CN107513426A - The method for preparing PUR microwax - Google Patents
The method for preparing PUR microwax Download PDFInfo
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- CN107513426A CN107513426A CN201610432973.1A CN201610432973A CN107513426A CN 107513426 A CN107513426 A CN 107513426A CN 201610432973 A CN201610432973 A CN 201610432973A CN 107513426 A CN107513426 A CN 107513426A
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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
- C10G73/40—Physical treatment of waxes or modified waxes, e.g. granulation, dispersion, emulsion, irradiation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C10G73/42—Refining of petroleum waxes
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Abstract
The invention discloses a kind of method for preparing PUR microwax.This 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, micro-bubble is formed in wax layer using gas caused by the decomposable asymmetric choice net material dissolved in the feed simultaneously, the quick discharge of oil is also beneficial to, so that sweating de-oiling method can produce the PUR crystallite wax product of low oil content.The inventive method has the advantages that equipment investment 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 the method for preparing PUR microwax.
Background technology
PUR is a kind of adhesive of plasticity, and its physical state changes and changed with temperature in certain temperature range, and chemical characteristic is constant, and its is nonpoisonous and tasteless, belongs to environmentally friendly chemicals；The advantages that product is solid, is easy to pack, transports, stores, while has simple production process, and applying glue is convenient, bonding strength is big, speed is fast, thus be used widely in many fields.With ethene-vinyl acetate random copolymer（EVA）Based on the EVA hot-melt adhesive of resin be the most important kind of PUR.
EVA hot-melt adhesive is made up of compositions such as basic resin, tackifying resin, viscosity modifier and antioxidant.Basic resin is EVA resin, and its ratio, quality determine the basic performance of PUR（Such as the cementitiousness of glue, melting temperature and adhesion strength）.Tackifying resin can improve the mobility of colloid and the wetability to adherend, improve adhesive property, reach required adhesion strength.Tackifying resin mainly has rosin, modified rosin, C5 Petropols, C9 Petropols, terpene resin etc..The effect of viscosity modifier is to increase mobility, the regulation setting rate of colloid molten state, to reach the purpose being quickly firmly bonded.Viscosity modifier is typically chosen paraffin, microwax, synthetic wax etc..Antioxidant is to prevent the premature aging of EVA hot-melt adhesive, it is ensured that adhesive property does not change under the high temperature conditions.In addition, can also mix cold-resistance agent that some are adapted to frigid zone temperature or the antiheat agent for being adapted to tropical temperature according to the difference of temperature, area, a small amount of filler can be also added to increase interstitial and reduce cost.
The viscosity and mobility and sizability of PUR are closely related.Maximum to PUR applying glue viscosity influence is viscosity modifier, i.e. wax.Because wax is the composition that viscosity is minimum in PUR, the viscosity of PUR can be significantly reduced, increase its mobility by increasing the dosage of wax.The PUR of some specific uses, such as aluminum foil seal gasket PUR, it is desirable to be not more than 1.0% using 80~88 DEG C of melt drop temperature, oil content（Mass content）, kinematic viscosity（100℃）Not less than 10 mm2/ s microwax is as viscosity modifier.
Microwax is one kind of pertroleum wax, is that decompression residuum produces 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, have than other pertroleum waxes under solid-state, such as soap manufacturing paraffin and paraffin, more tiny needle-like crystal structure.The melt drop temperature of the crystallite wax product of specification is 67 DEG C~92 DEG C in national standard, and oil content is less than 5.0%.The oil content of the microwax of domestic production at present is generally between 1.5%~3.5%, it is impossible to meets the requirement of aluminum foil seal gasket PUR.
In pertroleum wax production process, dewaxing is that the process for the slack wax that oil content is 10~30% or so is prepared by raw material of crude oil fractions.De-oiling is that the process of base oil wax of the oil content below 5% is prepared using slack wax as raw material, 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 obtains 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 separated.Solvent deoiling technique have the advantages that production process is continuous, wax high income, finished product wax oil content can it is very low, production cost is relatively low, be the main flow de-oiling technique of current large-scale production petroleum paraffin product.But solvent deoiling technique productions equipment investment is big；Need largely to use solvent in production process, 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 just be at normal temperatures liquid condition, i.e., usually said oil.
Common sweating de-oiling technique mainly includes the following steps that：（1）Preparation：Pad water（Sweatbox ware plate underlying 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 below its fusing point 10~20 DEG C with the rate of temperature fall no more than 4 DEG C/h.In cooling procedure, various components are crystallized to form solid successively by the order of fusing point from high to low；（3）Sweating：After wax layer temperature reaches default cooling final temperature, pad water is bled off；Raw material is slowly heated to default sweating final temperature again.In sweating effort, various components are successively fused into liquid by the order of fusing point from low to high and flowed out（Under wax）, the wax layer residue that finally obtains（On wax）It is exactly high-melting-point, the wax of low oil-containing；（4）It is refined：Collect crude product（Sweating effort terminates follow-up high-temperature of continuing rising, is taken out with fusing on wax, as crude product）, through clay-filtered（Predetermined temperature is warming up to after crude product is melted, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the scheduled time）Afterwards, reshaping, packaging are purpose product.
Common sweating de-oiling technique can produce the soap manufacturing paraffin and low melt point paraffin under solid-state with thick flaky crystal structure, can not but produce the microwax under solid-state with tiny needle-like crystal structure.There is experiment to show, during common sweating de-oiling technique productions microwax, even if using the method for extending sweating sessions and improving 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 so far there are no with the report of sweating de-oiling technique productions crystallite wax product.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is relatively low, the production cycle is longer, but sweating de-oiling technique have the advantages that small investment, production process are simple, operating cost is low, production process is safe, energy-conservation and it is environmentally safe, still have at present part producer using this method production soap manufacturing paraffin product.
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 production equipment；CN91206202（A kind of high-efficient sweat pot for paraffin wax）Improved on sweating process, but these methods are there are still the shortcomings of product yield is relatively low, the production cycle is longer, and can not still produce microwax.
Sweating de-oiling technique is to be currently known unique solvent-free separation method for commercial scale petroleum paraffin product, and in promotion green low-carbon, today of environmental protection and energy saving, the demand that PUR microwax is prepared using sweating de-oiling technique is more urgent.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of method for preparing PUR microwax, specifically using sweatbox, on the basis of common sweating de-oiling technique, the material that oil-soluble decomposable asymmetric choice net produces gas is added after raw material heating fusing；And the oily to force to separate wax and oil of liquid is carried out by wax layer using air-flow in sweating effort, enhance separating effect and accelerate separating rate, this solvent-free de-oiling method of sweating is produced PUR crystallite wax product.The inventive method has the advantages that equipment investment is low, production process is simple and operating cost is low, energy-saving safe and solvent-free pollution.
The method for preparing PUR microwax of the present invention, including herein below：
（1）Charging：Using the commodity microwax that melt drop temperature is 75 DEG C~85 DEG C as raw material, load sweatbox after heating fusing；
（2）Crystallization：Wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h speed, high temperature constant temperature is for a period of time；5 DEG C~20 DEG C below raw material melt drop temperature of cooling final temperature is cooled to 0.5 DEG C/h~2.5 DEG C/h speed again, and cryogenic thermostat is for a period of time；
（3）Sweating：Heated up with 0.5 DEG C/h~2.5 DEG C/h speed；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：After refined it is PUR crystallite wax product on wax.
In the method for the present invention, the melt drop temperature of the source commodity microwax is 75 DEG C~85 DEG C, and oil content is 1.0%~5.0%（Mass content）.
In the method for the present invention, after raw material heating fusing, the oil soluble material that decomposable asymmetric choice net produces gas is preferably added to.Concrete operations are first to heat sweating raw material and melt, then load sweatbox after the material of oil-soluble decomposable asymmetric choice net generation gas is dissolved in into raw material.Described oil-soluble decomposable asymmetric choice net material includes organic azo compound, sulfonyl hydrazines compound, organic nitroso compounds, organic peroxide etc., the preferably one or more in organic azo compound and organic peroxide.The addition of oil-soluble decomposable asymmetric choice net material is the 0.01%~15.00% of raw material weight, preferably 0.03%~8.00%.
Wherein, described organic azo compound is selected from ABVN（ABVN）, azodiisobutyronitrile（AIBN）, azo diisopropyl imidazoline hydrochloride（ACCN）The one group of material formed；Described sulfonyl hydrazines compound is selected from benzene sulfonyl hydrazide, unifor, 4,4 '-bis oxide（Benzene sulfonyl hydrazide）The one group of material formed；Described organic nitroso compounds are selected from dinitrosopentamethylene tetramine and/or N, N '-dimethyl N, N '-dinitroso phthalic amide；The organic peroxide is selected from dibenzoyl peroxide（BPO）, dilauroyl peroxide（LPO）, diacetyl peroxide, dicetyl peroxydicarbonate isopropyl ester（IPP）, di-cyclohexylperoxy di-carbonate（DCPO）Etc. one group of material of composition.
In the method for the present invention, described sweatbox is sweating ware, and increases in wax layer pressue device added above and/or below wax layer vacuum plant.In step（3）Sweating effort in, it is described force air flow through wax layer and use increase air pressure above wax layer and/or air pressure 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, step（2）In the temperature-fall period of crystallization, 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+2.0 DEG C of -1.0 DEG C~melt drop temperature of raw material microwax melt drop temperature, preferably raw material microwax melt drop temperature~+1.0 DEG C of melt drop temperature.The time of the high-temperature constant temperature section of temperature-fall period is 0~4.0 hour, preferably 0.1~4.0 hour, more preferably 1.0~4.0 hours.
In the method for the present invention, step（2）Rate of temperature fall preferably 1.0 DEG C/h~2.0 DEG C/h of the temperature-fall period after high-temperature constant temperature section.Described cooling final temperature is preferably 8 DEG C~15 DEG C below raw material microwax melt drop temperature.After wax layer is cooled to final temperature, the increase cryogenic thermostat stage, the time in cryogenic thermostat stage was 0~3.0 hour, preferably 0.1~3.0 hour, more preferably 1.0~3.0 hours so that solid crystal is more abundant.
In the method for the present invention, step（3）The speed of the heating preferably 1.0 DEG C/h~2.0 DEG C/h.The final temperature of wherein temperature-rise period is that predetermined temperature is less than 2 DEG C~10 DEG C of purpose product melt drop temperature.After preset temperature is warming up to, the increase constant temperature stage, the time in constant temperature stage was 0~5.0 hour, preferably 0.1~5.0 hour, preferably 1.0~5.0 hours so that wax separates more fully with oil.
In the method for the present invention, the programming rate and cooling rate of said wax layer, it can be controlled by air bath, water-bath, oil bath or other feasible modes, it is preferred to use water-bath or oil bath.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 program cooling/heating function, and the circulatory system adds the material such as water or conduction oil as circulatory mediator.
In the method for the present invention, step（3）Described in force air flow through wax layer and can implement in sweating effort any stage, preferably implement initial stage in sweating.
In the method for the present invention, the described wax layer that forces air flow through is utilized in what increase air pressure above wax layer was realized, can such as apply 0.2~2.0 atmospheric pressure above wax layer（Gauge pressure）Pressure, and wax layer below remain normal pressure.
In the method for the present invention, the described wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized, and normal pressure can be such as kept above wax layer, and -0.2~-0.8 atmospheric pressure is maintained below wax layer（Gauge pressure）Pressure.
Sweating de-oiling method is to be separated using the wax property different with oily fusing point to produce pertroleum wax, and the research for pertroleum wax sweating effort shows, oil is gradually discharged along crystalline portion in sweating effort, situation about being flowed similar to liquid in capillary.For commercially available crystallite wax product, because its main component is isoparaffin and cycloalkane, 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 only being difficult to be kept completely separate by wax in the common sweating effort of gravity natural separation and oil.Therefore common sweating de-oiling technique can not effectively reduce the oil content of crystallite wax product.
The present invention can prepare PUR crystallite wax product in order that obtaining this solvent-free de-oiling method of sweating, pass through the further investigation to common sweating effort, the reason for being difficult to separate with oil for wax, force oil to be separated with wax by using to force air flow through wax layer and carry fuel-displaced method in sweating effort, enhance separating effect and accelerate separating rate；Increasing the high temperature constant temperature stage in crystallization process can make the crystallization of microwax bigger, be advantageous to discharge oily in sweating effort.Research for microwax crystallization process shows, the chemical composition of microwax is to determine the main factor of crystal habit, the condition of cooling procedure can also influence crystal habit simultaneously, and especially influence of the cooling condition at the temperature near melt drop temperature to crystal habit is most obvious.Microwax existing partially crystallizable when being cooled near melt drop temperature separates 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, form larger sized crystal, it is also highly beneficial to sweating stage discharge oil although this larger sized crystal is thick not as the crystallization of soap manufacturing paraffin and low melt point paraffin.Oil-soluble decomposable asymmetric choice net material further preferably is added after raw material heating fusing simultaneously, these material decomposable asymmetric choice nets produce gas, and have preferable dissolubility in the feed and be dispersed in wax layer.Wax layer is in softer solid state in the time that raw material microwax terminates after being cooled to below melt drop temperature to sweating effort, decomposable asymmetric choice net material slowly decomposes the gas discharged during this, dispersed 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 advantageous to discharge oily in sweating effort.It is preferred that the oil-soluble decomposable asymmetric choice net material of the gas of the generation nontoxic no special odor such as nitrogen or carbon dioxide is decomposed, and the other materials molecular weight generated is low, and wax layer will be discharged with oil in sweating effort.Being aided with the cryogenic thermostat stage of crystallization process again makes solid crystal more abundant, and the constant temperature stage of sweating effort makes wax separate the methods of more abundant with oil so that sweating process can prepare PUR crystallite wax product.
This have the advantage that：By in sweating effort use air-flow by wax layer carry fuel-displaced method enhance wax with oil separating effect and accelerate separating rate；Crystalline size is increased using high temperature crystallization, while dispersed micro-bubble is formed in wax layer using gas caused by oil-soluble decomposable asymmetric choice net substance decomposition, is also beneficial to the quick discharge of oil；So that sweating process can prepare PUR crystallite wax product, and have the advantages that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution environment.
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；The heating of raw material microwax is melted and is preferably added to load sweating ware after oil-soluble decomposable asymmetric choice net produces the material of gas；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature be down to raw material melt drop temperature temperature nearby 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；In sweating effort, start compressor with wax layer malleation formed above, and/or start vavuum pump with wax layer negative pressure formed below, to force air flow through wax layer；Wax layer temperature reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；After refined it is PUR crystallite wax product on wax.
1-4 illustrates the method for preparing PUR microwax of the present invention by the following examples.
Embodiment
1
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）Heating-constant temperature sweating,（4）The processes such as product purification.
（1）Preparation
Pad water below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using water as heat-conducting medium, start the heating function of the circulatory system, recirculated water is warming up to 86 DEG C.
With No. 80 microwaxes（Sinopec Jinan branch company, 83.5 DEG C of fusing point, 83.3 DEG C of melt drop temperature, oil content 2.80wt%, kinematic viscosity（100℃）18.94mm2/s）For raw material, sweating ware is added after being heated to 86 DEG C of fusings.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, wax layer temperature is dropped to 84.0 DEG C and 2.0 hours progress high temperature constant temperatures of constant temperature with 2.0 DEG C/h rate of temperature fall, so that crystal fully increases；Wax layer temperature is set to drop to 72.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature with 1.5 DEG C/h rate of temperature fall again, so that crystallization is more abundant.Close the refrigerating function of the circulatory system.
（3）Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅰ）To receive under wax；The sealing system on sweating ware top is installed；Start compressor and keep pressurized buffer pressure inside the tank stable 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 78.0 DEG C with 1.5 DEG C/h heating rate.Stop compressor.
Open vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Wax layer temperature is set to be increased to 83.0 DEG C of simultaneously constant temperature 4.0 hours with 1.0 DEG C/h heating rate, so that the wax in wax layer is sufficiently separated with oil.Stop vavuum pump, terminate sweating degreasing process.
Sweating ware exports changing-over crude product storage tank（Ⅰ）To receive on wax；Continue the temperature of rise recirculated water to 95 DEG C, taken out with fusing on wax, as crude product（Ⅰ）.
（4）Product purification
Crude product（Ⅰ）It is PUR crystallite wax product after clay-filtered, shaping, packaging（Ⅰ）.
PUR crystallite wax product（Ⅰ）Property：Melt drop temperature：85.2 DEG C, oil content：0.85%th, kinematic viscosity（100℃）18.65mm2/ s, meet the index request of aluminum foil seal gasket PUR microwax.PUR crystallite wax product（Ⅰ）Yield be 46.7%（Relative to raw material microwax）.
Embodiment
2
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）Heating-constant temperature sweating,（4）The processes such as product purification.
（1）Preparation
Pad water below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using water as heat-conducting medium, start the heating function of the circulatory system, recirculated water is warming up to 86 DEG C.
With No. 80 microwaxes（With embodiment 1）For raw material, 86 DEG C of fusings are heated to, 0.32% azo diisopropyl imidazoline hydrochloride is added, sweating ware is added after stirring.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, wax layer temperature is dropped to 84.0 DEG C and 2.0 hours progress high temperature constant temperatures of constant temperature with 2.0 DEG C/h rate of temperature fall, so that crystal fully increases；Wax layer temperature is set to drop to 72.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature with 1.5 DEG C/h rate of temperature fall again, so that crystallization is more abundant.Close the refrigerating function of the circulatory system.
（3）Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；The sealing system on sweating ware top is installed；Start compressor and keep pressurized buffer pressure inside the tank stable 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 78.0 DEG C with 1.5 DEG C/h heating rate.Stop compressor.
Open vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.4~-0.6 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Wax layer temperature is set to be increased to 83.0 DEG C of simultaneously constant temperature 4.0 hours with 1.0 DEG C/h heating rate, so that the wax in wax layer is sufficiently separated with oil.Stop vavuum pump, terminate sweating degreasing process.
Sweating ware exports changing-over crude product storage tank（Ⅱ）To receive on wax；Continue the temperature of rise recirculated water to 95 DEG C, taken out with fusing on wax, as crude product（Ⅱ）.
（4）Product purification
Crude product（Ⅱ）It is PUR crystallite wax product after clay-filtered, shaping, packaging（Ⅱ）.
PUR crystallite wax product（Ⅱ）Property：Melt drop temperature：84.8 DEG C, oil content：0.47%th, kinematic viscosity（100℃）18.38mm2/ s, meet the index request of aluminum foil seal gasket PUR microwax.PUR crystallite wax product（Ⅱ）Yield be 51.3%（Relative to raw material microwax）.
Embodiment
3
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）Heating-constant temperature sweating,（4）The processes such as product purification.
（1）Preparation
Pad water below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using water as heat-conducting medium, start the heating function of the circulatory system, recirculated water is warming up to 86 DEG C.
With No. 80 microwaxes（With embodiment 1）For raw material, 86 DEG C of fusings are heated to, 2.8% diacetyl peroxide is added, sweating ware is added after stirring.
Process（2）~（4）With embodiment 2.
PUR manufactured in the present embodiment crystallite wax product（Ⅲ）Property：Melt drop temperature：84.5 DEG C, oil content：0.51%th, kinematic viscosity（100℃）18.42mm2/ s, meet the index request of aluminum foil seal gasket PUR microwax.PUR crystallite wax product（Ⅲ）Yield be 50.6%（Relative to raw material microwax）.
Embodiment
4
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）Heating-constant temperature sweating,（4）The processes such as product purification.
（1）Preparation
Pad water below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；Using water as heat-conducting medium, start the heating function of the circulatory system, recirculated water is warming up to 86 DEG C.
With No. 80 microwaxes（With embodiment 1）For raw material, 86 DEG C of fusings are heated to, 6.5% azodiisobutyronitrile is added, sweating ware is added after stirring.
Process（2）~（4）With embodiment 2.
PUR manufactured in the present embodiment crystallite wax product（Ⅳ）Property：Melt drop temperature：84.2 DEG C, oil content：0.50%th, kinematic viscosity（100℃）18.47mm2/ s, meet the index request of aluminum foil seal gasket PUR microwax.PUR crystallite wax product（Ⅳ）Yield be 51.2%（Relative to raw material microwax）.
The method of the invention for preparing PUR microwax can be seen that by embodiment 1-4, pass through the improvement for increasing pressurization and/or vacuum facility etc. to sweatbox；Dispersed short space is formed in wax layer using gas caused by oil-soluble decomposable asymmetric choice net material, 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 sweating effort；Enhance the separating effect of wax and oil and accelerate separating rate, so that sweating de-oiling technique can prepare PUR crystallite wax product.
Claims (19)
1. a kind of method for preparing PUR microwax, including herein below：
（1）Charging：Using the commodity microwax that melt drop temperature is 75 DEG C~85 DEG C as raw material, the material that oil-soluble decomposable asymmetric choice net produces gas is added after heating fusing, loads sweatbox；
（2）Crystallization：Wax layer is cooled to by proper temperature with 1.0 DEG C/h~3.0 DEG C/h speed, high temperature constant temperature is for a period of time；5 DEG C~20 DEG C below raw material melt drop temperature of cooling final temperature is cooled to 0.5 DEG C/h~2.5 DEG C/h speed again, and cryogenic thermostat is for a period of time；
（3）Sweating：Heated up with 0.5 DEG C/h~2.5 DEG C/h speed；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：After refined it is PUR crystallite wax product on wax.
2. in accordance with the method for claim 1, it is characterised in that the addition that described oil-soluble decomposable asymmetric choice net produces the material of gas is the 0.01%~15.00% of raw material weight.
3. in accordance with the method for claim 2, it is characterised in that the addition that described oil-soluble decomposable asymmetric choice net produces the material of gas is the 0.03%~8.00% of raw material weight.
4. in accordance with the method for claim 1, it is characterised in that the material that described oil-soluble decomposable asymmetric choice net produces gas is selected from one group of material that organic azo compound, sulfonyl hydrazines compound, organic nitroso compounds, organic peroxide are formed.
5. in accordance with the method for claim 4, it is characterised in that described organic azo compound is selected from one group of material that ABVN, azodiisobutyronitrile, azodicarbonamide and azo diisopropyl imidazoline hydrochloride are formed；Described sulfonyl hydrazines compound is selected from one group of material that benzene sulfonyl hydrazide, unifor, 4,4 '-bis oxide (benzene sulfonyl hydrazide) are formed；Described organic nitroso compounds are selected from dinitrosopentamethylene tetramine and/or N, N '-dimethyl N, N '-dinitroso phthalic amide；Described organic peroxide is selected from one group of material that dibenzoyl peroxide, dilauroyl peroxide, dicetyl peroxydicarbonate isopropyl ester and di-cyclohexylperoxy di-carbonate are formed.
6. in accordance with the method for claim 1, it is characterised in that the material that described oil-soluble decomposable asymmetric choice net produces gas is organic azo compound and/or organic peroxide.
7. in accordance with the method for claim 1, it is characterised in that step（2）Described in proper temperature be raw material microwax -1.0 DEG C of melt drop temperature~+2.0 DEG C of melt drop temperature.
8. in accordance with the method for claim 8, it is characterised in that step（2）Described in proper temperature be raw material microwax melt drop temperature~+1.0 DEG C of melt drop temperature.
9. in accordance with the method for claim 1, it is characterised in that step（2）Described in high-temperature constant temperature section time be 0.1~4.0 hour.
10. in accordance with the method for claim 1, it is characterised in that step（2）Described in the predetermined temperature that cools be less than 8 DEG C~15 DEG C of raw material microwax melt drop temperature.
11. in accordance with the method for claim 1, it is characterised in that step（2）Described in the cryogenic thermostat stage time be 0.1~3.0 hour.
12. in accordance with the method for claim 1, it is characterised in that step（3）Described in the predetermined temperature that heats up be less than 2 DEG C~10 DEG C of purpose product melt drop temperature.
13. 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.
14. 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 that described pressure differential is 0.1~5.0 atmospheric pressure.
15. in accordance with the method for claim 14, it is characterised in that the described wax layer that forces air flow through uses the increase air pressure above wax layer to realize, applies the gauge of 0.2~2.0 atmospheric pressure above wax layer, and remains normal pressure below wax layer.
16. in accordance with the method for claim 14, it is characterised in that the described wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized：Air pressure keeps normal pressure above wax layer, and the gauge of -0.2~-0.8 atmospheric pressure is maintained below wax layer.
17. in accordance with the method for claim 1, it is characterised in that the described wax layer that forces air flow through is implemented initial stage in sweating.
18. in accordance with the method for claim 14, it is characterised in that described pressure differential is 0.2~2.0 atmospheric pressure.
19. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
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| CN107513426B (en) | 2019-06-18 |
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