CN110028799A - A kind of high dispersive emulsifying wax and preparation method thereof - Google Patents
A kind of high dispersive emulsifying wax and preparation method thereof Download PDFInfo
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- CN110028799A CN110028799A CN201910297200.0A CN201910297200A CN110028799A CN 110028799 A CN110028799 A CN 110028799A CN 201910297200 A CN201910297200 A CN 201910297200A CN 110028799 A CN110028799 A CN 110028799A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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Abstract
The invention belongs to emulsifying wax production technical fields, and in particular to a kind of high dispersive emulsification wax product for the method and its preparation that emulsifying wax is prepared based on supercritical extraction technique.The method of preparation high dispersive emulsifying wax of the present invention, nano level superfine Wax particles are prepared as emulsifying wax presoma first with supercritical extract process, again by being mixed with single emulsifier or prepared compound emulsifying agent and distilled water in required ratio and sequence, organic solvent can directly obtain final product emulsifying wax in evaporation system while being uniformly mixed.The existing traditional approach of uniformity and partial size based on Wax particles in emulsifying wax prepared by the present invention is not achieved, and stability is also better than traditional approach preparation gained and emulsifies wax product.
Description
Technical field
The invention belongs to emulsifying wax production technical fields, and in particular to one kind prepares emulsifying wax based on supercritical extraction technique
Method and its preparation high dispersive emulsify wax product.
Background technique
Wax is often referred to oil caused by animal, plant or mineral, and the solid of water is insoluble under room temperature, and temperature is slightly higher
When soften, temperature decline when can be hardened, have certain plasticity.Currently, more commonly used wax include paraffin, Fischer-Tropsch wax or its
His natural and synthetic wax, is widely used in the fields such as lubrication, fiberboard, coating, food and fruit freshness preserving.But since wax is normal
Lower temperature is mainly in solid-state, it has not been convenient to be used, therefore, people are by research emulsifying wax come the shortcomings that making up its illiquidity.
Emulsifying wax, which refers to, is evenly dispersed in the various waxes including pertroleum wax in water, inhales by the orientation of emulsifier
Attached effect, and a kind of manufactured homogeneous (uniform) fluid that the content of wax is aqueous is emulsified under mechanical external force effect.Due under emulsifying wax room temperature
In fluid state, it can be diluted use as needed, can use at normal temperature, and have when use without being dissolved through solvent
There is spreadability good and safety, economy, many advantages, such as facilitating.Therefore, emulsifying wax is easier to be applied to plate than general solid wax
The fields such as material production, printing ink, agriculture fresh-keeping and daily chemical products, and there is better application effect.
In the prior art, during preparing emulsifying wax, control wax particle formed mode mainly include mechanical mixing method,
Static mixing method, colloid milling, high pressure homogenizer method and high speed shearing emulsification method etc..Mechanical mixing method is by stirrer paddle
Quickly rotation forms particle after being crushed wax；Wax particles are completed in the flow at high speed impact that static mixing method mainly passes through liquid；
Colloid milling is that the interaction between the stator by centrifugal action and colloid mill and rotor makes wax obtain crushing simultaneously particle
Change；High pressure homogenizer method is that the shear action generated in the pressure hole formed inside homogenizer by wax makes material particle
Change；High speed shearing emulsification rule is by aquashear effect and pressure wave effect so that material micronized.The above method is
Wax after making solid wax by mechanical force or melt realizes micronized, and then completes emulsion process with emulsifier.But
Via wax particle made from above-mentioned mechanical means during emulsification prepares emulsifying wax, ask there is particle diameter distribution is non-uniform
Topic, and cause the stability for emulsifying wax product undesirable in turn, the extensive use of emulsification wax product is limited to a certain extent.
Summary of the invention
For this purpose, technical problem to be solved by the present invention lies in provide one kind to prepare emulsifying wax based on supercritical extraction technique
Method, to solve Mechanical Method in the prior art, to prepare wax particle uneven there are particle and lead to emulsifying wax product stability not
Ideal problem；
Second technical problem to be solved by this invention is to provide a kind of high dispersive prepared by the above method
Emulsifying wax.
In order to solve the above technical problems, a kind of method for preparing high dispersive emulsifying wax of the present invention, including walk as follows
It is rapid:
(1) solid wax stock is put into high-pressure extraction device, it is spare；
(2) solvent is continuously injected into the high-pressure extraction device, while adjusting the temperature in the high-pressure extraction device
And pressure, so that the solvent is reached overcritical or subcritical state, so that the solid wax stock is quickly dissolved in the solvent
In；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
Flow continually out the high-pressure extraction device；Flow out the content of wax solvent of the high-pressure extraction device with the change of pressure and temperature,
Its overcritical or subcritical state releases therewith, and the ultra-fine Wax particles being dissolved in the solvent are precipitated from solvent, is contained
Wax particles slurry；
(4) it takes emulsifier and water and the wax-contained particle slurry to mix to emulsify, and removes the solvent to get required high score
Dissipate emulsifying wax.
Specifically, the solid wax stock includes paraffin, Fischer-Tropsch wax, native paraffin or synthetic wax in the step (1)；
The feeding mode that the solid wax stock puts into the high-pressure extraction device includes directly with the broken solid
Wax stock carry out solid feeding mode, by the liquid feed mode after solid wax stock heating melting to flow regime, or with
The solid-liquid mixed material feeding mode being blended after the solid wax stock is broken with solvent.
It preferably, further include carrying out the high-pressure extraction device to be preheated to the critical of the solvent in the step (1)
The step of temperature ± 50 DEG C.
Specifically, the solvent includes at least one in alkane, aromatic hydrocarbons, alcohols or gas-solvent in the step (2)
Kind.
Preferably, the solvent selection n-alkane, further preferably boiling point are lower than 100 DEG C of normal alkane solvent.
It preferably, further include critical-temperature ± 50 for carrying out the solvent to be preheated to the solvent in the step (2)
DEG C the step of.
Preferably, the temperature of the high-pressure extraction device is set in the critical or subcritical temperature of solvent or more, preferably
Within the scope of solvent critical temperature ± 50 DEG C, pressure is set within the scope of the critical pressure or subcritical pressure of solvent, preferably pressure
For 3-10MPa.
It preferably, further include the content of wax solvent investment knockout drum that will flow out the high-pressure extraction device in the step (3)
The step of, and keep its overcritical or subcritical state releasing by adjusting the pressure and temperature in the knockout drum, it is dissolved in institute
The ultra-fine Wax particles stated in solvent are precipitated from solvent, and the bottom of the knockout drum is gathered in the form of paste wax, or
The ultra-fine Wax particles being precipitated are made to flow into solvent recovery with the solvent by adjusting the flow velocity that the solvent flows out the knockout drum
Tank forms emulsion, and chooses the paste wax and/or emulsion as wax-contained particle slurry and carry out subsequent processing.
Preferably, the mass ratio of the emulsifier, water and the solid wax stock is 10-100:400-2400:800-
820。
Specifically, including the steps that preparing w/o type emulsifying wax or preparation O/W type emulsifying wax in the step (4)；
Described the step of preparing w/o type emulsifying wax is that water is gradually added into the wax-contained particle slurry to emulsify；
The step of preparation O/W type emulsifying wax is that the wax-contained particle slurry is gradually added into water to emulsify.
With it is identical in the prior art, using supercritical extract obtain nanoscale wax particle after, in corresponding single emulsifier
It is organic in mixed system by being removed after being mixed in different order with distilled water by evaporation or under the action of compound emulsifying agent
Solvent, available respective type emulsifying wax.Emulsifying wax during the preparation process, wax is known as oily phase, and aqueous solution is known as water phase, root
Two class emulsifying wax of Water-In-Oil (W/O) type or oil-in-water (W/O) type can successively be made according to oil-water ratio when preparation and mixing.As general
When water is gradually added into oily phase, water phase is scattered in continuous phase in the form of uniform small droplet, forms w/o type reverse micro emulsion；As general
When oil is mutually gradually added into water, oil is mutually scattered in water phase in the form of uniform small droplet, forms O/W positive microemulsion.It is found that
During preparing two types emulsifying wax, water phase and oil are added to sequence and have any different.
Specifically, in the method for the preparation high dispersive emulsifying wax:
In described the step of preparing w/o type emulsifying wax, the HLB value of the emulsifier is 3-6；
In the step of preparation O/W type emulsifying wax, the HLB value of the emulsifier is 8-18.
Emulsifier is the key that prepare emulsifying wax, every kind of emulsifier have specific HLB value (i.e. hydrophilic lipophilic balance,
Hydrophily/lipophilic group lipophilicity of HLB=hydrophilic group), HLB value is bigger, and the hydrophily that represents is stronger, and HLB value is smaller to represent oleophylic
Property is stronger.The HLB value of nonionic surfactant has additive property, and the two or more mixed HLB values of surfactant can be with
By formula HLBAB=(HLBA×WA+HLBB×WB)/(WA+WB) be calculated.Emulsification of the present invention preferably as O/W type emulsion
Agent its HLB value is often between 8-18, often between 3 and 6 as the emulsifier of w/o type emulsion its HLB value.Preparing emulsifying wax
When, in addition to according to the type selection emulsifier of emulsion is wished to get, oil property difference used is also different to the HLB value of emulsifier
It is required that also, emulsifier HLB value should with it is consistent needed for the oily phase that is emulsified.
The invention also discloses the high dispersive emulsifying waxs being prepared by the method.
The method of preparation high dispersive emulsifying wax of the present invention, is original with paraffin or Fischer-Tropsch wax or other natural and synthetic waxs
Material is based on supercritical extraction technique, is shown extremely strong deliquescent principle under its supercriticality using organic solvent, is used
Supercritical solvent extraction method first dissolves solid wax stock, and is when releasing its supercriticality, to make by changing solvent state
Wax particles are precipitated from solvent, can produce partial size during the crystallization of the dissolution and precipitation of wax in Nano grade and the wax that is evenly distributed
Particle, nanoscale wax particle obtained can be evenly distributed on corresponding solvent, so facilitate be made dispersibility more preferably, property
The more stable emulsification wax product of energy.
The method of preparation high dispersive emulsifying wax of the present invention, prepares nano level superfine first with supercritical extract process
Wax particles are as emulsifying wax presoma, then by pressing required ratio with single emulsifier or prepared compound emulsifying agent and distilled water
Example and sequence are mixed, and organic solvent can directly obtain final product cream in evaporation system while being uniformly mixed
Change wax.The existing traditional approach of uniformity and partial size based on Wax particles in emulsifying wax prepared by the present invention is not achieved, surely
It is qualitative also to emulsify wax product better than traditional approach preparation gained.
The emulsified wax appearance that the present invention is prepared is creamy white, and is apparently milky homogeneous liquid, O/W type emulsifying wax
Solid matter wax content is in 30%-50%, and w/o type emulsifying wax solid wax content is in 60%-80%, pH value 7-9, Wax particles diameter
Less than 1 μm, emulsion-stabilizing, stand six months it is not stratified, in use, through arbitrary proportion dilute it is not stratified, be not demulsified, do not agglomerate,
Good dispersion, for qualified emulsification wax product.
Detailed description of the invention
In order to make the content of the present invention more clearly understood, it below according to specific embodiments of the present invention and combines
Attached drawing, the present invention is described in further detail, wherein
Fig. 1 is the process equipment schematic diagram of supercritical extract step of the present invention；
Fig. 2 is the process equipment schematic diagram of the present invention for preparing emulsifying wax step；
Appended drawing reference indicates in figure are as follows: 1- extraction equipment, 2- rectifying column, 3- filter, 4- control valve, 5- surge tank, 6-
Knockout drum, 7- condenser, 8- solvent recovery tank, 9- collecting tank, 10- high-pressure solvent pump, 11- preheater, 12- stirred tank, 13- are produced
Product tank.
Specific embodiment
The method that the high dispersive emulsifying wax is prepared in the following each embodiments of the present invention, is according to process shown in FIG. 1
Figure carries out supercritical extract and prepares paste wax or wax emulsion, and the preparation of emulsifying wax is carried out according to schematic diagram shown in Fig. 2.
As shown in Figure 1, solid wax stock and the solvent after the preheater 11 preheating are put into the extraction equipment 1
In, by controlling the temperature and pressure state in the extraction equipment 1, so that under the solvent of investment is in a supercritical state, and
Continuous supercritical extract processing is carried out to solid wax stock therein, so that the solid wax stock is dissolved completely in the solvent
In；After the completion of extraction, content of wax solvent flows out the extraction equipment 1, and after 3 primary filtration of rectifying column 2 and filter, passes through institute
The adjusting for stating control valve 4 controls via the surge tank 5 and flows into the knockout drum 6 in turn to be passed through in the knockout drum 6
Change the temperature and pressure of whole system, so that the supercriticality of entire dicyandiamide solution releases therewith, at this point, being dissolved in described
Ultra-fine Wax particles in solvent are precipitated from solvent, and the bottom for being gathered in the knockout drum 6 forms paste wax and by the receipts
Collection tank 9 is collected, and isolated solvent then further enters solvent recovery tank 8 after the condensation of condenser 7 and is collected, wherein small part
Ultra-fine Wax particles can enter the solvent recovery tank 8 with solvent and form emulsion, and solvent after the recovery is then through high pressure solvent
It is preheated and is recycled in the investment extraction equipment 1 into the preheater 11 after 10 processing of pump and carry out cycling extraction.
As shown in Fig. 2, taking the emulsion formed in the paste wax or the solvent recovery tank 8 collected in the collecting tank 9
It puts into the stirred tank 12, and is added a selected amount of emulsifier and water is stirred mixing emulsification, the emulsification wax product of formation
Into products pot 13, and the solvent that part is evaporated then realizes recycling into the solvent recovery tank 8 via after condenser 7.
Embodiment 1
The preparation method of high dispersive emulsifying wax described in the present embodiment, including according to flow chart shown in FIG. 1 based on overcritical
Abstraction technique prepares the step of paste wax or wax emulsion, and the step of emulsifying wax preparation is carried out according to schematic diagram shown in Fig. 2
Suddenly, specifically comprise the following steps:
(1) 8.10kg paraffin is prepared into serum, is sent into supercritical extraction unit, and in advance heat extraction equipment system
It is preheated to 220 DEG C；
(2) select pentane for dissolution solvent, critical-temperature is 196.6 DEG C, critical pressure 3.37MPa；Continuously will
Preheated to 220 DEG C of pentane solvent injects in the extraction kettle, while controlling the extraction equipment internal pressure and rising to
6MPa, at this point, the pentane solvent is in a supercritical state, and is continuously extracted to paraffin raw material, so that paraffin is former
Material is quickly dissolved in the pentane solvent；Extraction equipment outlet valve is then adjusted, stablizes system pressure in 6MPa,
It keeps carrying out continuous extraction under this temperature, pressure state, extraction time 1h, it is ensured that entire course of dissolution needs to control entire body
System is constantly under supercriticality；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
It flows continually out the high-pressure extraction device and puts into knockout drum；In the knockout drum, by adjusting the pressure in the knockout drum
Power and temperature release the supercriticality of whole system, at this point, the ultra-fine Wax particles being dissolved in the solvent are from solvent
It is precipitated, and is gathered in the bottom of the knockout drum in the form of paste wax, after measured, after the completion of extraction, obtain containing paraffin
The paste paraffin of 7.98kg；
(4) it takes the sorbester p18 that 0.033kgHLB value is 4.7 and the Tween 80 that 0.081kgHLB value is 15 to be uniformly mixed, obtains
The compound emulsifying agent that HLB value is 12, it is spare；
14.72kg distilled water is added in stirred tank, adds above-mentioned compound emulsifying agent, then by the paste wax of above-mentioned preparation
It is added, starts simultaneously at stirring and heating, mixing speed 600r/min is set, heating temperature is set as 65 DEG C, stirs by 35min
After heating, stirred tank is discharged in no solvent residue in system, obtains O/W type emulsification wax product 22.81kg).After measured, the emulsification
Agent mass fraction in emulsification wax product is 0.5wt%.
Gained emulsifying wax appearance be milky homogeneous liquid, it is transparent, solid wax content be 35.0%, 0.1 μm of average grain diameter,
Water content 64.5%, experiment test condition 35 days it is not stratified, be not demulsified, do not agglomerate, and can mix with water arbitrary proportion, be qualified
O/W type emulsifies wax product.
Embodiment 2
The preparation method of high dispersive emulsifying wax described in the present embodiment, including according to flow chart shown in FIG. 1 based on overcritical
Abstraction technique prepares the step of paste wax or wax emulsion, and the step of emulsifying wax preparation is carried out according to schematic diagram shown in Fig. 2
Suddenly, specifically comprise the following steps:
(1) 8.16kg Fischer-Tropsch wax is prepared into serum, is sent into supercritical extraction unit, and in advance add extraction equipment system
Heat is preheated to 220 DEG C；
(2) select pentane for dissolution solvent, critical-temperature is 196.6 DEG C, critical pressure 3.37MPa；Continuously will
Preheated to 220 DEG C of pentane solvent injects in the extraction kettle, while controlling the extraction equipment internal pressure and rising to
6MPa, at this point, the pentane solvent is in a supercritical state, and is continuously extracted to Fischer-Tropsch wax stock, so that Fischer-Tropsch
Wax stock is quickly dissolved in the pentane solvent；Extraction equipment outlet valve is then adjusted, system pressure is stablized
6MPa keeps carrying out continuous extraction under this temperature, pressure state, extraction time 1h, it is ensured that entire course of dissolution needs to control
Whole system is constantly under supercriticality；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
It flows continually out the high-pressure extraction device and puts into knockout drum；In the knockout drum, by adjusting the pressure in the knockout drum
Power and temperature release the supercriticality of whole system, at this point, the ultra-fine Wax particles being dissolved in the solvent are from solvent
It is precipitated, and is gathered in the bottom of the knockout drum in the form of paste wax, after measured, after the completion of extraction, obtain containing Fischer-Tropsch wax
The paste Fischer-Tropsch wax of 8.04kg；
(4) it takes the sorbester p18 that 0.026kg HLB value is 4.7 and the Tween 80 that 0.108kgHLB value is 15 to be uniformly mixed, obtains
The compound emulsifying agent for being 13 to HLB value, it is spare；
18.60kg distilled water is added in stirred tank, adds above-mentioned compound emulsifying agent, then the paste of above-mentioned preparation is taken
It asks wax to be added, starts simultaneously at stirring and heating, mixing speed 600r/min is set, and heating temperature is set as 65 DEG C, by 35min
After agitating and heating, stirred tank is discharged in no solvent residue in system, obtains O/W type emulsification wax product 26.77kg.After measured, the cream
Agent mass fraction in emulsification wax product is 0.5wt%.
Gained emulsifying wax appearance be milky homogeneous liquid, it is transparent, solid wax content be 30.0%, 0.1 μm of average grain diameter,
Water content 69.5%, experiment test 30 days it is not stratified, be not demulsified, do not agglomerate, and can mix with water arbitrary proportion, for qualification O/W
Type emulsifies wax product.
Embodiment 3
The preparation method of high dispersive emulsifying wax described in the present embodiment, including according to flow chart shown in FIG. 1 based on overcritical
Abstraction technique prepares the step of paste wax or wax emulsion, and the step of emulsifying wax preparation is carried out according to schematic diagram shown in Fig. 2
Suddenly, specifically comprise the following steps:
(1) 8.04kg Fischer-Tropsch wax is prepared into serum, is sent into supercritical extraction unit, and in advance add extraction equipment system
Heat is preheated to 220 DEG C；
(2) select pentane for dissolution solvent, critical-temperature is 196.6 DEG C, critical pressure 3.37MPa；Continuously will
Preheated to 220 DEG C of pentane solvent injects in the extraction kettle, while controlling the extraction equipment internal pressure and rising to
6MPa, at this point, the pentane solvent is in a supercritical state, and is continuously extracted to Fischer-Tropsch wax stock, so that Fischer-Tropsch
Wax stock is quickly dissolved in the pentane solvent；Extraction equipment outlet valve is then adjusted, system pressure is stablized
6MPa keeps carrying out continuous extraction under this temperature, pressure state, extraction time 1h, it is ensured that entire course of dissolution needs to control
Whole system is constantly under supercriticality；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
It flows continually out the high-pressure extraction device and puts into knockout drum；In the knockout drum, by adjusting the pressure in the knockout drum
Power and temperature release the supercriticality of whole system, at this point, the ultra-fine Wax particles being dissolved in the solvent are from solvent
It is precipitated, and is gathered in the bottom of the knockout drum in the form of paste wax, after measured, after the completion of extraction, obtain containing Fischer-Tropsch wax
The paste wax of 7.95kg；
(4) it takes the sorbester p18 that 0.031kgHLB value is 4.7 and the Tween 80 that 0.297kg HLB value is 15 to be uniformly mixed, obtains
The compound emulsifying agent for being 14 to HLB value, it is spare；
23.80kg distilled water is added in stirred tank, adds above-mentioned compound emulsifying agent, then by the paste wax of above-mentioned preparation
It is added, starts simultaneously at stirring and heating, mixing speed 600r/min is set, heating temperature is set as 65 DEG C, stirs by 35min
After heating, stirred tank is discharged in no solvent residue in system, obtains O/W type emulsification wax product 32.08kg.After measured, the emulsifier
Mass fraction is 1wt% in emulsification wax product.
Gained emulsifying wax appearance be milky homogeneous liquid, it is transparent, solid wax content be 25.0%, 0.1 μm of average grain diameter,
Water content 74.0%, sealing place 28 days it is not stratified, be not demulsified, do not agglomerate, and can mix with water arbitrary proportion, for qualification O/W
Type emulsifies wax product.
Embodiment 4
The preparation method of high dispersive emulsifying wax described in the present embodiment, including according to flow chart shown in FIG. 1 based on overcritical
Abstraction technique prepares the step of paste wax or wax emulsion, and the step of emulsifying wax preparation is carried out according to schematic diagram shown in Fig. 2
Suddenly, specifically comprise the following steps:
(1) 8.04kg paraffin is prepared into serum, is sent into supercritical extraction unit, and in advance heat extraction equipment system
It is preheated to 220 DEG C；
(2) select pentane for dissolution solvent, critical-temperature is 196.6 DEG C, critical pressure 3.37MPa；Continuously will
Preheated to 220 DEG C of pentane solvent injects in the extraction kettle, while controlling the extraction equipment internal pressure and rising to
6MPa, at this point, the pentane solvent is in a supercritical state, and is continuously extracted to paraffin raw material, so that paraffin is former
Material is quickly dissolved in the pentane solvent；Extraction equipment outlet valve is then adjusted, stablizes system pressure in 6MPa,
It keeps carrying out continuous extraction under this temperature, pressure state, extraction time 1h, it is ensured that entire course of dissolution needs to control entire body
System is constantly under supercriticality；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
It flows continually out the high-pressure extraction device and puts into knockout drum；In the knockout drum, by adjusting the pressure in the knockout drum
Power and temperature release the supercriticality of whole system, at this point, the ultra-fine Wax particles being dissolved in the solvent are from solvent
It is precipitated, and is gathered in the bottom of the knockout drum in the form of paste wax, after measured, after the completion of extraction, obtain containing paraffin
The paste paraffin of 7.95kg；
(4) it takes the sorbester p17 that 0.115kgHLB value is 4.3 and the polysorbate60 that 0.008kgHLB value is 14.5 to be uniformly mixed, obtains
The compound emulsifying agent for being 5 to HLB value, it is spare；
The paste wax of above-mentioned preparation is added in stirred tank, and above-mentioned compound emulsifying agent is added, adds 4.2kg distillation
Water starts simultaneously at stirring and heating, and mixing speed 600r/min is arranged, and heating temperature is set as 65 DEG C, adds by 35min stirring
After heat, stirred tank is discharged in no solvent residue in system, obtains w/o type emulsification wax product 12.27kg.After measured, the emulsifier
Mass fraction is 1wt% in emulsification wax product.
Gained emulsifying wax appearance is milky homogeneous liquid, and solid wax content is 65.0%, 0.1 μm of average grain diameter, aqueous
Amount 34.5%, sealing place 35 days it is not stratified, be not demulsified, do not agglomerate, and can mix with oily arbitrary proportion, it is newborn for qualified w/o type
Change wax product.
Embodiment 5
The preparation method of high dispersive emulsifying wax described in the present embodiment, including according to flow chart shown in FIG. 1 based on overcritical
Abstraction technique prepares the step of paste wax or wax emulsion, and the step of emulsifying wax preparation is carried out according to schematic diagram shown in Fig. 2
Suddenly, specifically comprise the following steps:
(1) 8.01kg Fischer-Tropsch wax is prepared into serum, is sent into supercritical extraction unit, and in advance add extraction equipment system
Heat is preheated to 220 DEG C；
(2) select pentane for dissolution solvent, critical-temperature is 196.6 DEG C, critical pressure 3.37MPa；Continuously will
Preheated to 220 DEG C of pentane solvent injects in the extraction kettle, while controlling the extraction equipment internal pressure and rising to
6MPa, at this point, the pentane solvent is in a supercritical state, and is continuously extracted to Fischer-Tropsch wax stock, so that Fischer-Tropsch
Wax stock is quickly dissolved in the pentane solvent；Extraction equipment outlet valve is then adjusted, system pressure is stablized
6MPa keeps carrying out continuous extraction under this temperature, pressure state, extraction time 1h, it is ensured that entire course of dissolution needs to control
Whole system is constantly under supercriticality；
(3) make the solvent for having dissolved the solid wax stock under overcritical or subcritical state in holding whole system
It flows continually out the high-pressure extraction device and puts into knockout drum；In the knockout drum, by adjusting the pressure in the knockout drum
Power and temperature release the supercriticality of whole system, at this point, the ultra-fine Wax particles being dissolved in the solvent are from solvent
It is precipitated, and is gathered in the bottom of the knockout drum in the form of paste wax, after measured, after the completion of extraction, obtain containing Fischer-Tropsch wax
The paste Fischer-Tropsch wax of 7.91kg；
(4) it takes the sorbester p17 that 0.110kgHLB value is 4.3 and the polysorbate60 that 0.022kgHLB value is 14.5 to be uniformly mixed, obtains
The compound emulsifying agent for being 6 to HLB value, it is spare；
The above-mentioned paste wax being prepared is added in stirred tank, and above-mentioned compound emulsifying agent is added, adds 5.08kg
Distilled water starts simultaneously at stirring and heating, and mixing speed 600r/min is arranged, and heating temperature is set as 65 DEG C, stirs by 35min
After mixing heating, stirred tank is discharged in no solvent residue in system, obtains w/o type emulsification wax product 13.12kg.After measured, the cream
Agent mass fraction in emulsification wax product is 1wt%.
Gained emulsifying wax appearance is milky homogeneous liquid, and solid wax content is 60.0%, 0.1 μm of average grain diameter, aqueous
Amount 39.0%, sealing place 28 days it is not stratified, be not demulsified, do not agglomerate, and can mix with oily arbitrary proportion, it is newborn for qualified w/o type
Change wax product.
Experimental example
The performance that wax product is emulsified made from above-described embodiment 1-5 is examined according to prior art common detection methods
It surveys, specific Testing index and testing result see the table below 1.
1 emulsifying wax properties of product testing result of table.
From upper table data it is found that the present invention is based on supercritical extraction techniques to extract solid wax stock system with organic solvent
The method of standby emulsifying wax, emulsifying wax product appearance obtained are creamy white, and are apparently milky homogeneous liquid, O/W type emulsifying wax
Solid matter wax content is in 30%-50%, and w/o type emulsifying wax solid wax content is in 60%-80%, pH value 7-9；And entire emulsification
In wax product, wax exists with nanoparticular form, and Wax particles diameter is less than 1 μm, emulsion-stabilizing, stand six months regardless of
Layer, product stability is good and emulsifies wax product better than traditional approach preparation gained；In use, through arbitrary proportion dilute it is not stratified,
It is not demulsified, do not agglomerate, good dispersion, for qualified emulsification wax product.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of method for preparing high dispersive emulsifying wax, which comprises the steps of:
(1) solid wax stock is put into high-pressure extraction device, it is spare；
(2) solvent is continuously injected into the high-pressure extraction device, while adjusting temperature and pressure in the high-pressure extraction device
Power makes the solvent reach overcritical or subcritical state, so that the solid wax stock is quickly dissolved in the solvent；
(3) keep the solvent for having dissolved the solid wax stock continuous under overcritical or subcritical state in holding whole system
Flow out the high-pressure extraction device；The content of wax solvent of the high-pressure extraction device is flowed out with the change of pressure and temperature, is surpassed
Critical or subcritical state releases therewith, and the ultra-fine Wax particles being dissolved in the solvent are precipitated from solvent, obtains the content of wax
Grain slurry；
(4) it takes emulsifier and water and the wax-contained particle slurry to mix to emulsify, and removes the solvent to get required high dispersive cream
Change wax.
2. the method for preparation high dispersive emulsifying wax according to claim 1, which is characterized in that described in the step (1)
Solid wax stock includes paraffin, Fischer-Tropsch wax, native paraffin or synthetic wax；
The feeding mode that the solid wax stock puts into the high-pressure extraction device includes directly former with the broken solid wax
Expect the solid feeding mode carried out, by the liquid feed mode after solid wax stock heating melting to flow regime, or with described
The solid-liquid mixed material feeding mode being blended after solid wax stock is broken with solvent.
3. the method for preparation high dispersive emulsifying wax according to claim 1 or 2, which is characterized in that in the step (1),
Further include the steps that 50 DEG C of the critical-temperature for carrying out the high-pressure extraction device to be preheated to solvent soil.
4. the method for preparation high dispersive emulsifying wax according to claim 1-3, which is characterized in that the step
(2) in, the solvent includes at least one of alkane, aromatic hydrocarbons, alcohols or gas-solvent.
5. the method for preparation high dispersive emulsifying wax according to claim 4, which is characterized in that described in the step (2)
Solvent be boiling point lower than 100 DEG C, critical pressure be 3-10MPa normal alkane solvent.
6. the method for preparation high dispersive emulsifying wax according to claim 1-5, which is characterized in that the step
(2) in, further include the steps that carrying out the solvent into critical-temperature ± 50 DEG C for being preheated to the solvent.
7. the method for preparation high dispersive emulsifying wax according to claim 1-6, which is characterized in that the step
(3) in, further include the steps that the content of wax solvent investment knockout drum that will flow out the high-pressure extraction device, and by adjusting described point
Keep its overcritical from the pressure and temperature in tank or subcritical state releases, is dissolved in ultra-fine Wax particles in the solvent from molten
It is precipitated in agent, and is gathered in the bottom of the knockout drum in the form of paste wax, or by adjusting described in the solvent outflow
The flow velocity of knockout drum makes the ultra-fine Wax particles being precipitated flow into solvent recovery tank formation emulsion with the solvent, and chooses the cream
Shape wax and/or emulsion are as wax-contained particle slurry progress subsequent processing.
8. the method for preparation high dispersive emulsifying wax according to claim 1-7, which is characterized in that the emulsification
The mass ratio of agent, water and the solid wax stock is 10-100: 400-2400: 800-820.
9. the method for preparation high dispersive emulsifying wax according to claim 1-8, which is characterized in that the step
(4) in, include the steps that preparing w/o type emulsifying wax or preparation O/W type emulsifying wax；
Described the step of preparing w/o type emulsifying wax is that water is gradually added into the wax-contained particle slurry to emulsify, the cream
The HLB value of agent is 3-6；
The step of preparation O/W type emulsifying wax is that the wax-contained particle slurry is gradually added into water to emulsify, the cream
The HLB value of agent is 8-18.
10. the high dispersive emulsifying wax being prepared by any one of claim 1-9 the method.
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