CN106883878A - 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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- CN106883878A CN106883878A CN201510928616.XA CN201510928616A CN106883878A CN 106883878 A CN106883878 A CN 106883878A CN 201510928616 A CN201510928616 A CN 201510928616A CN 106883878 A CN106883878 A CN 106883878A
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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
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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
Abstract
The invention discloses a kind of sweating and the method for producing explosive insensitiveness wax.The method is on the basis of common sweating de-oiling technique, the oil of liquid is carried out to force to separate 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 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 sweating and production the explosive method of 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.Widely using for explosive serves important facilitation to the material progress of human society.
Main explosive used is TNT during World War II, and conventional explosive is RDX at present（RDX, the ammonium nitrate of ring cyclonite three）And HMX（HMX, HMX）.With the development of science and technology, various explosives develop in terms of high-power, high security.
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.General goods oil content in paraffin wax 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, a small amount of isoparaffin and cycloalkane, usual fusing point is 50 DEG C~74 DEG C.
Dewaxing is the process with lube cut as the slack wax that raw material production oil content is 10~30% or so, and dewaxing technique mainly has squeezing to dewax and solvent dewaxing.De-oiling is the process of the base oil wax as raw material production oil content below 2% 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 petroleum paraffin product 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, and the fusing point of the less n-alkane of molecular weight is relatively low；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane will 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；Charging, loads 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；Sweating effort terminates follow-up high-temperature of continuing rising, is taken out on wax with melting, as crude product；（4）It is refined：Predetermined temperature is warming up to after crude product fusing, carclazyte is added and constant temperature is stirred to the scheduled time filtering, then be 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 paraffin 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 the technical requirement of explosive insensitiveness wax.
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 de-oiling 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 explosive insensitiveness wax product of the fusing point at 70 DEG C~80 DEG C.
Sweating de-oiling technique is to be currently known the unique solvent-free de-oiling method for commercial scale petroleum paraffin product, is being advocated today of green low-carbon, environmental protection and energy saving, more urgent with the demand of insensitiveness wax product using sweating de-oiling technique productions explosive.
The content of the invention
In view of the shortcomings of the prior art, a kind of method that the present invention provides sweating and production explosive insensitiveness wax, specifically use sweatbox, on the basis of common sweating de-oiling technique, the oil of liquid is carried out to force to separate wax and oil by wax layer using air-flow in sweating effort, pressure is applied to accelerate the separating rate of wax and oil and ensure airflow through wax layer to wax layer by way of placing solid mass in wax layer in sweating effort, this solvent-free de-oiling method of sweating de-oiling 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 general goods paraffin allotment.
A kind of sweating of the invention and the 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, 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 grade wax（In mass）Generally less than 2.0%；Fusing point is generally 60 DEG C~74 DEG C, preferably 64 DEG C~70 DEG C.
In the method for the present invention, in step（3）In sweating effort, solid mass preferably is placed to apply the pressure of more than 0.5kPa to wax layer by wax layer surface.Solid mass surfacing, overall dimensions are slightly less than sweatbox inner wall size（Such as, solid mass edge is generally 0.01~50mm, preferably 0.1~20mm with the gap of sweatbox inwall）, inside have the space run through up and down.The density of solid mass typically requires to be more than 4 g/cm3, can be the materials such as nonmetallic, metal and alloy, preferred density is 6~12 g/cm3Metal and alloy, such as zinc, iron, copper, lead and its more stable low price metal material of alloy chemical property.
In the present invention, place solid mass on wax layer surface one of in the following ways and apply pressure with to wax layer：（1）It is disposable in sweating effort to add the solid mass that produce more than 0.5kPa pressure, it is disposable preferably when sweating starts to add the solid mass that produce 1.4~20.0kPa pressure；（2）In sweating effort several times（It is preferred that 2~3 times）Add, i.e., being added in every 0.1~20.0 h can produce the solid mass of more than 0.5kPa pressure, being added preferably in every 0.1~10.0 h can produce the solid mass of 1.4~10.0kPa pressure.
In the method for the present invention, described sweatbox is sweating ware, and 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 difference and realize.Described pressure difference is generally 10~500 kPa, preferably 20~200 kPa, 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 source commodity paraffin melting point.Described cools to final temperature, increases the cryogenic thermostat stage so that solid crystal is more abundant, and the time in cryogenic thermostat stage is 0~3.0 hour, more preferably preferably 0.1~3.0 hour, 1.0~3.0 hours.
In the method for the present invention, the step（3）Sweating effort heating rate 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 the i.e. explosive insensitiveness wax of purpose product.
In the method for the present invention, the step（3）Sweating be warming up to the predetermined temperature for producing product after, increasing the constant temperature stage can be such that wax is separated with oil more fully, and 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, and the circulatory system has programmed cooling/heating function, and the circulatory system adds the materials such as water or conduction oil as circulatory mediator；Coil pipe is submerged and is fixed in wax layer after charging, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the method for the present invention, the step（3）Force air flow through wax layer and can implement in sweating effort any stage, preferably implement at the sweating initial stage.
In the method for the present invention, the step（3）Force air flow through wax layer be utilized in wax layer top increase air pressure realize, 20~150 kPa can be such as applied above wax layer（Gauge pressure）Air 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 be utilized in wax layer lower section and reduce what air pressure was realized, air pressure that such as can be above wax layer keeps normal pressure, and -20~-80 kPa are maintained below wax layer（Gauge pressure）Air pressure.
In the method for the present invention, step（4）Products therefrom can serve as explosive insensitiveness wax blend component, can be with the allotment of general goods paraffin with reduces cost.Therefore, the method for the present invention 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 be generally 64 DEG C~74 DEG C, oil content be 0.5%~2.0%；Blend component is 10%~99.9% with the allotment ratio of paraffin grade wax：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 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 paraffin of sweating de-oiling is applied to production fusing point in 70 DEG C~80 DEG C, explosive insensitiveness wax product of the oil content less than 0.5%, 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, while increasing the processes such as constant temperature stage of high temperature constant temperature stage and cryogenic thermostat stage and sweating effort further preferably in crystallization process；And pressure is applied to wax layer by way of placing solid mass on wax layer surface in sweating effort, 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 during cooling can make the crystallization of pertroleum wax bigger, be conducive to the discharge of oil in intensification 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.During common sweating process, with the gradually discharge of oil, wax layer can produce the contraction of vertical direction and the contraction of horizontal direction, when pressure difference is formed to force air flow through wax layer up and down in wax layer, it some times happens that air-flow flows through and without the phenomenon of wax layer through gap between wax layer and ware plate.In the inventive method, apply the means of pressure to wax layer by way of placing solid mass on wax layer surface, the oil coated in extrudable wax crystallization is so as to accelerate wax and oily separating rate, prior can be to make wax layer only produce the contraction of vertical direction without the contraction of generation horizontal direction, increase the resistance between wax layer and baffle plate and ware plate；Simultaneously because there is the space run through up and down inside solid mass, it can be ensured that air-flow is fuel-displaced to carry by wax layer.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 68 DEG C~72 DEG C of fusing point, the paraffin grade wax that oil content is 0.5%~1.0% and sweating product allotment can then reduce production cost.
It is an advantage of the invention 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；Accelerate the separating rate of wax and oil and ensure airflow through wax layer by placing solid mass in wax layer in sweating effort simultaneously, so that sweating de-oiling technique 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；Load sweating ware after paraffin raw material heating fusing；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature be down near raw material melting temperature and constant temperature for a period of time；Continue to be cooled to preset temperature and constant temperature 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；Preferably gradually increase solid pressure 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 it is refined,（Allocated with paraffin grade wax,）Explosive insensitiveness wax product is after shaping, packaging.
The method that sweating of the present invention and production explosive insensitiveness wax are illustrated below by way of specific embodiment.
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
By sweating ware（Inwall is the square of 1m × 1m）Sealing system connected with pressurized buffer tank and compressor；Pressure-reducing cushioning tank is installed in sweating ware bottom and vavuum pump is connected；Sweating ware chuck and removable coil pipe are connected with the circulatory system, 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.
With 66#Semi-refined wax（Jinan petro-chemical corporation, 66.35 DEG C of fusing point, oil content 0.76%）It is raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and fixed.
（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.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；Connection sweating ware sealing device for upper portion of annular；Start compressor and keep pressurized buffer tank internal pressure strong stability in 110~130kPa（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 1.5 DEG C/h.
Stop compressor.Remove sealing device.Open vavuum pump and keep surge tank internal pressure strong stability in -40~-60 kPa（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 1.5 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 clay-filtered, shaping, packaging（Ⅰ）.
Explosive insensitiveness wax product（Ⅰ）Property：72.75 DEG C of fusing point；Oil content 0.35%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.Explosive insensitiveness wax product（Ⅰ）Yield be 19.8%（Relative to raw material 66#Semi-refined wax）.
（5）Product preparing
Explosive insensitiveness wax（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：72.68 DEG C of fusing point；Oil content 0.45%；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
Prepare stainless steel plate some, every piece of stainless steel plate overall dimensions are 0.98
M × 0.98m × 0.02 m, and the through hole of the m of equally distributed φ 0.0015 is bored on stainless steel（Drilling, hole center spacing 0.04m are played at edge 0.01m）（The pressure about 1.5kPa that every piece of stainless steel plate is produced）, it is standby.
By sweating ware（With embodiment 1）Sealing system connected with pressurized buffer tank and compressor；Pressure-reducing cushioning tank is installed in sweating ware bottom and vavuum pump is connected；Sweating ware chuck and removable coil pipe are connected with the circulatory system, 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.
With 66#Semi-refined wax（With embodiment 1）It is raw material, sweating ware is added after heating fusing.Coil pipe is immersed in raw material wax layer and fixed.
（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.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.First piece of foregoing stainless steel plate of horizontal positioned on wax layer surface.Connection sweating ware sealing device for upper portion of annular.Start compressor and keep pressurized buffer tank internal pressure strong stability in 110~130kPa（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 1.5 DEG C/h.
Stop compressor.Remove sealing device.Second piece of foregoing stainless steel plate is placed on wax layer surface.Start vavuum pump and keep surge tank internal pressure strong stability in -40~-60 kPa（Gauge pressure）, wax layer top air pressure holding normal pressure.Continuation makes wax layer temperature be increased to 68.0 DEG C with the heating rate of 1.5 DEG C/h.The 3rd piece of foregoing stainless steel plate is placed on wax layer surface, continues constant temperature 4.0 hours so that the wax in wax layer is sufficiently separated with oil.Stop vavuum pump, terminate sweating degreasing process.
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）Explosive insensitiveness wax product is after clay-filtered, shaping, packaging（Ⅲ）.
Explosive insensitiveness wax product（Ⅲ）Property：72.68 DEG C of fusing point；Oil content 0.21%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.Explosive insensitiveness wax product（Ⅲ）Yield be 25.2%（Relative to raw material 66#Semi-refined wax）.
（5）Product preparing
Explosive insensitiveness wax（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：71.86 DEG C of fusing point；Oil content 0.46%；Mechanical admixture, nothing.Meet the associated specifications of explosive insensitiveness wax product.
The production method of sweating of the present invention and explosive insensitiveness wax is can be seen that by embodiment 1-2, by increasing the improvement to sweatbox such as pressurization and/or vacuum facility；By placing solid mass in wax layer, and the improvement to sweating process such as wax layer, the constant temperature stage for increasing cooling and temperature-rise period 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 (24)
1. a kind of sweating and the production explosive method of insensitiveness wax, 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 the proper temperature of -1.0 DEG C of starting paraffin fusing point~+2.0 DEG C of fusing point 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, and the predetermined temperature is 1 DEG C~10 DEG C of the fusing point less than explosive insensitiveness wax；Wax layer is forced air flow through in sweating effort, and places solid mass to apply wax layer the pressure of more than 0.5kPa on wax layer surface；
（4）It is refined：Explosive is with insensitiveness wax product or as explosive insensitiveness wax product blend component after refined on wax.
2. in accordance with the method for claim 1, it is characterised in that described solid mass surfacing, overall dimensions are slightly less than sweatbox inner wall size, there is the hole for running through up and down inside.
3. in accordance with the method for claim 1, it is characterised in that the density of described solid mass is more than 4g/cm3。
4. in accordance with the method for claim 3, it is characterised in that the density of described solid mass is 6~12g/cm3。
5. in accordance with the method for claim 1, it is characterised in that described places solid mass in the following ways on wax layer surface：It is disposable in sweating effort to add the solid mass that produce more than 0.5kPa pressure.
6. in accordance with the method for claim 5, it is characterised in that disposable when sweating starts to add the solid mass that produce 1.4~20.0kPa pressure.
7. in accordance with the method for claim 1, it is characterised in that described places solid mass in the following ways on wax layer surface：Added several times in sweating effort, i.e., being added in every 0.1~20.0 h can produce the solid mass of more than 0.5kPa pressure.
8. in accordance with the method for claim 7, it is characterised in that being added in every 0.1~10.0 h can produce the solid mass of 1.4~10.0 kPa pressure.
9. 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 difference and realize, described pressure difference is 10~500 kPa.
10. in accordance with the method for claim 9, it is characterised in that described pressure difference is 20~200 kPa.
11. in accordance with the method for claim 1, it is characterised in that described melting point of paraffin wax is 64 DEG C~70 DEG C, and oil content is less than 2.0%.
12. 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.
13. in accordance with the method for claim 1, it is characterised in that step（2）Described in proper temperature be starting paraffin fusing point~+1.0 DEG C of fusing point.
14. in accordance with the method for claim 1, it is characterised in that step（2）The time of the high-temperature constant temperature section of middle temperature-fall period is 0.1~4.0 hour, and the time in cryogenic thermostat stage is 0.1~3.0 hour.
15. in accordance with the method for claim 1, it is characterised in that step（2）Described in cooling final temperature for starting paraffin fusing point below 8 DEG C~15 DEG C.
16. 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.
17. 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.
18. in accordance with the method for claim 9, it is characterised in that step（3）Described in force air flow through wax layer be utilized in wax layer top increase air pressure realize：Apply the gauge pressure pressure of 20~150 kPa above wax layer, and wax layer lower section remains normal pressure.
19. in accordance with the method for claim 9, it is characterised in that step（3）Described in force air flow through wax layer be utilized in wax layer lower section reduce air pressure realize：Air pressure keeps normal pressure above wax layer, and the gauge pressure pressure of -20~-80 kPa is maintained below wax layer.
20. in accordance with the method for claim 1, it is characterised in that step（3）Described in force air flow through wax layer the intensification sweating initial stage implement.
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 0.5%~2.0%；Blend component is 10%~99.9% with the allotment ratio of paraffin grade wax：0.1%~90%.
23. in accordance with the method for claim 22, it is characterised in that the fusing point of described allotment paraffin grade wax is 68 DEG C~72 DEG C, oil content is 0.5%~1.0%.
24. in accordance with the method for claim 1, it is characterised in that described 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574785A (en) * | 2020-10-23 | 2021-03-30 | 国家能源集团宁夏煤业有限责任公司 | Deoiling method and application of Fischer-Tropsch synthetic wax |
Citations (3)
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|---|---|---|---|---|
| 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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- 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574785A (en) * | 2020-10-23 | 2021-03-30 | 国家能源集团宁夏煤业有限责任公司 | Deoiling method and application of Fischer-Tropsch synthetic wax |
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