With scientific skill
The development of art, various explosives develop in terms of high-power, high security, and currently used explosive is that TNT, high explosive are black
Suo Jin (RDX, three ammonium nitrate of ring cyclonite) and octogen (HMX, cyclotetramethyltetranitrosamine) etc..
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 has at home and abroad continued to use over half a century as the deterrent of explosive, its efficient insensitive action is
For recognized by people.Explosive insensitiveness wax has highly important effect to the insensitiveness of explosive, is to ensure that explosive in storage, fortune
In the defeated, entire life cycle that uses an important factor for safety.The insensitiveness wax of some special dynamites requires fusing point 70 DEG C~80
Between DEG C, oil content less than 0.5%, without mechanical admixture.Common petroleum wax oil content of the fusing point between 70 DEG C~80 DEG C usually exists
Between 0.8%~2.0%, it is not able to satisfy the requirement of certain special dynamite insensitiveness waxes.
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, isoparaffin and a small amount of cycloalkane, usual fusing point is 50 DEG C~
74℃.Microwax be decompression residuum after propane equal solvent depitching again through dewaxing, de-oiling, purification and molding and etc. production
, generally by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition, usual dropping point be 65 DEG C~92 DEG C, Gu
There is the needle-like crystal structure more tiny than paraffin under state.
Dewaxing is that the process for the slack wax that oil content is 10~30% or so, dewaxing technique are prepared 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 prepared 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 de-oiling of current large-scale production pertroleum wax
Technique.But solvent deoiling technique investment of production equipment is big；It needs largely to use solvent in production process, recycling design needs to consume
A large amount of energy；Contain 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；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will be lower than n-alkane, and isomery degree gets over high-melting-point just
It is lower, or even be 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 (with water full of sweatbox
Ware plate lower space) charge (raw material is heated to being packed into sweatbox when fusing point or more is in a liquid state) afterwards；(2) crystallize: by raw material with
Rate of temperature fall no more than 4 DEG C/h progressively cools to 10~20 DEG C of its fusing point or less.In cooling procedure, various components press fusing point
Sequence from high to low successively crystallizes and forms solid；(3) sweating: after wax layer temperature reaches preset cooling final temperature,
Bleed off pad water；Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components by fusing point by
Low to high sequence be successively fused into liquid and flow out the wax layer residue (on wax) finally obtained (under wax) be exactly high-melting-point,
The wax of low oil-containing；Continue to increase temperature, be taken out on wax with fusing, as crude product；(4) it refines: generalling use clay-filtered (incite somebody to action
It is warming up to predetermined temperature after crude product fusing, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the predetermined time)；It formed, packed again
It is purpose 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 oil wax product when, even if using sweating sessions and the method that improves sweating final temperature, sweating is extended
Oil content on later period wax is unrelated with yield, i.e., the oil content on wax does not decline with the decline of yield, so common sweating is de-
Oily 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 skill
Art index request.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is lower, the production cycle is longer, but
Be sweating de-oiling technique have small investment, production process is simple, operating cost is low, production process is safe, it is energy saving and to environment without
The advantages that pollution, still has part of the manufacturer producing soap manufacturing paraffin product using this method at present.
For many years, sweating method has obtained some development in production equipment and process aspect, such as CN89214332(vertical type square
Shape multipul sections spacer diaphoresis tank), CN94223980.6(ware type sudorific device), CN98233254.8(Paraffin sweating pot),
CN200920033500.X(novel paraffin sweating tank), a kind of Efficient paraffin sweatbox of CN201210508905.0(),
CN201320127680.4(tubular type paraffin deoiler) etc., it is improved in sweating 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~
Between 80 DEG C, the oil content insensitiveness wax product of the explosive less than 0.5%.
Sweating process is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product, is being mentioned
It is the today for advocating green low-carbon, environmental protection and energy saving, more urgent with the demand of insensitiveness wax product using sweating process production explosive.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of method for producing explosive insensitiveness wax, specifically adopts
The oil of liquid is carried out by wax layer using air-flow in sweating effort on the basis of common sweating process with sweatbox
To force separation wax and oil, enhances separating effect and accelerate separating rate；Preferably in pressure condition after raw material heating fusing
The lower decomposable inorganic salt powder for generating gas of incorporation；And increase high temperature constant temperature stage and the cryogenic thermostat stage of crystallization process with
And the constant temperature stage of sweating effort, so that this solvent-free de-oiling method of sweating is produced explosive insensitiveness wax product.It can also
Explosive insensitiveness wax product is produced in a manner of using sweating product and paraffin grade wax to deploy to reduce production cost.
A kind of method producing explosive insensitiveness wax of the invention, 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 is less than 2.0%；Fusing point is general
It is 60 DEG C~74 DEG C, preferably 64 DEG C~70 DEG C.
It in step (1), generally heats the raw material to more than raw material fusing point 1 DEG C~5 DEG C, raw material is all melted.
Process of the present invention it is preferred incorporation can decompose the nothing for generating gas under stress after raw material heating fusing
Machine salt powder, the pressure are generally (gauge pressure) 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.It is described
Inorganic salt powder can slowly be decomposed in sweating effort and release gas and itself and decomposition product is soluble easily in water, can be with
It is one or more of ammonium salt, carbonate, bicarbonate.The granularity of the inorganic salt powder is 50~500 mesh, additional amount
Account for 0.1%~10.0%(weight of starting paraffin), preferred ratio is 0.2%~3.0%.In the cryogenic thermostat process and hair of crystallization
Inorganic salts are absorbed during sweat decomposes the pernicious gas generated.It is unreacted inorganic using water-washing method removal in subtractive process
Salt and decomposition product.
In method of the invention, the sweatbox is sweating ware, and in wax layer dismountable sealing system added above
System and pressurizing device, to inhibit nothing during step (1) charging process and the temperature-fall period and high temperature constant temperature of step (2) crystallization
Machine salt decomposes the gas generated and escapes wax layer.The pressure (gauge pressure) be 0.5~15.0 atmospheric pressure, preferably 1.0~8.0
A atmospheric pressure.
In method of the invention, the sweating ware increases in wax layer pressurizing device added above and/or below wax layer
Vacuum plant.In step (3) sweating effort, it is described force air flow through wax layer use increase above wax layer air pressure and/
Or air pressure is reduced below wax layer, so that wax layer upper and lower is formed pressure difference and realizes.The pressure difference is generally 0.1~5.0
Atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force air flow through wax layer.
In method of the invention, in the temperature-fall period of step (2) 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 starting paraffin fusing point or less.The drop
After temperature to final temperature, increase the cryogenic thermostat stage so that solid crystal is more abundant, the time in cryogenic thermostat stage is 0~3.0
Hour, preferably 0.1~3.0 hour, more preferably 1.0~3.0 hours.Pressure is gradually decreased while cryogenic thermostat to normal
Pressure, rate of pressure reduction are generally 0.1~150 atm/h, preferably 0.3~8 atm/h.
In method of the invention, heating rate preferably 1.0 DEG C/h~2.0 DEG C/h of step (3) sweating effort.It is described
The predetermined temperature (i.e. final temperature) of heating is lower than 1 DEG C~10 DEG C of fusing point of purpose product.
In method of the invention, after step (3) sweating is warming up to the predetermined temperature for producing product, increase the constant temperature stage
Wax can be made to separate with oil more sufficiently, time in constant temperature stage is 0~5.0 hour, preferably 0.1~5.0 hour, most preferably
1.0~5.0 hours.
In method of the invention, the heating rate and cooling rate of said wax layer can pass through air bath, water-bath, oil bath
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer heating is controlled using water-bath or oil bath mode
When rate and rate of temperature fall, collet can be increased outside sweating ware, collet is connected with removable coil pipe and the circulatory system, collet, disk
Pipe etc. can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature；The circulatory system has program cooling/heating function, circulation
The substances such as water or conduction oil are added as circulatory mediator in system.
In method of the invention, the wax layer that forces air flow through of step (3) sweating effort can be in sweating effort times
The meaning stage implements, and preferably implements at sweating initial stage.
In method of the invention, the wax layer that forces air flow through of step (3) sweating effort is utilized in above wax layer
Increase what air pressure was realized, can such as apply the pressure of 0.2~1.5 atmospheric pressure (gauge pressure) above wax layer, and is kept below wax layer
For normal pressure.
In method of the invention, the wax layer that forces air flow through of step (3) sweating effort is utilized in below wax layer
It reduces what air pressure was realized, normal pressure can be such as kept above wax layer, and maintain -0.2~-1.0 atmospheric pressure (tables below wax layer
Pressure) pressure.
In method of the invention, the sweatbox can also connect absorption system, in the cryogenic thermostat mistake of crystallization
Inorganic salts are absorbed in journey and sweating effort decomposes the pernicious gas generated.Absorption system uses liquid absorption mode.
In method of the invention, blend component obtained by step (4) refines can be deployed with paraffin grade wax to reduce cost,
Explosive insensitiveness wax product is obtained after molding, packaging.Therefore, the method for the present invention can also include step (5): acquired reconciliation
Component and paraffin grade wax are deployed, and obtain explosive insensitiveness wax product after molding, packaging；The allotment fusing point of paraffin grade wax
For 64 DEG C~74 DEG C, oil content be 0.5%~2.0%；Preferably 68 DEG C~72 DEG C of fusing point, oil content are 0.5%~1.0%.It reconciles
Component and the allotment weight ratio of paraffin grade wax are 10%~99.9%:0.1~90%, preferably 10%~90%:10~90%.
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 pertroleum wax method be suitable for production explosive insensitiveness wax
Product is difficult to separate reason with oil for wax by the further investigation to common sweating effort, by using in sweating effort
Wax layer is forced air flow through, and increases the perseverance of high temperature constant temperature stage and cryogenic thermostat stage and sweating effort in crystallization process
The processes such as thermophase；Incorporation can decompose the inorganic salt fines for generating gas under stress further preferably after raw material heating fusing simultaneously
End, these measures significantly reduce the oil content of product, can satisfy the technical requirements of 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；In temperature-fall period
Increasing the high temperature constant temperature stage can make the crystallization of pertroleum wax bigger, be conducive to discharge oily in sweating effort.For pertroleum wax knot
Brilliant process studies have shown that the chemical composition of pertroleum wax is to determine the main factor of crystal habit, while the item of cooling procedure
Part 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 with
As the nucleus for being subsequently formed crystallization, increase the high temperature constant temperature stage at this time, nucleus can be enable sufficiently to increase, forms bigger ruler
Very little crystal, although this larger sized crystal is coarse not as good as the crystallization of low melt point paraffin, the crystal of this increase
Structure is also highly beneficial to sweating stage discharge oil.Incorporation can divide under stress after the fusing of preferred raw material heating simultaneously
Solution generates the inorganic salt powder of gas, these substances slowly settle in the wax layer of liquid due to granularity is smaller.Keep pressure strip
Raw material is cooled to 10 DEG C~15 DEG C of fusing point or less under part, and constant temperature 0.1h~3.0h is so that wax layer crystallization is more abundant；Exist simultaneously
Pressure is gradually decreased in thermostatic process to normal pressure.Raw material is cooled in the time terminated after fusing point or less to sweating effort at wax layer
In softer solid state, inorganic salts slowly decompose the gas released during this, micro-bubble can be formed in wax layer, this
The space that minute bubbles are formed slightly is easy to be formed in sweating effort several tiny channels in wax layer, to be conducive to sweating
Oily discharge in the process.The cryogenic thermostat stage for being aided with crystallization process again keeps solid crystal more abundant and the perseverance of sweating effort
It is the methods of more abundant that thermophase separates wax with oil, and sweating de-oiling technique is allow to produce explosive insensitiveness wax product.
By select fusing point for 64 DEG C~74 DEG C, oil content be 0.5%~2.0%, preferably fusing point be 68 DEG C~72 DEG C, oil-containing
Amount is deployed for 0.5%~1.0% commodity oil wax and sweating product, can reduce production cost.
This have the advantage that: the method by using air-flow to carry out fluid oil by wax layer in sweating effort
The separation for forcing wax and oil, enhances separating effect and accelerates separating rate；The gas generated is decomposed using inorganic salts simultaneously
Short space is formed in wax layer, is also beneficial to the quick discharge of oil；And increase high temperature constant temperature stage and the low temperature of crystallization process
The processes such as constant temperature stage and the constant temperature stage of sweating effort, so that sweating process be allow to produce explosive insensitiveness wax product.
Method of the invention has that plant investment is low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution environment
The advantages that.
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；Raw material heating is melted and is filled after preferably mixing inorganic salt powder under stress
Enter sweating ware；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature is down near raw material melting temperature simultaneously one section of high temperature constant temperature
Time；Continue to be cooled to preset temperature and cryogenic thermostat for a period of time；Wax layer heating reaches preset temperature and constant temperature for a period of time
After stop sweating effort；In sweating effort, start compressor in wax layer positive pressure formed above, and/or starting vacuum pump with
In wax layer negative pressure formed below, to force air flow through wax layer；Through purification, (being deployed with paraffin grade wax) molding, packaging on wax
It is afterwards explosive insensitiveness wax product.
The method of present invention production explosive insensitiveness wax is illustrated by the following examples.
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
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；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.The sealing system on sweating ware top is installed and is connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump；Starting compressor simultaneously keeps pressurized buffer pressure inside the tank steady
It is scheduled on 3.2~3.4 atmospheric pressure (gauge pressure).
With 66#Semi-refined wax (Jinan petro-chemical corporation, 66.35 DEG C of fusing point, oil content 0.76%) is raw material, is heated to 70 DEG C and melts
Sweating ware is added after change under 3.2~3.4 atmospheric pressure (gauge pressure).
(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.The constant temperature stage is slow by emptying system control pressurization
It rushes pressure inside the tank and is gradually decrease to normal pressure with 5.0 atmospheric pressure/h rates.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；Start compressor and keeps adding
Pressure buffering pressure inside the tank is stablized keeps normal pressure below 1.1~1.3 atmospheric pressure (gauge pressure), sweating ware ware plate；Start cyclic system
System heating function, makes wax layer temperature be increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h；Stop compressor.
Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize on -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer
Square air pressure keeps normal pressure；Continue to make with the heating rate of 2.0 DEG C/h wax layer temperature to be increased to 68.0 DEG C and constant temperature 4.0 hours so that
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 to increase circulating water temperature to 85 DEG C, is taken out on wax with fusing, as crude product (I).
(4) product purification
Crude product (I) is explosive with insensitiveness wax product (I) after washing, clay-filtered, molding, packaging.
Explosive insensitiveness wax product (I) property: 72.58 DEG C of fusing point；Oil content 0.39%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.The yield of explosive insensitiveness wax product (I) is 17.6%(relative to raw material 66#Half
Refine wax).
(5) product preparing
Explosive with insensitiveness wax product (I) and No. 70 semi-refined waxs (Dalian Petrochemical Industry Company, 70.35 DEG C of fusing point；Oil content 0.81%)
It is weighed by weight for the ratio of 80%:20%, is heated to 90 DEG C and melts and be uniformly mixed, as explosive is with blunt after forming, pack
Feel wax product (II).
Explosive insensitiveness wax product (II) property: 72.10 DEG C of fusing point；Oil content 0.48%；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
Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；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.The sealing system on sweating ware top is installed and is connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump；Pressurized buffer tank emptying system and sweating ware lower part are arranged
Port is connected with gas absorption system respectively, using 5% NaOH solution as absorbing medium.
Starting compressor simultaneously keeps pressurized buffer pressure inside the tank to stablize in 3.2~3.4 atmospheric pressure (gauge pressure).It grinds and sieves
Separate 100 mesh~200 mesh sodium bicarbonate.
With 66#Semi-refined wax (with embodiment 1) is raw material, is heated to after 70 DEG C of fusings in 3.2~3.4 atmospheric pressure (gauge pressure)
The aforementioned sodium bicarbonate powder of lower incorporation 1.0%, is added sweating ware after mixing；Pressurized buffer pressure inside the tank is kept to stablize
3.2~3.4 atmospheric pressure.
(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.The cryogenic thermostat stage is added by emptying system control
Pressure buffering pressure inside the tank, is gradually decrease to normal pressure with 5.0 atmospheric pressure/h rates.The cryogenic thermostat stage gas of discharge passes through
5% NaOH solution decomposes the carbon dioxide generated to absorb sodium bicarbonate.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；Starting compressor is simultaneously kept
Pressurized buffer pressure inside the tank is stablized keeps normal pressure below 1.1~1.3 atmospheric pressure (gauge pressure), sweating ware ware plate；Starting circulation
System heating function makes wax layer temperature be increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h；Stop compressor.
Starting vacuum pump simultaneously keeps pressure-reducing cushioning pressure inside the tank to stablize on -0.4~-0.6 atmospheric pressure (gauge pressure), wax layer
Square air pressure keeps normal pressure；Continue to make with the heating rate of 2.0 DEG C/h wax layer temperature to be increased to 68.0 DEG C and constant temperature 4.0 hours so that
Wax in wax layer is sufficiently separated with oil.The gas being discharged in sweating effort absorbs sodium bicarbonate decomposition by 5% NaOH solution
The carbon dioxide of generation.
Stop vacuum pump, terminates sweating effort.The outlet of sweating ware is changed to connection crude product storage tank (II) to receive on wax.Continue
Circulating water temperature is increased to 85 DEG C, is taken out on wax with fusing, as crude product (II).
(4) product purification
Crude product (II) through washing, it is clay-filtered be explosive with insensitiveness wax product (III).
Explosive insensitiveness wax product (III) property: 72.60 DEG C of fusing point；Oil content 0.23%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.The yield of explosive insensitiveness wax product (III) is 22.9%(relative to raw material 66#Half
Refine wax).
(5) product preparing
Explosive insensitiveness wax product (III) claims with No. 70 semi-refined waxs (with embodiment 1) by weight for the ratio of 60%:40%
It takes, is heated to 90 DEG C and melts and be uniformly mixed, be explosive insensitiveness wax product (IV) after forming, packing.
Explosive insensitiveness wax product (IV) property: 71.62 DEG C of fusing point；Oil content 0.47%；Mechanical admixture, nothing.Meet explosive
With the associated specifications of insensitiveness wax product.
The production method that can be seen that explosive insensitiveness wax of the present invention by embodiment 1-2, by increase pressurization and/or
The improvement to sweatbox such as vacuum facility；It is decomposed using inorganic salts and forms short space in wax layer and in heating sweating effort
In force air flow through the improvement to sweating process such as wax layer；It enhances the separating effect of wax and oil and accelerates separating rate,
To allow sweating de-oiling technique to produce fusing point between 70 DEG C~80 DEG C, oil content frying less than 0.5%, without mechanical admixture
Medicinal insensitiveness wax product.Production cost can be reduced by the allotment with general goods paraffin.
Claims (20)
1. a kind of 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 raw material, the decomposable life of incorporation under stress after heating fusing
At the inorganic salt powder of gas, it is packed into sweatbox；
(2) cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization: wax layer is cooled to 1.0 DEG C/h~3.0 DEG C/h rate suitable
Work as temperature, high temperature constant temperature 0.1~4.0 hour；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 0.1~3.0 hour；
(3) heating-constant temperature sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate, wax layer reach predetermined temperature and constant temperature 0.1~
Stop sweating after 5.0 hours；Wax layer is forced air flow through in sweating effort；
(4) refine: on wax after refining, as explosive insensitiveness wax product or be used as explosive insensitiveness wax product blend component；
Wherein, proper temperature described in step (2) is -1.0 DEG C of starting paraffin fusing point~+2.0 DEG C of fusing point, institute in step (3)
The predetermined temperature stated is lower than 1 DEG C~10 DEG C of purpose product fusing point.
2. according to the method for claim 1, which is characterized in that the inorganic salt powder decomposes release in sweating effort
Gas out, and itself and decomposition product are soluble easily in water.
3. according to the method for claim 1, which is characterized in that the inorganic salts are selected from ammonium salt, carbonate, bicarbonate
One or more of.
4. according to the method for claim 1, which is characterized in that the granularity of the inorganic salt powder is 50~500 mesh.
5. according to the method for claim 2, which is characterized in that the additional amount of the inorganic salt powder accounts for raw material weight
0.1%~10.0%.
6. according to the method for claim 1, which is characterized in that the pressure is 0.5~15.0 atmosphere of gauge
Pressure.
7. according to the method for claim 1, which is characterized in that in the cooling that step (1) charging process and step (2) crystallize
Apply air pressure above wax layer during process and high temperature constant temperature, the gas generated to inhibit inorganic salts to decompose escapes wax layer, institute
The air pressure stated is 0.5~15.0 atmospheric pressure of gauge.
8. according to the method for claim 1, which is characterized in that force air flow through wax layer use described in step (3)
Increase air pressure above wax layer and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize, the pressure
Power difference is 0.1~5.0 atmospheric pressure.
9. according to the method for claim 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.
10. 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 wax fusing point.
11. according to the method for claim 1, which is characterized in that step gradually decreases pressure in (2) while cryogenic thermostat
For power to normal pressure, rate of pressure reduction is 0.1~150 atm/h.
12. 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.
13. according to the method for claim 1, which is characterized in that force air flow through wax layer described in step (3) and sending out
Sweat initial stage implements.
14. according to the method for claim 8, which is characterized in that force air flow through wax layer use described in step (3)
Increase air pressure above wax layer to realize, apply the gauge of 0.2~2.0 atmospheric pressure above wax layer, and is protected below wax layer
It holds as normal pressure.
15. according to the method for claim 8, which is characterized in that force air flow through wax layer use described in step (3)
Air pressure is reduced below wax layer and realizes that air pressure keeps normal pressure above wax layer, and remains -0.2~-1.0 big below wax layer
The gauge of air pressure.
16. according to the method for claim 1, which is characterized in that adopted in the cryogenic thermostat process and sweating effort of crystallization
Inorganic salts are absorbed with liquid absorption mode and decompose the pernicious gas generated, and unreacted is removed using water-washing method in subtractive process
Inorganic salts and decomposition product.
17. 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.
18. according to the method for claim 17, 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 0.5wt%~2.0wt%；The allotment weight ratio of blend component and paraffin grade wax be 10%~99.9%:0.1~
90%。
19. according to the method for claim 1, which is characterized in that the sweatbox is sweating ware.
20. according to the method for claim 8, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.
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| CN201510928607.0A CN106883082B (en) | 2015-12-15 | 2015-12-15 | A method of producing explosive insensitiveness wax |
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|---|---|---|---|---|
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN1189527A (en) * | 1997-01-27 | 1998-08-05 | 王福祥 | Quick sweating wax making tech. |
| CN1289745A (en) * | 1999-09-29 | 2001-04-04 | 中国石油化工集团公司 | Composite wax for powdered nitramon explosive |
| CN101172914A (en) * | 2006-11-01 | 2008-05-07 | 中国石油化工股份有限公司 | Composite wax for powder emulsifying blasting agent |
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2015
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Patent Citations (4)
| 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. |
| CN1289745A (en) * | 1999-09-29 | 2001-04-04 | 中国石油化工集团公司 | Composite wax for powdered nitramon explosive |
| CN101172914A (en) * | 2006-11-01 | 2008-05-07 | 中国石油化工股份有限公司 | Composite wax for powder emulsifying blasting agent |
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