CN106883082A - A kind of method for producing explosive insensitiveness wax - Google Patents
A kind of method for producing explosive insensitiveness wax Download PDFInfo
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- CN106883082A CN106883082A CN201510928607.0A CN201510928607A CN106883082A CN 106883082 A CN106883082 A CN 106883082A CN 201510928607 A CN201510928607 A CN 201510928607A CN 106883082 A CN106883082 A CN 106883082A
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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 method for producing explosive insensitiveness wax.The method is on the basis of common sweating process, the oil of liquid is carried out to force to separate wax and oil by wax layer using air-flow in sweating effort, being decomposed using inorganic salts simultaneously produces gas that short space is formed in wax layer, the quick discharge of oil is also beneficial to, so that this solvent-free de-oiling method of sweating can produce explosive insensitiveness wax product.The inventive method has the advantages 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 field, more particularly to a kind of method for producing explosive insensitiveness wax.
Background technology
Explosive can be the material for rapidly burning or decomposing, under certain outside energy effect, can in very short time vigorous combustion（Explode）Substantial amounts of heat and gas are produced, the detonation formula acting stablized to external world.With the development of science and technology, various explosives develop in terms of high-power, high security, and conventional explosive is TNT, high explosive RDX at present（RDX, the ammonium nitrate of ring cyclonite three）And HMX（HMX, HMX）Deng.
Under given conditions, the various sensitivity of explosive have close relationship with the security that powder charge is used, and various sensitivity are lower within the specific limits, and 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 high explosives, very well or the performance with certain special requirement, simply security is poor for their other explosion propertys, the use requirement of high-power and high security can not simultaneously be met, it is necessary to consider for sensitivity to give insensitiveness or insensitiveness treatment with different methods.
Explosive phlegmatizer refers to the material for reducing 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, and its efficient insensitive action has been recognized by people.Explosive insensitiveness wax has highly important effect to the insensitiveness of explosive, is to ensure that the key factor of explosive security in the entire life cycle for storing, transporting, using.The insensitiveness wax requirement fusing point of some special dynamites is between 70 DEG C~80 DEG C, oil content is less than 0.5%, mechanical impurity.Common petroleum wax oil content of the fusing point between 70 DEG C~80 DEG C is generally between 0.8%~2.0%, it is impossible to meet the requirement of some special dynamite insensitiveness waxes.
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 atoleine, soap manufacturing 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 contains C20~C50The component such as n-alkane, isoparaffin and a small amount of cycloalkane, usual fusing point is 50 DEG C~74 DEG C.Microwax is that decompression residuum is produced through steps such as dewaxing, de-oiling, refined and shapings again after propane equal solvent depitching, typically by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition, usual melt drop temperature be 65 DEG C~92 DEG C, under solid-state have the needle-like crystal structure more tiny than paraffin.
Dewaxing is the process for preparing the slack wax that oil content is 10~30% or so as raw material with lube cut, and dewaxing technique mainly has squeezing to dewax and solvent dewaxing.De-oiling is the process for preparing base oil wax of the oil content below 2% as raw material with slack wax, and de-oiling technique mainly has solvent deoiling and sweating de-oiling.Base oil wax is again through clay-filtered or hydrofinishing and shaping, packaging and other steps, you can obtain commodity oil wax.
Solvent deoiling method is in selective solvent according to wax with oil（Acetone, benzene and toluene mixture；Or acetone, toluene；Or MEK, toluene）What the property of middle different solubility was separate.Solvent deoiling technique has the advantages that production process is continuous, wax high income, finished product wax oil content can very low, production cost it is relatively low, be the main flow de-oiling technique for mass producing pertroleum wax at present.But solvent deoiling technique productions equipment investment is big；Needed in production process largely using solvent, recycling design needs to consume substantial amounts of energy；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.The molecular weight of various hydro carbons and structure Bu Tong can all make its fusing point different in pertroleum wax.When being all n-alkane structure, the fusing point of the larger n-alkane of molecular weight is higher；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will be less than n-alkane, and isomery degree more high-melting-point is lower, or even be in just at normal temperatures liquid condition, i.e., usually said oil.
Common sweating de-oiling technique is mainly included the following steps that：（1）Preparation：Pad water（Sweatbox ware plate lower space is full of with water）After feed（Load sweatbox when raw material is heated to more than fusing point being in a liquid state）；（2）Crystallization：Raw material is progressively cooled to 10~20 DEG C below its fusing point with being not more than the rate of temperature fall of 4 DEG C/h.In cooling procedure, order of the various components by fusing point from high to low crystallizes to form solid successively；（3）Sweating：After wax layer temperature reaches default cooling final temperature, pad water is bled off；Raw material is lentamente heated to default sweating final temperature again.In sweating effort, order of the various components by fusing point from low to high is successively fused into liquid and flows out（Under wax）, the wax layer residue for finally obtaining（On wax）It is exactly high-melting-point, the wax of low oil-containing；Continue to rise high-temperature, taken out on wax with melting, as crude product；（4）It is refined：Generally using clay-filtered（Predetermined temperature is warming up to after crude product is melted, carclazyte is added and constant temperature is stirred to the scheduled time filtering）；It is again purpose product through shaping, packaging.
Common sweating de-oiling technique can produce soap manufacturing paraffin and low melt point paraffin of the fusing point at 40 DEG C~60 DEG C, be not suitable for producing 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 in 70 DEG C or so of high melting point oil wax product, even if the method using sweating sessions are extended and improve sweating final temperature, oil content on sweating later stage wax is unrelated with yield, oil content i.e. 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, especially oil-containing figureofmerit can not meet technical requirement.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is relatively low, the production cycle is more long, but sweating de-oiling technique has the advantages that small investment, production process are simple, operating cost is low, production process safety, energy-conservation and environmentally safe, still has part producer producing soap manufacturing paraffin product using the method at present.
For many years, sweating method has obtained some development, such as CN89214332 in production equipment and process aspect（Vertical square multipul sections spacer diaphoresis tank）、CN94223980.6（Ware type sudorific device）、CN98233254.8（Paraffin sweating pot）、CN200920033500.X（Novel paraffin sweating tank）、CN201210508905.0（A kind of Efficient paraffin sweatbox）、CN201320127680.4（Tubular type paraffin deoiler）Deng being improved in sweating de-oiling production equipment；CN91206202（A kind of high-efficient sweat pot for paraffin wax）Improved in sweating de-oiling technique, but these improvement can not still produce fusing point between 70 DEG C~80 DEG C, oil content less than 0.5% explosive insensitiveness wax product.
Sweating process is to be currently known the unique solvent-free de-oiling method for commercial scale petroleum paraffin product, is advocating today of green low-carbon, environmental protection and energy saving, more urgent with the demand of insensitiveness wax product using sweating process production explosive.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of method for producing explosive insensitiveness wax, specifically use sweatbox, on the basis of common sweating process, the oil of liquid is carried out to force to separate wax and oil by wax layer using air-flow in sweating effort, separating effect is enhanced and is accelerated separating rate；The inorganic salt powder that decomposable asymmetric choice net generates gas is preferably mixed under stress after raw material heating fusing；And increase the high temperature constant temperature stage and cryogenic thermostat stage and the constant temperature stage of sweating effort of crystallization process, this solvent-free de-oiling method of sweating is produced explosive insensitiveness wax product.Sweating product can also be used to produce explosive insensitiveness wax product to reduce production cost with the mode of paraffin grade wax allotment.
A kind of method for producing explosive insensitiveness wax of the invention, including herein below：
（1）Charging：With paraffin that fusing point is 60 DEG C~74 DEG C as raw material, sweatbox is loaded after heating fusing；
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization：Wax layer is cooled to by proper temperature with the speed of 1.0 DEG C/h~3.0 DEG C/h, high temperature constant temperature is for a period of time；Cooled to raw material fusing point 5 DEG C~20 DEG C of cooling final temperature with the speed of 0.5 DEG C/h~2.5 DEG C/h again, and cryogenic thermostat is for a period of time；
（3）The sweating of intensification-constant temperature：Heated up with the speed of 0.5 DEG C/h~2.5 DEG C/h, wax layer reaches predetermined temperature and constant temperature stops sweating afterwards for a period of time；Wax layer is forced air flow through in sweating effort；
（4）It is refined：Explosive is with insensitiveness wax product or as explosive insensitiveness wax product blend component after refined on wax.
In the method for the present invention, the oil content of the sweating raw material paraffin（In mass）Less than 2.0%；Fusing point is generally 60 DEG C~74 DEG C, preferably 64 DEG C~70 DEG C.
Step（1）In, raw material is typically heated 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 mixing the inorganic salt powder that decomposable asymmetric choice net generates gas under stress after raw material heating fusing, described pressure is generally（Gauge pressure）0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.Described inorganic salt powder can slowly be decomposed in sweating effort and discharge gas and itself and catabolite is soluble in water, can be one or more in ammonium salt, carbonate, bicarbonate.The granularity of described inorganic salt powder is 50~500 mesh, and addition accounts for the 0.1%~10.0% of starting paraffin（Weight）, preferred ratio is 0.2%~3.0%.Inorganic salts are absorbed in the cryogenic thermostat process and sweating effort of crystallization and decomposes the pernicious gas for producing.Unreacted inorganic salts and catabolite are removed using water-washing method in subtractive process.
In the method for the present invention, described sweatbox is sweating ware, and in wax layer dismountable sealing system added above and pressue device, with step（1）Charging process and step（2）Suppress inorganic salts during the temperature-fall period and high temperature constant temperature of crystallization and decompose the gas effusion wax layer for producing.Described pressure（Gauge pressure）It is 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.
In the method for the present invention, described sweating ware increases vacuum plant in wax layer pressue device added above and/or below wax layer.In step（3）In sweating effort, it is described force air flow through wax layer and use increase above wax layer air pressure and/or air pressure is reduced below wax layer, wax layer upper and lower is formed pressure differential and realize.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force air flow through wax layer.
In the method for the present invention, the step（2）In the temperature-fall period of crystallization, the rate of temperature fall preferably 1.5 DEG C/h~2.5 DEG C/h before high-temperature constant temperature section.The proper temperature of the high-temperature constant temperature section of described 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 of the process that cools is 0~4.0 hour, more preferably preferably 0.1~4.0 hour, 1.0~4.0 hours.
In the method for the present invention, the step（2）Rate of temperature fall of the temperature-fall period of crystallization after high-temperature constant temperature section preferably 1.0 DEG C/h~2.0 DEG C/h.Described cooling final temperature is preferably 8 DEG C~15 DEG C below starting paraffin fusing point.It is described be cooled to final temperature after, increase the cryogenic thermostat stage so that solid crystal is more abundant, the time in cryogenic thermostat stage is 0~3.0 hour, more preferably preferably 0.1~3.0 hour, 1.0~3.0 hours.Pressure to normal pressure is gradually reduced while cryogenic thermostat, rate of pressure reduction is generally 0.1~150 atm/h, preferably 0.3~8 atm/h.
In the method for the present invention, the step（3）The heating rate of sweating effort preferably 1.0 DEG C/h~2.0 DEG C/h.The predetermined temperature of the intensification（That is final temperature）It is 1 DEG C~10 DEG C of the fusing point less than purpose product.
In the method for the present invention, the step（3）After sweating is warming up to the predetermined temperature for producing product, the increase constant temperature stage can be such that wax is separated with oil more fully, and the time in constant temperature stage is 0~5.0 hour, most preferably preferably 0.1~5.0 hour, 1.0~5.0 hours.
In the method for the present invention, the programming rate and cooling rate of said wax layer can be controlled, it is preferred to use water-bath or oil bath by air bath, water-bath, oil bath or other feasible modes.When controlling wax layer heating rate and rate of temperature fall using water-bath or oil bath mode, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, chuck, coil pipe etc. can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature；The circulatory system has programmed cooling/heating function, and the circulatory system adds the materials such as water or conduction oil as circulatory mediator.
In the method for the present invention, the step（3）Forcing air flow through wax layer and can implementing in sweating effort any stage for sweating effort, preferably implements at the sweating initial stage.
In the method for the present invention, the step（3）The wax layer that forces air flow through of sweating effort is utilized in what increase air pressure in wax layer top was realized, and 0.2~1.5 atmospheric pressure can be such as applied above wax layer（Gauge pressure）Pressure, and wax layer lower section remain normal pressure.
In the method for the present invention, the step（3）The wax layer that forces air flow through of sweating effort is utilized in what reduction air pressure in wax layer lower section was realized, and normal pressure can be such as kept above wax layer, and -0.2~-1.0 atmospheric pressure are maintained below wax layer（Gauge pressure）Pressure.
In the method for the present invention, described sweatbox can also connect absorption system, and the pernicious gas for producing is decomposed to absorb inorganic salts in the cryogenic thermostat process and sweating effort of crystallization.Absorption system uses liquid absorption mode.
In the method for the present invention, step（4）Blend component can obtain explosive insensitiveness wax product with paraffin grade wax allotment with reduces cost after shaping, packaging obtained by refined.Therefore, the inventive method can also include step（5）：Resulting blend component is allocated with paraffin grade wax, and explosive insensitiveness wax product is obtained after shaping, packaging；The fusing point of the allotment paraffin grade wax is 64 DEG C~74 DEG C, oil content is 0.5%~2.0%；Preferably 68 DEG C~72 DEG C of fusing point, oil content are 0.5%~1.0%.Blend component is 10%~99.9% with the allotment weight ratio of paraffin grade wax：0.1~90%, preferably 10%~90%：10~90%.
Sweating de-oiling method is separated to produce pertroleum wax using the wax property different with oily fusing point, and the research for pertroleum wax sweating effort shows, in sweating effort, oil is gradually discharged along crystalline portion, similar to the situation that liquid flows in capillary.But the high melting point paraffin product for fusing point at 70 DEG C or so, because the material such as isoparaffin and cycloalkane increases in raw material, chemical composition is complicated, cause the more tiny densification of crystals upon crystallization structure, discharge to oil forms huge filter flow resistance power, and this results in and only is difficult to be kept completely separate with oil by wax in the common sweating effort of gravity natural separation.Therefore common sweating de-oiling technique can not produce fusing point in 70 DEG C~80 DEG C, explosive insensitiveness wax product of the oil content less than 0.5%.
The present invention is in order that the method for this solvent-free production pertroleum wax of sweating de-oiling is applied to production explosive insensitiveness wax product, by the further investigation to common sweating effort, it is difficult to separate reason for wax and oil, wax layer is forced air flow through by being used in sweating effort, and increases the processes such as constant temperature stage of high temperature constant temperature stage and cryogenic thermostat stage and sweating effort in crystallization process；The inorganic salt powder that decomposable asymmetric choice net generates gas is further preferably mixed under stress after raw material heating fusing simultaneously, and these measures significantly reduce the oil content of product, can meet the technical requirements of explosive insensitiveness wax product.
The reason for separating is difficult to for wax in sweating effort and oil, forces oil to be separated with wax by the method that wax layer carries out fluid oil using air-flow by sweating effort, enhanced separating effect and accelerate separating rate；Increasing the high temperature constant temperature stage in temperature-fall period can make the crystallization of pertroleum wax bigger, be conducive to the discharge of oil in sweating effort.Research for pertroleum wax crystallization process shows, the chemical composition of pertroleum wax is the main factor for determining crystal habit, the condition of cooling procedure can also influence crystal habit simultaneously, and especially influence of the cooling condition at the temperature near fusing point to crystal habit is most obvious.Pertroleum wax is when being cooled near fusing point, the n-alkane of larger molecular weight has formed crystallization and has separated out, this partially crystallizable body can be as the nucleus for being subsequently formed crystallization, now increase the high temperature constant temperature stage, nucleus can be enable fully to increase, larger sized crystal is formed, although this larger sized crystal is thick not as the crystallization of low melt point paraffin, the crystal structure of this increase is also highly beneficial to sweating stage discharge oil.The inorganic salt powder that decomposable asymmetric choice net generates gas is mixed under stress after the fusing of preferred feedstock heating simultaneously, and these materials are slowly settled because granularity is smaller in the wax layer of liquid.Keep that raw material is cooled to 10 DEG C~15 DEG C below fusing point under pressure condition, and constant temperature 0.1h~3.0h is so that wax layer crystallization is more abundant；Pressure to normal pressure is gradually reduced in thermostatic process simultaneously.Wax layer is in softer solid state in the time that raw material terminates after being cooled to below fusing point to sweating effort, inorganic salts slowly decompose the gas for discharging during this, micro-bubble can be formed in wax layer, the space that these micro-bubbles are formed is easy to form some tiny passages in wax layer in sweating effort, so as to be conducive to the discharge of oil in sweating effort.The cryogenic thermostat stage for being aided with crystallization process again makes solid crystal more abundant, and the constant temperature stage of sweating effort makes wax that the method such as more abundant is separated with oil, sweating de-oiling technique is produced explosive insensitiveness wax product.
It is 0.5%~2.0% for 64 DEG C~74 DEG C, oil content by selecting fusing point, preferably fusing point is 68 DEG C~72 DEG C, the commodity oil wax that oil content is 0.5%~1.0% is allocated with sweating product, can reduce production cost.
This have the advantage that：By forcing the separation of wax and oil by the method that wax layer carries out fluid oil using air-flow in sweating effort, enhance separating effect and accelerate separating rate；The gas for producing is decomposed using inorganic salts simultaneously short space is formed in wax layer, be also beneficial to the quick discharge of oil；And increase the process such as the high temperature constant temperature stage and cryogenic thermostat stage of crystallization process and the constant temperature stage of sweating effort, so that sweating process can produce explosive insensitiveness wax product.The method of the present invention has the advantages that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution environment.
Specific embodiment
Sweating ware top connects dismountable sealing device and is connected with pressurized buffer tank and compressor, and/or connects pressure-reducing cushioning tank and vavuum pump in sweating ware bottom；Raw material heating fusing simultaneously preferably mixes loading sweating ware after inorganic salt powder under stress；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature be down near raw material melting temperature and high temperature constant temperature for a period of time；Continue to be cooled to preset temperature and cryogenic thermostat for a period of time；Wax layer intensification reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；In sweating effort, start compressor with wax layer malleation formed above, and/or start vavuum pump in wax layer negative pressure formed below, to be used to force air flow through wax layer；On wax through it is refined,（Allocated with paraffin grade wax,）Explosive insensitiveness wax product is after shaping, packaging.
The method for illustrating present invention production explosive insensitiveness wax by the following examples.
Embodiment
1
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）The sweating of intensification-constant temperature,（4）Product purification,（5）The processes such as product preparing.
（1）Preparation
Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；With water as medium；Start the heating function of the circulatory system, recirculated water is warming up to 70 DEG C.
Sweating ware ware plate lower section pad water.The sealing system on sweating ware top is installed and is connected with pressurized buffer tank and compressor；Pressure-reducing cushioning tank is installed in sweating ware bottom and vavuum pump is connected；Start compressor and keep pressurized buffer pressure inside the tank stabilization in 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%）Be raw material, be heated to 70 DEG C fusing after in 3.2~3.4 atmospheric pressure（Gauge pressure）Lower addition sweating ware.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, wax layer temperature drop is made to 67.0 DEG C with the rate of temperature fall of 2.0 DEG C/h and constant temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Wax layer temperature drop is made to 56.0 DEG C with the rate of temperature fall of 1.5 DEG C/h again and constant temperature carries out cryogenic thermostat in 2.0 hours, so that crystallization is more abundant.The constant temperature stage controls pressurized buffer pressure inside the tank to be gradually decrease to normal pressure with the speed of 5.0 atmospheric pressure/h by emptying system.Close the refrigerating function of the circulatory system.
（3）The sweating of intensification-constant temperature
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅰ）To receive under wax；Start compressor and keep pressurized buffer pressure inside the tank stabilization in 1.1~1.3 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system function, wax layer temperature is increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h；Stop compressor.
Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stabilization in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue to make wax layer temperature be increased to 68.0 DEG C and constant temperature 4.0 hours so that the wax in wax layer is sufficiently separated with oil with the heating rate of 2.0 DEG C/h.
Stop vavuum pump, terminate sweating degreasing process.The outlet of sweating ware is changed to connect crude product storage tank（Ⅰ）To receive on wax.Continue to raise circulating water temperature to 85 DEG C, taken out on wax with melting, as crude product（Ⅰ）.
（4）Product purification
Crude product（Ⅰ）Explosive insensitiveness wax product is after washing, clay-filtered, shaping, packaging（Ⅰ）.
Explosive insensitiveness wax product（Ⅰ）Property：72.58 DEG C of fusing point；Oil content 0.39%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.Explosive insensitiveness wax product（Ⅰ）Yield be 17.6%（Relative to raw material 66#Semi-refined wax）.
（5）Product preparing
Explosive insensitiveness wax product（Ⅰ）With No. 70 semi-refined waxs（Dalian Petrochemical Industry Company, 70.35 DEG C of fusing point；Oil content 0.81%）By weight it is 80%：20% ratio is weighed, and is heated to 90 DEG C and is melted and be well mixed, be molded, pack after be explosive insensitiveness wax product（Ⅱ）.
Explosive insensitiveness wax product（Ⅱ）Property：72.10 DEG C of fusing point；Oil content 0.48%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.
Embodiment
2
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）The sweating of intensification-constant temperature,（4）Product purification,（5）The processes such as product preparing.
（1）Preparation
Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；With water as medium；Start the heating function of the circulatory system, recirculated water is warming up to 70 DEG C.
Sweating ware ware plate lower section pad water.The sealing system on sweating ware top is installed and is connected with pressurized buffer tank and compressor；Pressure-reducing cushioning tank is installed in sweating ware bottom and vavuum pump is connected；Pressurized buffer tank emptying system and sweating ware lower exhaust port are connected with gas absorption system respectively, using 5% NaOH solution as absorbing medium.
Start compressor and keep pressurized buffer pressure inside the tank stabilization in 3.2~3.4 atmospheric pressure（Gauge pressure）.Grind and screen out the sodium acid carbonate of 100 mesh~200 mesh.
With 66#Semi-refined wax（With embodiment 1）Be raw material, be heated to 70 DEG C fusing after in 3.2~3.4 atmospheric pressure（Gauge pressure）The foregoing sodium bicarbonate powder of lower incorporation 1.0%, sweating ware is added after being well mixed；Pressurized buffer pressure inside the tank stabilization is kept in 3.2~3.4 atmospheric pressure.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, wax layer temperature drop is made to 67.0 DEG C with the rate of temperature fall of 2.0 DEG C/h and constant temperature carries out high temperature constant temperature in 2.0 hours, so that crystallization fully increases；Wax layer temperature drop is made to 56.0 DEG C with the rate of temperature fall of 1.5 DEG C/h again and constant temperature carries out cryogenic thermostat in 2.0 hours, so that crystallization is more abundant.The cryogenic thermostat stage controls pressurized buffer pressure inside the tank by emptying system, and normal pressure is gradually decrease to the speed of 5.0 atmospheric pressure/h.The gas of cryogenic thermostat stage discharge decomposes the carbon dioxide for generating by 5% NaOH solution to absorb sodium acid carbonate.Close the refrigerating function of the circulatory system.
（3）The sweating of intensification-constant temperature
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；Start compressor and keep pressurized buffer pressure inside the tank stabilization in 1.1~1.3 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system function, wax layer temperature is increased to 62.0 DEG C with the heating rate of 2.0 DEG C/h；Stop compressor.
Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stabilization in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue to make wax layer temperature be increased to 68.0 DEG C and constant temperature 4.0 hours so that the wax in wax layer is sufficiently separated with oil with the heating rate of 2.0 DEG C/h.The gas discharged in sweating effort decomposes the carbon dioxide for generating by 5% NaOH solution to absorb sodium acid carbonate.
Stop vavuum pump, terminate sweating effort.The outlet of sweating ware is changed to connect crude product storage tank（Ⅱ）To receive on wax.Continue to raise circulating water temperature to 85 DEG C, taken out on wax with melting, as crude product（Ⅱ）.
（4）Product purification
Crude product（Ⅱ）Through washing, clay-filtered as explosive 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 the associated specifications of explosive insensitiveness wax product.Explosive insensitiveness wax product（Ⅲ）Yield be 22.9%（Relative to raw material 66#Semi-refined wax）.
（5）Product preparing
Explosive insensitiveness wax product（Ⅲ）With No. 70 semi-refined waxs（With embodiment 1）By weight it is 60%：40% ratio is weighed, and is heated to 90 DEG C and is melted and be well mixed, be molded, pack after be explosive insensitiveness wax product（Ⅳ）.
Explosive insensitiveness wax product（Ⅳ）Property：71.62 DEG C of fusing point；Oil content 0.47%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.
The production method of explosive insensitiveness wax of the present invention is can be seen that by embodiment 1-2, by increasing the improvement to sweatbox such as pressurization and/or vacuum facility；Decomposed using inorganic salts and short space is formed in wax layer and the improvement to sweating process such as wax layer is forced air flow through in intensification sweating effort；Enhance the separating effect of wax and oil and accelerate separating rate so that sweating de-oiling technique can produce fusing point between 70 DEG C~80 DEG C, oil content less than 0.5%, the explosive insensitiveness wax product of mechanical impurity.Production cost can be reduced by the allotment with general goods paraffin.
Claims (23)
1. a kind of method for producing explosive insensitiveness wax, including herein below：
（1）Charging：With paraffin that fusing point is 60 DEG C~74 DEG C as raw material, the inorganic salt powder that decomposable asymmetric choice net generates gas is mixed after heating fusing under stress, load sweatbox；
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization：Wax layer is cooled to by proper temperature with the speed of 1.0 DEG C/h~3.0 DEG C/h, high temperature constant temperature is for a period of time；Cooled to raw material fusing point 5 DEG C~20 DEG C of cooling final temperature with the speed of 0.5 DEG C/h~2.5 DEG C/h again, and cryogenic thermostat is for a period of time；
（3）The sweating of intensification-constant temperature：Heated up with the speed of 0.5 DEG C/h~2.5 DEG C/h, wax layer reaches predetermined temperature and constant temperature stops sweating afterwards for a period of time；Wax layer is forced air flow through in sweating effort；
（4）It is refined：On wax after refined, as explosive is with insensitiveness wax product or as explosive insensitiveness wax product blend component.
2. in accordance with the method for claim 1, it is characterised in that described inorganic salt powder is decomposed in sweating effort and discharges gas, and itself and catabolite are soluble in water.
3. in accordance with the method for claim 1, it is characterised in that described inorganic salts are selected from one or more in ammonium salt, carbonate, bicarbonate.
4. in accordance with the method for claim 1, it is characterised in that the granularity of described inorganic salt powder is 50~500 mesh.
5. in accordance with the method for claim 2, it is characterised in that the addition of described inorganic salt powder accounts for the 0.1%~10.0% of raw material weight.
6. in accordance with the method for claim 1, it is characterised in that described pressure is 0.5~15.0 atmospheric pressure of gauge.
7. in accordance with the method for claim 1, it is characterised in that in step（1）Charging process and step（2）Apply air pressure above wax layer during the temperature-fall period and high temperature constant temperature of crystallization, the gas produced to suppress inorganic salts to decompose escapes wax layer, described air pressure is 0.5~15.0 atmospheric pressure of gauge.
8. in accordance with the method for claim 1, it is characterised in that step（3）Described in the wax layer that forces air flow through use to increase above wax layer and air pressure and/or air pressure reduced below wax layer, wax layer upper and lower is formed pressure differential and realize, described pressure differential is 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure.
9. in accordance with the method for claim 1, it is characterised in that step（2）Rate of temperature fall of the middle temperature-fall period before high-temperature constant temperature section 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. in accordance with the method for claim 1, it is characterised in that step（2）Described in the proper temperature of high-temperature constant temperature section lowered the temperature be -1.0 DEG C of starting paraffin fusing point~+2.0 DEG C of fusing point, time of high-temperature constant temperature section is 0.1~4.0 hour.
11. in accordance with the method for claim 1, it is characterised in that step（2）Described in cooling final temperature for 8 DEG C~15 DEG C below starting paraffin fusing point.
12. in accordance with the method for claim 1, it is characterised in that step（2）Described in temperature-fall period the cryogenic thermostat stage time be 0.1~3.0 hour.
13. in accordance with the method for claim 1, it is characterised in that step（2）In gradually reduce pressure to normal pressure while cryogenic thermostat, rate of pressure reduction is 0.1~150 atm/h.
14. in accordance with the method for claim 1, it is characterised in that step（3）Described in sweating effort heating rate be 1.0 DEG C/h~2.0 DEG C/h.
15. in accordance with the method for claim 1, it is characterised in that step（3）Described in the predetermined temperature that heats up of sweating effort be less than 1 DEG C~10 DEG C of purpose product fusing point.
16. in accordance with the method for claim 1, it is characterised in that step（3）Described in constant temperature time be 0.1~5.0 hour.
17. in accordance with the method for claim 1, it is characterised in that step（3）Described in force air flow through wax layer the sweating initial stage implement.
18. in accordance with the method for claim 8, it is characterised in that step（3）Described in force air flow through wax layer use above wax layer increase air pressure realize, above wax layer apply 0.2~2.0 gauge of atmospheric pressure, and wax layer lower section remain normal pressure.
19. in accordance with the method for claim 8, it is characterised in that step（3）Described in force air flow through wax layer use below wax layer reduce air pressure realize, above wax layer air pressure keep normal pressure, and below wax layer maintain -0.2~-1.0 gauges of atmospheric pressure.
20. in accordance with the method for claim 1, it is characterized in that, the pernicious gas that inorganic salts decompose generation is absorbed using liquid absorption mode in the cryogenic thermostat process and sweating effort of crystallization, unreacted inorganic salts and catabolite are removed using water-washing method in subtractive process.
21. in accordance with the method for claim 1, it is characterised in that step（4）It is used as explosive insensitiveness wax product blend component on middle wax after refined.
22. in accordance with the method for claim 21, it is characterised in that also including step（5）：Resulting blend component is allocated with paraffin grade wax, and explosive insensitiveness wax product is obtained after shaping, packaging；The fusing point of the allotment paraffin grade wax is 64 DEG C~74 DEG C, oil content is 0.5wt%~2.0wt%；Blend component is 10%~99.9% with the allotment weight ratio of paraffin grade wax：0.1~90%.
23. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
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| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin 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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