CN107523343A - A kind of method of sweating production plastic processing wax - Google Patents
A kind of method of sweating production plastic processing wax Download PDFInfo
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- CN107523343A CN107523343A CN201710444657.0A CN201710444657A CN107523343A CN 107523343 A CN107523343 A CN 107523343A CN 201710444657 A CN201710444657 A CN 201710444657A CN 107523343 A CN107523343 A CN 107523343A
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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
- 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 of sweating production plastic processing wax.The inventive method is using the Tissuemat E of polyethylene by-product as sweating raw material, on the basis of common sweating process, the quick discharge of liquid composition during sweating raw material is formed into stable micro-bubble in favor of sweating effort in wax layer in the presence of bubble stabilizer, liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow in sweating effort simultaneously, so as to effectively remove the lower-molecular-weight component in raw material.The inventive method has the advantages that equipment investment is low, production process is simple and operating cost is low, safe and solvent-free pollution, and products therefrom can be used as plastic processing used additives.
Description
Technical field
The invention belongs to Wax special production technical field, more particularly to a kind of side of sweating production plastic processing wax
Method.
Background technology
Wax is the auxiliary agent commonly used in plastic processing, is such as used as the lubricant of various plastic processings.
The lubricant used in plastic processing is in order to improve plastics, particularly thermoplastic, in machine-shaping
Mobility and release property, its main function be reduce in process between plastic material and processing equipment and with plastics material
Expect the phase mutual friction between interior molecules, so as to improve the processing characteristics of plastics, and improve the performance of product.While lubricant is also
Melting accelerator can be played, prevented adhesion with antistatic agent, slipping agent etc..
According to the mechanism of action of the lubricant in plastics forming, lubricant is divided into in-lubricant and external lubricant.
Lubricant has many uses, hard PVC, polyolefin, PS, ABS, phenolic resin, melmac, cellulose acetate, insatiable hunger
With polyester, polyamide and rubber etc. some lubricants are all used in processing.The polymer of low molecule amount, such as Tissuemat E,
It is used as lubricant extensively, its inside and outside lubricity is all preferable and nontoxic, is processed suitable for the material such as PVC extrusion molding, calendering.
In polythene production process, a small amount of oligomer can be produced, i.e., low molecular weight polyethylene or do Tissuemat E.
The melt drop temperature of the Tissuemat E of some polyethylene by-products is 70 DEG C~95 DEG C, is typically carried out that piece is made after simply decolourizing
Or powder is sprayed into, such Tissuemat E product molecular weight distribution is wide, melting range is wide.It is big due to containing in the Tissuemat E in this source
The low-molecular-weight component of amount, plastic products can be produced with many bad influences when being directly used as plastic processing additives.
In terms of wax product production technology, conventional separation manufacturing process has distillation, solvent separation, sweating separation etc..
Distillation is to reach the purpose of separating-purifying using the boiling point difference of different hydrocarbons, and the boiling range for reducing distillation can be effective
Reduce the width of product carbon distribution, such as CN201410217632.3（A kind of method for improving Fischer-Tropsch wax pour point）Introduce raw material
Low-boiling point material is removed under high temperature high vacuum, then further distillation is refined under XHV, to prepare high melting-point wax product.
Still-process needs raw material being heated to more than boiling point, consumes substantial amounts of energy, while the boiling of hydro carbons of the fusing point more than 70 DEG C
O'clock at 500 DEG C（Normal pressure）More than, efficiency is greatly reduced when being separated using distillation.
Solvent separation is the mesh for reaching separation using the different solubility of the alkane of different structure and molecular weight in a solvent
, such as CN200410043806.5（A kind of method for splitting Tissuemat E）、CN201110351185.7（One kind separation polyethylene
The method of accessory substance Tissuemat E）.Solvent separating technology investment of production equipment is big；Need largely to use solvent in production process,
Recycling design needs to consume substantial amounts of energy；Benzene homologues are usually contained in solvent, environment can be impacted；Solvent is inflammable, holds
Easily cause production accident.
Sweating separation method is to carry out separating-purifying using the different property of various component fusing points in wax.Various groups in wax
The molecular weight divided Bu Tong can all make its fusing point different with structure.When being all n-alkane, the larger n-alkane of molecular weight
Fusing point 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
To be less than n-alkane, and isomery degree more high-melting-point is lower.So sweating separation method can reduce the distribution of product carbon
Width and can improves normal paraffin content.
Compared with distillating method, because the melting temperature of various hydro carbons is far below boiling temperature, so sweating separation process
Energy consumption far below distillation；Compared with solvent fractionation method, sweating separation process is without using solvent, so sweating separation process is pacified
Entirely, save and on environment without influence.
Common sweating process mainly includes the following steps that：（1）Preparation：Pad water（Sweatbox ware plate is full of with water
Lower space）After feed（Load sweatbox when raw material is heated to more than fusing point being in a liquid state）；（2）Crystallization：By raw material with little
10 DEG C~20 DEG C are progressively cooled to below its fusing point in 4 DEG C/h rate of temperature fall.In cooling procedure, various components by fusing point by
High to Low order crystallizes to form solid successively；（3）Sweating：After wax layer temperature reaches default cooling final temperature, put
Fall to pad water；Raw material is slowly heated to default sweating final temperature again.In sweating effort, various components are by fusing point by low
Successively liquid is fused into high order and is flowed out（Under wax）, the wax layer residue that finally obtains（On wax）It is exactly high-melting-point, low
The wax of 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, is thick
Product）, through clay-filtered（Predetermined temperature is warming up to after crude product is melted, carclazyte is added and constant temperature was stirred to the scheduled time
Filtering）Afterwards, reshaping, packaging are purpose product.
To common sweating method, the solids fraction in sweating effort（The wax of higher melt）And liquid composition（It is oily and relatively low
The wax of fusing point）Although being respectively at two kinds of phases of solid and liquid, it also is difficult to be kept completely separate.To make the oil-containing of final products
Amount meets the requirements, and generally use extends sweating sessions（Reduce programming rate）With the method for improving sweating final temperature, but so
The production cycle can be caused long and product yield declines.
Common sweating process can produce fusing point has the soap of thick flaky crystal structure under 40 DEG C~60 DEG C of solid-state
With wax and low melt point paraffin, it is not suitable for producing wax product of the fusing point more than 70 DEG C.Experiment shows that common sweating process production is molten
O'clock in 70 DEG C or so of wax product, the carbon dispersion of distribution and oil content on sweating later stage wax are unrelated with yield, i.e., the carbon on wax
The dispersion of distribution and oil content do not decline with the decline of yield, and fusing point is produced at 70 DEG C or so with sweating process so so far there are no
Wax product report.
Compared with solvent separates, sweating process is intermittently operated, and product yield is relatively low, the production cycle is longer, but is sent out
Sweat technique have small investment, production process are simple, operating cost is low, production process is safe, energy-conservation and it is environmentally safe etc. excellent
Point, still there is part producer at present using this method production soap manufacturing paraffin product.
For many years, sweating method has obtained some development, such as CN89214332 in equipment and process aspect（Vertical type square is more
Section dividing plate sweat 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 equipment；CN91206202（It is a kind of efficient
Paraffin sweating pot）Improved on sweating process, but these improvement can not still produce wax product of the fusing point more than 70 DEG C.
Sweating process is to be currently known unique solvent-free separation method for commercial scale wax product, green advocating
Color low-carbon, today of environmental protection and energy saving, the demand that plastic processing wax is prepared using sweating process are more urgent.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of method of sweating production plastic processing wax.Specifically
Say it is using the Tissuemat E of polyethylene by-product as sweating raw material, on the basis of common sweating process, preferably sweating raw material exists
Gas is mixed in the presence of bubble stabilizer and stable micro-bubble is formed in wax layer, is advantageous to sweating stage liquid component
Discharge；Simultaneously in sweating effort using air-flow by wax layer to force to separate solids fraction and liquid composition, enhance point
From effect and accelerate separating rate；And increase the constant temperature stage of crystallization and sweating effort, make this solvent-free de-oiling side of sweating
Method can produce melt drop temperature more than 70 DEG C and remove the plastic processing wax of low-melting component substantially.The inventive method has
Investment of production equipment is low, preparation process is simple and operating cost is low, safety, energy-conservation and the advantages that solvent-free pollution.
A kind of method of sweating production plastic processing wax of the present invention, including herein below：
（1）Preparation：Using the Tissuemat E of polyethylene by-product as sweating raw material, bubble stabilizer is added after heating fusing,
Gas is passed through under stirring and loads sweatbox after forming stable micro-bubble；
（2）Crystallization：Wax layer is cooled to by sweating raw material melt drop temperature~+4 DEG C of melt drop temperature with 1.0 DEG C/h~4.0 DEG C/h speed
Temperature range, and high temperature constant temperature is for a period of time；Again with 0.5 DEG C/h~3.5 DEG C/h speed be cooled to sweating raw material melt drop temperature with
Lower 8 DEG C~15 DEG C of crystallization final temperature, and cryogenic thermostat is for a period of time；
（3）Sweating：Heated up with 1.0 DEG C/h~3.0 DEG C/h speed, wax layer reaches predetermined temperature and constant temperature stops afterwards for a period of time
Sweating；Wax layer is forced air flow through in sweating effort；
（4）It is refined：After refined it is plastic processing wax on wax.
In the method for the present invention, described sweating material polyethylene wax is caused oligomer warp in polythene production process
Decolourize, be molded production, its melt drop temperature is usually 70~95 DEG C.
In the method for the present invention, sweating raw material is passed through gas in the presence of bubble stabilizer, formed under agitation stable
Micro-bubble after carry out sweating.Step（1）Described bubble stabilizer is selected from nonionic surface active agent, anionic table
One or more in face activating agent, cationic surface active agent, amphoteric surfactant.The freezing point of surfactant
Or fusing point is less than step（3）The maximum temperature of sweating（That is step（3）Described predetermined temperature）.
Wherein, it is stearic to be selected from sorbitan monooleate, anhydrous sorbitol list for described nonionic surface active agent
Acid esters, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol list are stearic
One group of material that acid esters, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester are formed；It is cloudy
Ionic surfactant is selected from fatty alcohol sulfate monoethanolamine salt, pareth sulfate, oleamide yl carboxylic acid
Sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurates, sodium butylnaphthalenesulfonate, Disodium sulfosuccinate, suitable succinate monoester
One group of material that sodium sulfonate is formed.Described cationic surface active agent is selected from benzyl quaternary ammonium salt, dodecyl dimethyl benzyl
Ammonium chloride, DTAC, cetyl trimethylammonium bromide, OTAC, three second
One group of material that acid amides oleate is formed；Amphoteric surfactant is selected from empgen BB, dodecyl dimethyl oxygen
Change ammonium, aliphatic group imidazolidine derivatives, alkyl imidazoline derivatives, derivative of fatty acid, amphoteric modified epoxy ethane to add
The one group of material formed into thing.
In the method for the present invention, described bubble stabilizer is preferably nonionic surface active agent, anionic surface
One group of material that activating agent and cationic surface active agent mixing are formed.The HLB value of bubble stabilizer is 4~10, preferably 6
~8.The addition of the bubble stabilizer is the 0.01%~10.0% of sweating material quality, preferably 0.1%~2.0%.
In the method for the present invention, step（1）Described in gas can be that chemical property is stable under the conditions of sweating appoint
Will and spirit body, is preferably easy to get and one or more of the air of nontoxic no special odor, carbon dioxide, nitrogen.Mixed gas
Account for the 2%~20% of sweating raw material volume, preferably 5%~10%.
In the method for the present invention, step（1）Described in stirring can use colloid mill or other machinery device.Stirring
Rotating speed is 500~10000 r/min, preferably 1000~8000 r/min, uniform, tiny, stably to be produced in sweating raw material
Foam.
In the method for the present invention, step（2）Described in high-temperature constant temperature section time be 0.1~6.0 hour, preferably 0.5
~5.0 hours, more preferably 1.0~4.0 hours；The time of the cryogenic thermostat is 0.1~5.0h, preferably 0.5~3.0h.
In the method for the present invention, the preferred sweating ware of described sweatbox, and in wax layer pressue device added above and/or
Increase vacuum plant below wax layer, in step（3）During make wax layer up and down form pressure differential.Described pressure air-flow
Used by wax layer increases pressure above wax layer（Air pressure）And/or pressure is reduced below wax layer（Air pressure）, make wax layer upper and lower
Side（Side）Pressure differential is formed to realize.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 air
Pressure, to force air flow through wax layer.
In the method for the present invention, step（3）Described in the predetermined temperature that heats up（That is final temperature）For purpose product drip melt
- 10 DEG C of point~-1 DEG C of purpose product melt drop temperature.After predetermined temperature is warming up to, the increase constant temperature stage can make solids fraction and liquid
The separation of state component is more abundant, and the time in constant temperature stage is 0.1~10.0 hour, preferably 1.0~8.0 hours, most preferably 2.0
~5.0 hours.
In the method for the present invention, the programming rate and cooling rate of said wax layer, air bath, water-bath, oil bath can be passed through
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer is controlled to heat up using water-bath or oil bath mode
When speed and rate of temperature fall, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function, the circulatory system adds the material such as water or conduction oil as circulatory mediator；Coil pipe is soaked after charging
Not and be fixed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the method for the present invention, step（3）The described wax layer that forces air flow through can be real in sweating effort any stage
Apply, preferably implement initial stage in sweating.
In the method for the present invention, step（3）The described wax layer that forces air flow through is utilized in increase air pressure above wax layer
Realize, can such as apply the gauge of 0.2~2.0 atmospheric pressure above wax layer, and normal pressure is remained below wax layer.
In the method for the present invention, step（3）The described wax layer that forces air flow through is utilized in reduction air pressure below wax layer
Realize, normal pressure can be such as kept above wax layer, and the gauge of -0.2~-0.8 atmospheric pressure is maintained below wax layer.
Analysis shows, the melt viscosity of the Tissuemat E of polyethylene by-product is low, and this is with wax to being used as plastic processing
Beneficial, but it is produced much to plastic products when as plastic processing additives due to a large amount of low-melting components be present
Bad influence, when being such as used for PE, PVC plastics, the indexs such as the hardness of product, intensity, softening point, modulus can be caused to reduce；
During for foam PS, it can cause to foam uneven, therefore the Tissuemat E of polyethylene by-product is not suitable for being directly used as plastic processing
Auxiliary agent.
Sweating method is separated using the different property of various component fusing points.For the research table of sweating effort
Bright, liquid composition is gradually discharged along crystalline portion in sweating effort, situation about being flowed similar to liquid in capillary.
But for fusing point in 70 DEG C and the high melting-point wax of the above, because raw material chemical composition is complicated, cause crystals upon crystallization structure thin
Small densification, the discharge to liquid composition form huge filter flow resistance power, and this results in the common sweating for only leaning on gravity natural separation
During solids fraction be difficult to be kept completely separate with liquid composition, therefore common sweating separating technology can not produce fusing point at 70 DEG C and
Wax product above.
The present invention passes through going deep into for the composition of the Tissuemat E to polyethylene by-product to produce plastic processing wax product
Research, a large amount of low-melting components are contained for it（Fusing point is less than 50 DEG C）Cause to be not suitable for being directly used as plastic processing wax
Reason, these non-Suitable ingredients are removed by using sweating method.By the further investigation to common sweating effort, for solid-state
Component is difficult to separate reason with liquid composition, is used in sweating effort and forces air flow through wax layer, and in crystallization process and hair
The processes such as sweat process increase constant temperature stage；Stable, dispersed micro-bubble is formed further preferably in sweating raw material simultaneously
After carry out sweating, these measures effectively removes the non-Suitable ingredients of the plastic processing wax such as low-melting component.
The present invention is in order that this solvent-free de-oiling method of sweating can produce plastic processing wax product, by common
The further investigation of sweating effort, the reason for being difficult to separate with liquid composition for solids fraction in sweating effort, by sweating
During using force air flow through wax layer carry out liquid composition method force solids fraction separated with liquid composition, enhancing
Separating effect simultaneously accelerates separating rate；Increasing the high temperature constant temperature stage in crystallization process can make the crystallization of wax bigger, have
Beneficial to the discharge of liquid composition in sweating effort.Research for wax crystallization process shows that the chemical composition of wax is to determine crystallization
The main factor of form, while the condition of cooling procedure can also influence crystal habit, the temperature especially near melt drop temperature
Under influence of the cooling condition to crystal habit it is most obvious.Wax is when being cooled near melt drop temperature, the N-alkanes of larger molecular weight
Hydrocarbon has formed crystallization and separated out, and this partially crystallizable body can now increase the high temperature constant temperature stage as the nucleus for being subsequently formed crystallization,
Nucleus can be enable fully to increase, form larger sized crystal, although this larger sized crystal is not so good as low melting point stone
The crystallization of wax is thick like that, but it is also highly beneficial that the crystal structure of this increase discharges liquid composition to the sweating stage.Together
When sweating raw material is further preferably passed through gas under bubble stabilizer and mechanical agitation, these gases are in bubble stabilizer
Effect is lower to form stable, dispersed micro-bubble in wax layer.Research shows, from HLB value between 4~10
Bubble stabilizer can produce relatively stable bubble, and bubble stabilizer of the HLB value between 6~8 can produce the foam of exquisiteness
Structure and stability is more preferable；And when using anionic surfactant with cationic surface active agent compounding, due to both
Strong electrostatic interaction, adsorbance of the anions and canons on gas-liquid interface is added, and make intermembranous liquid phase viscosity increase, so as to big
Width improves the stability of bubble, and can forms stable bubble in the case of less dosage in other words.In sweating effort,
These uniform, tiny bubbles are easy to form some tiny passages in wax layer, are advantageous to the discharge of liquid composition, study table
The volume fraction of bright bubble solids fraction and trend that liquid composition separating effect strengthens when within 10% is more apparent, thereafter gas
The increase of foam fraction slows down to the effect tendency of separating effect；Selected surfactant fusing point or freezing point are less than sweating
The maximum temperature of journey, and contain functional group, it is poor with the intermiscibility of paraffin, it can be arranged in sweating effort with liquid composition
Go out.Being aided with the cryogenic thermostat stage again makes solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction and liquid
The methods of component separation is more abundant so that sweating process can produce the plastic processing wax for not containing low-melting component.
This have the advantage that：The method for carrying out liquid composition by wax layer using air-flow in sweating effort is strong
The separation of solids fraction processed and liquid composition, enhance separating effect and accelerate separating rate；Increased using high temperature crystallization brilliant
Body size, while micro-bubble is formed in wax layer using gas, it is also beneficial to the quick discharge of liquid composition；And increase low temperature
The process such as constant temperature stage and the constant temperature stage of sweating effort, so that sweating process can produce plastic processing wax.This hair
Bright method has that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution environment etc. are excellent
Point.
Embodiment
The present invention is sweating raw material from the Tissuemat E of polyethylene by-product, on the basis of common sweating process, sweating
Ware top connects dismountable sealing device and is connected with pressurized buffer tank and compressor, and/or connection subtracts in sweating ware bottom
Press surge tank and vavuum pump；The heating of sweating raw material is melted and is preferably added to bubble stabilizer, is filled after forming stable micro-bubble
Enter sweating ware；Wax layer heating-cooling speed is controlled with oil bath；Wax layer temperature is down to sweating raw material melt drop temperature temperature nearby and high-temperature constant
Warm 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；Purpose product is plastic processing wax after refined
Product.
The method that 1-2 illustrates the sweating production plastic processing wax of the present invention by the following examples.As without especially
Indicate, it is mass percent to be related to % below, and the pressure is gauge pressure.
Embodiment 1
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization,（3）Heating-
Constant temperature sweating,（4）Refine four steps.
（1）Preparation
The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed simultaneously in sweating ware bottom
Connect vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；With heat conduction
Oil is heating medium；Start the heating function of the circulatory system, recycle oil is warming up to 95 DEG C.Pad water below sweating ware ware plate.
The Tissuemat E of Liaoyang petrifaction ethylene factory of CNPC polyethylene device by-product（85.8 DEG C of melt drop temperature；Needle penetration（25
℃）52（10-1mm）；Needle penetration（55℃）＞ 200（10-1mm）.It can be seen that in the raw material and contain from the needle penetration of 25 DEG C and 55 DEG C
There are a large amount of low melting points）0.6 % diethylene glycol fatty acid ester, 0.1% suitable succinic acid list are added after being heated to 95 DEG C of fusings
Ester sodium sulfonate and 0.1% cetyl trimethylammonium bromide, air is passed through after well mixed, while with colloid mill in 3000r/
Stirring is stopped being passed through after air and stirred again with 7500r/min speed to sweating raw material volume increase by 5% under min speed
10min adds sweating ware after uniform, tiny bubble to be formed.The sealing system of sweating ware is installed.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, control wax layer temperature drops to wax layer temperature with 2.0 DEG C/h rate of temperature fall
88.0 DEG C and 3.0 hours progress high temperature constant temperatures of constant temperature, so that crystal fully increases；Wax layer is made with 1.5 DEG C/h rate of temperature fall again
Temperature drops to 75.0 DEG C so that wax layer crystallizes to form solid, and constant temperature 3.0h is so that wax layer crystallization is more abundant.Close cyclic system
The refrigerating function of system.
（3）Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅰ）To receive under wax；Start compressor and keep pressurization slow
Rush the stable holding normal pressure below 1.5~1.7 atmospheric pressure, sweating ware ware plate of pressure inside the tank；Start circulation system function,
Wax layer temperature is set to be increased to 84.0 DEG C with 1.5 DEG C/h heating rate.Stop compressor.
Open vavuum pump and keep the stable air pressure above -0.5~-0.7 atmospheric pressure, wax layer of pressure-reducing cushioning pressure inside the tank
Keep normal pressure；Wax layer temperature is set to be increased to 89.0 DEG C of simultaneously constant temperature 4.0 hours with 1.5 DEG C/h heating rate, so that in wax layer
Solids fraction and liquid composition are sufficiently separated.Stop vavuum pump, terminate sweating effort.
The outlet of sweating ware is changed to connect crude product storage tank（Ⅰ）To receive on wax.Continue to raise the temperature of conduction oil to 115
DEG C, taken out with fusing on wax, as crude product（Ⅰ）.
（4）It is refined
Crude product（Ⅰ）It is plastic processing wax product after clay-filtered（Ⅰ）.
Plastic processing wax product（Ⅰ）Property：92.3 DEG C of melt drop temperature；Needle penetration（25℃）2（10-1mm）；Needle penetration（55
℃）29（10-1mm）.Plastic processing wax product（Ⅰ）Yield is 27.6%（Relative to the polyethylene of sweating material polyethylene by-product
Wax）.
Plastic processing wax product is can be seen that from 25 DEG C and 55 DEG C of needle penetrations（Ⅰ）Middle low melting point removes substantially.
Embodiment 2
The present embodiment includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization,（3）Heating-
Constant temperature sweating,（4）Refine four steps.
（1）Preparation
The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed simultaneously in sweating ware bottom
Connect vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；With heat conduction
Oil is heating medium；Start the heating function of the circulatory system, recycle oil is warming up to 95 DEG C.Pad water below sweating ware ware plate.
The Tissuemat E of Liaoyang petrifaction ethylene factory of CNPC polyethylene device by-product（With embodiment 1）95 DEG C are heated to melt
1.0% sorbitan monooleate, 0.3% sodium alkyl benzene sulfonate and 0.3% dodecyl dimethyl benzyl is added after change
Ammonium chloride, nitrogen is passed through after well mixed, while is stirred to sweating raw material volume and increased under 2000r/min speed with colloid mill
Add 9%, stop being passed through and sent out again with 6000r/min speed stirring 10min with being formed after uniform, tiny bubble to add after nitrogen
Sweat ware.The sealing system of sweating ware is installed.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, control wax layer temperature drops to wax layer temperature with 2.5 DEG C/h rate of temperature fall
88.0 DEG C and 2.0 hours progress high temperature constant temperatures of constant temperature, so that crystal fully increases；Wax layer is made with 2.0 DEG C/h rate of temperature fall again
Temperature drops to 75.0 DEG C so that wax layer crystallizes to form solid, and constant temperature 2.0h is so that wax layer crystallization is more abundant.Close cyclic system
The refrigerating function of system.
（3）Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；Start compressor and keep pressurizeing
Buffer the stable holding normal pressure below 1.5~1.7 atmospheric pressure, sweating ware ware plate of pressure inside the tank；Start circulation system work(
Can, wax layer temperature is increased to 84.0 DEG C with 2.0 DEG C/h heating rate.Stop compressor.
Open vavuum pump and keep the stable air pressure above -0.5~-0.7 atmospheric pressure, wax layer of pressure-reducing cushioning pressure inside the tank
Keep normal pressure；Wax layer temperature is set to be increased to 89.0 DEG C of simultaneously constant temperature 3.0 hours with 2.0 DEG C/h heating rate, so that in wax layer
Solids fraction and liquid composition are sufficiently separated.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 the temperature of conduction oil to 115
DEG C, taken out with fusing on wax, as crude product（Ⅱ）.
（4）It is refined
Crude product（Ⅱ）It is plastic processing wax product after clay-filtered（Ⅱ）.
Plastic processing wax product（Ⅱ）Property：92.6 DEG C of melt drop temperature；Needle penetration（25℃）2（10-1mm）；Needle penetration（55
℃）25（10-1mm）.Plastic processing wax product（Ⅱ）Yield is 30.5%（Relative to the poly- second of sweating material polyethylene by-product
Alkene wax）.
Plastic processing wax product is can be seen that from 25 DEG C and 55 DEG C of needle penetrations（Ⅱ）Middle low melting point removes substantially.
The present invention can be seen that by embodiment 1-2 sweating production modeling of the invention is can be seen that by embodiment 1-4
Processing wax method is expected, by increasing the improvement to sweatbox such as pressurization and/or vacuum facility；By the way that sweating raw material is mixed into
Constant temperature stage of micro-bubble, increase crystallization and sweating effort etc. is formed after bubble stabilizer in wax layer using gas to sweating
The improvement of technique；Enhance the separating effect of solids fraction and liquid composition and accelerate separating rate, so as to effectively eliminate
Lower-molecular-weight component in raw material, sweating process is set to produce plastic processing wax product.
Claims (18)
1. a kind of method of sweating production plastic processing wax, including herein below：
（1）Preparation：Using the Tissuemat E of polyethylene by-product as sweating raw material, bubble stabilizer is added after heating fusing,
Gas is passed through under stirring and loads sweatbox after forming stable micro-bubble；
（2）Crystallization：Wax layer is cooled to by sweating raw material melt drop temperature~+4 DEG C of melt drop temperature with 1.0 DEG C/h~4.0 DEG C/h speed, and
High temperature constant temperature is for a period of time；8 DEG C~15 DEG C are cooled to below sweating raw material melt drop temperature with 0.5 DEG C/h~3.5 DEG C/h speed again
Crystallization final temperature, and cryogenic thermostat is for a period of time；
（3）Sweating：Heated up with 1.0 DEG C/h~3.0 DEG C/h speed, wax layer reaches predetermined temperature and constant temperature stops afterwards for a period of time
Sweating；Wax layer is forced air flow through in sweating effort；
（4）It is refined：After refined it is plastic processing wax on wax.
2. in accordance with the method for claim 1, it is characterised in that described bubble stabilizer is selected from non-ionic surfactant
One group of material that agent, anionic surfactant, cationic surface active agent, amphoteric surfactant are formed；Surface
The freezing point or fusing point of activating agent are less than step（3）The maximum temperature of sweating.
3. in accordance with the method for claim 2, it is characterised in that the HLB value of described bubble stabilizer is 4~10, preferably
For 6~8.
4. according to the method described in Claims 2 or 3, it is characterised in that described nonionic surface active agent is selected from dehydration
Sorbitol monooleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, dehydration
It is sorbierite monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, poly-
One group of material that oxygen ethene fatty acid ester is formed；Described anionic surfactant is selected from fatty alcohol sulfate MEA
Salt, pareth sulfate, oleamide yl carboxylic acid sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurates, butyl
Sodium naphthalene sulfonate, Disodium sulfosuccinate, the one group of material formed along succinate monoester sodium sulfonate；Described cationic is lived
Property agent be selected from benzyl quaternary ammonium salt, dodecyl benzyl dimethyl ammonium chloride, DTAC, cetyl front three
One group of material that base ammonium bromide, OTAC, triacetamide oleate are formed；Live on described amphoteric surface
Property agent is selected from empgen BB, OA-12, aliphatic group imidazolidine derivatives, alkyl imidazoline spread out
One group of material that biology, derivative of fatty acid, amphoteric modified epoxy ethane additive product are formed.
5. in accordance with the method for claim 2, it is characterised in that described bubble stabilizer is non-ionic surfactant
One group of material that agent, anionic surfactant and cationic surface active agent mixing are formed.
6. in accordance with the method for claim 1, it is characterised in that described bubble stabilizer addition is sweating material quality
0.01%~10.0%, preferably 0.1%~2.0%.
7. in accordance with the method for claim 1, it is characterised in that described gas is air, carbon dioxide, in nitrogen extremely
Few one kind.
8. in accordance with the method for claim 1, it is characterised in that described stirring uses colloid mill, and rotating speed is 500~
10000 r/min。
9. in accordance with the method for claim 1, it is characterised in that the mixed gas account for sweating raw material volume 2%~
20%, preferably 5%~10%.
10. in accordance with the method for claim 1, it is characterised in that step（2）Described in time of high-temperature constant temperature section be
0.1~6.0 hour, the time of cryogenic thermostat section was 0.1~5.0h.
11. in accordance with the method for claim 1, it is characterised in that step（3）Described in force air flow through wax layer use
Increase air pressure above wax layer and/or air pressure is reduced below wax layer, wax layer upper and lower is formed pressure differential and realize, described pressure
Power difference is 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure.
12. in accordance with the method for claim 1, it is characterised in that step（3）Described in produce for the purpose of the predetermined temperature that heats up
- 10 DEG C of product melt drop temperature~-1 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 for 0.1~
10.0 hours.
14. in accordance with the method for claim 1, it is characterised in that described forces air flow through wax layer in sweating reality at initial stage
Apply.
15. in accordance with the method for claim 11, it is characterised in that the described wax layer that forces air flow through is used in wax layer
Fang Zengjia air pressure is realized, 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 11, it is characterised in that the described wax layer that forces air flow through is used under wax layer
Side reduces air pressure and realized, air pressure keeps normal pressure above wax layer, and the table of -0.2~-0.8 atmospheric pressure is maintained below wax layer
Pressure pressure.
17. according to the method described in claim 1, it is characterised in that the melt drop temperature of described Tissuemat E is 70~95 DEG C.
18. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
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| CN2016104330160 | 2016-06-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111205891A (en) * | 2018-11-21 | 2020-05-29 | 内蒙古伊泰煤基新材料研究院有限公司 | Wax for plastic processing and preparation method thereof |
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