CN107523224A - The method for producing wax polish - Google Patents
The method for producing wax polish Download PDFInfo
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- CN107523224A CN107523224A CN201710444763.9A CN201710444763A CN107523224A CN 107523224 A CN107523224 A CN 107523224A CN 201710444763 A CN201710444763 A CN 201710444763A CN 107523224 A CN107523224 A CN 107523224A
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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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/08—Other polishing compositions based on wax
- C09G1/10—Other polishing compositions based on wax based on mixtures of wax and natural or synthetic resin
- C09G1/12—Other polishing compositions based on wax based on mixtures of wax and natural or synthetic resin mixtures of wax and silicon-containing polycondensates
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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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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Cosmetics (AREA)
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Abstract
The invention discloses a kind of method for producing wax polish.This method is using F T synthetic products as raw material, through sweating, allotment production purpose product.The inventive method is on the basis of common sweating process, liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow in sweating effort, sweating is carried out after preferably the aqueous solution with the two or more materials for reacting generation gas is emulsified respectively simultaneously, increase thermostatic process in crystallization process, the quick discharge of liquid composition is also beneficial to, so as to produce the basic material for being free of low-melting component；It is glazing wax product that basic material is allocated with components such as silicone oil, native paraffin, solvents again.The inventive method has the advantages that investment of production equipment is low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution, and glazing wax product resistance to elevated temperatures is good.
Description
Technical field
The invention belongs to daily chemical product production technical field, more particularly to a kind of method for producing wax polish, especially
It applies to various hard surfaces（Floor, furniture, automobile etc.）Glazing wax product production method.
Background technology
Glazing product mainly produces or recovers various surfaces（Floor, furniture, automobile etc.）Gloss, while play clear
Clean, wear-resistant, anticorrosion（Expose to the weather）, waterproof, high temperature resistance, antiultraviolet, antistatic, the effect such as scratch resistance.
Wax polish is different by mode of appearance, can be divided into the types such as solid, lotion, liquid.It is different by decentralized medium, it can be divided into
The types such as solvent is scattered, emulsion dispersion；From composition, wax polish includes volatile component and film-forming components and accessory ingredients
（Emulsifying agent, grinding agent, thickener, antioxidant, UV resistant agent, essence etc.）Three major types material.Volatile component（To solvent point
It is various organic solvents to dissipate class product, is the materials such as water, alcohol to emulsion dispersion class product）It is intended, primarily, to improve the construction of wax polish
Performance is simultaneously cleaned by the stain of coating surface；Film-forming components play the effect such as glazing.The film-forming components of wax polish generally comprise wax,
Silicone oil, resin（Polycarbonate resin, polyurethane resin, fluororesin, polyacrylate resin etc.）Deng hydrophobic substance.Wax polish is made
Wax mainly includes pertroleum wax（Paraffin, microwax）, native paraffin（Beeswax, Chinese wax, Ka Naba waxes, candelila wax, lignite
Wax, rice bran wax etc.）, synthetic wax（Tissuemat E, polypropylene wax, OPE, its chlorinated polypropylene wax）Deng.
Using the plaster body wax polish that solvent disperses using earliest, have the brightness for wiping rear cere, gloss it is lasting
The advantages that property and water-resistance etc. are all relatively good, is used widely so far.
Some glazing wax products can run into higher environment temperature in use, if Automotive Paint Film Properties coating surface is in the summer
Maximum temperature is up to 70 DEG C~80 DEG C during its Exposure to Sunlight, if containing excessive low-melting component in formula, the cere of formation is in high temperature
It is easier to soften under environment, causes to adsorb dust, the gloss for making coating surface is declined, influences to need the outward appearance of glazing article.
Various native paraffins and synthetic wax can produce preferable gloss and heat-resist, but price is high.
The general name of the pertroleum wax obtained all kinds of wax products that are crude oil after refining is processed from wax-containing distillate, including liquid
Body paraffin, soap manufacturing paraffin, paraffin and microwax.Paraffin be in crude oil lube cut through steps such as dewaxing, de-oiling, refined and shapings
Production, typically contain C20~C50The component such as n-alkane, isoparaffin and a small amount of cycloalkane, usual fusing point is 50 DEG C~
74℃.Microwax 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, usual melt drop temperature be 65 DEG C~92 DEG C, Gu
There is the needle-like crystal structure more tiny than paraffin under state.
In pertroleum wax production process, dewaxing is that the slack wax that oil content is 10~30% or so is prepared by raw material of crude oil fractions
Process.De-oiling is that the process of base oil wax of the oil content below 2% is prepared using slack wax as raw material, and de-oiling technique mainly has solvent
De-oiling and sweating de-oiling.Base oil wax is again through clay-filtered or hydrofinishing and shaping, packaging and other steps, you can obtains commodity stone
Oily wax.
Pertroleum wax is the hydrocarbon mixture of the n-alkane, isoparaffin, cycloalkane of a variety of carbon numbers etc., carbon number distribution compared with
Width, therefore must wherein contain a number of low-melting component（Oily and relatively low fusing point wax）.Excessive use stone in wax polish
The pertroleum waxes such as wax, microwax can cause glazing film poor heat resistance.
Fischer-Tropsch（F-T）Synthetic technology is nineteen twenty-three invention, mainly includes high temperature synthesis techniques and low temperature synthesis technique,
F-T synthesis techniques and catalyst all achieve breakthrough progress since nineteen nineties, and F-T sinteticses are increasingly rich
It is rich.In F-T synthetic product chemical compositions based on n-alkane, there is a small amount of isoparaffin, also contain more alkene and oxygen-containing
Compound, and carbon number distribution is very wide.F-T synthetic products are due to containing a large amount of low-melting components, being directly used in wax polish formula
In can also make glazing film poor heat resistance.
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
The width of product carbon distribution is reduced, but still-process needs raw material being heated to more than boiling point, consumes substantial amounts of energy.Such as
CN201410217632.3（A kind of method for improving Fischer-Tropsch wax pour point）Introduce and raw material is removed into low boiling under high temperature high vacuum
Point material, then further distillation is refined under XHV, to prepare high melting-point wax product.Hydrocarbon of the fusing point more than 70 DEG C simultaneously
The boiling point of class is at 500 DEG C（Normal pressure）More than, efficiency is greatly reduced when being separated using distillation.
Solvent fractionation method is to carry out separating-purifying using the property of the different solubility of various components in a solvent in wax
, 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）, production of the gained high melting point polyethylene wax available for products such as wax polishs.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；Lead in solvent
Often contain benzene homologues, environment can be impacted；Solvent is inflammable, easily causes 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.
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.
Common sweating process can produce soap manufacturing paraffin and low melt point paraffin of the fusing point at 40 DEG C~60 DEG C, and it is molten to be not suitable for production
Wax product o'clock more than 70 DEG C.When common sweating process produces 40 DEG C~60 DEG C of soap manufacturing paraffin and low melt point paraffin, sweating
Solids fraction in journey（The wax of higher melt）And liquid composition（Oil and the wax compared with low melting point）Although two class components are respectively at solid
Two kinds of phases of body and liquid, but also be difficult to be kept completely separate.To make final products meet the requirements, generally use extends sweating sessions
（Reduce programming rate）And the method for improving sweating final temperature, but can so cause production cycle length and product yield decline；
When experiment shows wax product of the common sweating process production fusing point more than 70 DEG C, the carbon dispersion of distribution on sweating later stage wax and just
Structure Determination of Alkane Content is unrelated with yield, i.e., the carbon dispersion of distribution on wax does not decline with the decline of yield, and normal paraffin content is not yet
Improved with the decline of yield, report of the fusing point in 70 DEG C or so of wax product is produced with sweating process so so far there are no.
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, people is increasingly caused using high melting-point wax product of the sweating process production without low melting point
Concern, while while the performances such as wax polish high temperature resistant are not influenceed reduce glazing wax product production cost demand more
Add urgent.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of method for producing wax polish, including emulsification, sweating, tune
With three parts.It is sweating raw material specifically by more than 80% F-T synthetic products of n-alkane weight content, general
On the basis of logical sweating process, the aqueous solution that sweating raw material and two kinds and the above can preferably be reacted to the material of generation gas is distinguished
Sweating is carried out after emulsifying and mixing, short space is formed in wax layer using the gas of the aqueous solution and reaction generation, was being crystallized
Increase thermostatic process in journey, be advantageous to the discharge of sweating stage liquid component；And pass through wax layer using air-flow in sweating effort
Liquid composition is carried out to force to separate solids fraction and liquid composition, separating effect is enhanced and accelerates separating rate；From
And produce the basic material without low-melting component；Basic material is allocated on as with components such as silicone oil, native paraffin, solvents again
Light wax product.The inventive method has that investment of production equipment is low, production process is simple and operating cost is low, safety, energy-conservation and nothing
Solvent contamination, the advantages that glazing wax product resistance to elevated temperatures is good.
A kind of method for producing wax polish of the present invention, including herein below：
（A）Emulsification：Comprise the following steps：
（A1）It is prepared by oil phase material：Heated and melted as sweating raw material using F-T synthetic products；Oil soluble emulsifying agent is added, stirring is equal
It is even, form oil phase material；
（A2）It is prepared by water-phase material：By component（Ⅰ）And component（Ⅱ）Water is dissolved in respectively and is heated, and forms component（Ⅰ）Aqueous phase material
Material and component（Ⅱ）Water-phase material；
（A3）It is prepared by emulsion：By component（Ⅰ）Water-phase material and component（Ⅱ）Water-phase material respectively under agitation plus
Enter into oil phase material, continue stirring 5~60 minutes, to form component（Ⅰ）Emulsion and component（Ⅱ）Emulsion；
（B）Sweating：Comprise the following steps：
（B1）Preparation：Will（A3）Component prepared by process（Ⅰ）Emulsion and component（Ⅱ）Emulsion in pressure condition
It is lower well mixed, then mix emulsion fluid is loaded into sweatbox；
（B2）Crystallization：Mix emulsion fluid is first cooled to by sweating original with 1.0 DEG C/h~10.0 DEG C/h speed under stress
+ 4 DEG C of gob fusing point~+8 DEG C of melt drop temperature；Wax layer is cooled to by sweating raw material melt drop temperature with 1.0 DEG C/h~3.0 DEG C/h speed again
+ 4 DEG C of~melt drop temperature and constant temperature are for a period of time；Again with 2.0 DEG C/h~4.0 DEG C/h speed by wax layer be cooled to raw material melt drop temperature with
Lower 5 DEG C~30 DEG C of cooling final temperature；
（B3）Constant temperature：In crystallization final temperature constant temperature for a period of time, while pressure is reduced to normal pressure；
（B4）Sweating：Heated up with 0.5 DEG C/h~3.5 DEG C/h speed；Wax layer reaches predetermined temperature and constant temperature stops afterwards for a period of time
Only sweating；Wax layer is forced air flow through in sweating effort；
（B5）It is refined：After refined it is wax polish basic material on wax；
（C）Allotment：By basic material, melting mixing is uniform in proportion with silicone oil, native paraffin, solvent, is wax polish production after cooling
Product.
In the method for the present invention, described F-T synthetic products, its n-alkane weight content requirement is more than 80%, preferably
The F-T synthetic products that normal paraffin content is more than 90% are as sweating raw material.
The present invention method in, by sweating raw material in the presence of oil soluble emulsifying agent respectively with component（Ⅰ）The aqueous solution and
Component（Ⅱ）The aqueous solution emulsification be prepared into component（Ⅰ）Emulsion and component（Ⅱ）Emulsion, then carried out after mixing under stress
Sweating.Described oil soluble emulsifying agent is selected from nonionic surface active agent, anionic surfactant, cationic
One or more in activating agent, amphoteric surfactant.The HLB value of oil soluble emulsifying agent is in 1~10, preferably 3~8.
The freezing point or fusing point of the surfactant are less than step（B4）The maximum temperature of sweating（That is step（B4）Described in it is 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 present invention, described oil soluble emulsifying agent is preferably the compound emulsifying agent that two or more surface-actives are formed.
In the method for the present invention, step（A2）Described component（Ⅰ）And component（Ⅱ）Water is soluble in, and can interreaction
Generate one group of tie substance of gas.Such as, component（Ⅰ）At least one of water soluble acid, component can be selected from（Ⅱ）It can select
From at least one of carbonate, bicarbonate, sulphite, bisulfites, metal sulfide；Or component（Ⅰ）Also may be used
With selected from least one of inorganic base, component（Ⅱ）At least one of inorganic ammonium salt can be selected from；Or component（Ⅰ）Choosing
From hydrochloric acid, component（Ⅱ）Selected from least one of perchlorate, chlorate, hypochlorite；Or component（Ⅰ）It is also selected from salt
Acid, component（Ⅱ）Selected from urea.
Wherein, described water soluble acid includes inorganic acid and/or organic acid.Inorganic acid is selected from perchloric acid, hydroiodic acid, sulphur
One group of material that acid, hydrobromic acid, hydrochloric acid, nitric acid, acid iodide, sulfurous acid, phosphoric acid, nitrous acid, hydrofluoric acid are formed；Organic acid is selected from first
Sulfonic acid, benzene sulfonic acid, DBSA, trifluoromethanesulfonic acid, sulfamic acid, methyl-sulfinic acid, benzenesulfinic acid, thioacetic acid, first
Mercaptan, benzenethiol, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, positive enanthic acid, caprylic acid, oxalic acid, malonic acid, tartaric acid, amber
Amber acid, adipic acid, citric acid, acrylic acid, butenoic acid, oleic acid, fumaric acid, maleic acid, benzoic acid, phenylacetic acid, phthalic acid,
Terephthalic acid (TPA), salicylic acid, caffeic acid, glycolic, lactic acid, malic acid, chloroacetic acid, dichloroacetic acid, trichloroacetic acid, trifluoro second
One group of material that acid, perfluorobutyric acid, perfluoro caprylic acid are formed.
Described component（Ⅰ）And component（Ⅱ）Preferably cheap, wide material sources, itself and reaction product are nontoxic, nothing
The acid and carbonate of penetrating odor（Bicarbonate）.Such as component（Ⅰ）Preferably hydrochloric acid and/or sulfuric acid, component（Ⅱ）Preferably
At least one of sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus.In the present invention, component（Ⅰ）And component（Ⅱ）It is water-soluble
Component in liquid（Ⅰ）And component（Ⅱ）Mass concentration be 0.1%~10.0%, preferably 1.0%~5.0%.
In the method for the present invention, step（A3）The composition of resulting emulsion is：Sweating paraffin mass percent is
60.0%~90.0%, component（Ⅰ）And component（Ⅱ）The aqueous solution mass percent sum be 9.9%~30.0%, oil-soluble breast
The mass percent of agent is 0.1%~10.0%.Gained emulsion preferably constitute for：Sweating paraffin mass percent is
65.0%~84.0%, component（Ⅰ）And component（Ⅱ）The aqueous solution mass percent sum be 15.0%~30.0%, oil-soluble breast
The mass percent of agent is 1.0%~5.0%.
Step（A3）Described emulsification uses the routine operation of this area.As the condition emulsified is：75 DEG C~99
At DEG C, mixed 5~60 minutes with 50~5000 revs/min of mixing speed；Preferably at 85 DEG C~98 DEG C, with 100~
1000 revs/min of mixing speed mixes 10~30 minutes.Step（A1）And step（A2）In it is general respectively by oil phase material and
Water-phase material is heated to 90 DEG C~95 DEG C and 92 DEG C~99 DEG C.
In the method for the present invention, described sweatbox is generally sweating ware, and added above dismountable close in wax layer
Envelope system and pressue device, in step（B1）With（B2）During apply air pressure above wax layer to suppress in preparation
Wax layer is escaped with the gas that generation is reacted in crystallization process.Described pressure（Gauge pressure）For 5.0~50.0 atmospheric pressure, it is preferably
The air pressure of 20.0~35.0 atmospheric pressure.
In the method for the present invention, step（B2）During preferred hair is first cooled to 1.0 DEG C/h~10.0 DEG C/h speed
In the range of+8 DEG C of+4 DEG C~melt drop temperature of sweat raw material melt drop temperature；Thereafter in step（B2）Rate of temperature fall before constant temperature is preferably 1.5 DEG C/
H~2.5 DEG C/h；The time in constant temperature stage is preferably 1.0~4.0 hours；Rate of temperature fall after constant temperature be preferably 2.5 DEG C/h~
3.5℃/h；The final temperature that cools is preferably 8 DEG C~15 DEG C below sweating paraffin melt drop temperature.
In the method for the present invention, step（B3）The time of the constant temperature is 0.1~5.0 hour, preferably 0.5~3.0 hour；
Pressure is gradually reduced simultaneously to normal pressure.The speed that the pressure reduces is generally 0.1~150.0 atmospheric pressure/hour, is preferably
5.0~50.0 atmospheric pressure/hours.
In the method for the present invention, described sweating ware increases in wax layer pressue device added above and/or below wax layer
Vacuum plant, wax layer is set to form pressure differential up and down.Step（B4）The described wax layer that forces air flow through above wax layer using increasing
Plus-pressure（Air pressure）And/or pressure is reduced below wax layer（Air pressure）, make wax layer upper and lower（Side）Pressure differential is formed to realize.Institute
The pressure differential stated 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（B4）The heating rate preferably 1.0 DEG C/h~3.0 DEG C/h.The heating it is pre-
Constant temperature degree（That is final temperature）Based on -10 DEG C of material melt drop temperature~basic material melt drop temperature.Described is warming up to predetermined temperature
Afterwards, the increase constant temperature stage can be such that solids fraction is separated with liquid composition more fully, and the time in constant temperature stage is small for 0.1~10.0
When, preferably 1.0~8.0 hours, most preferably 2.0~6.0 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（B4）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（B4）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（B4）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~-1.0 atmospheric pressure is maintained below wax layer.
In the method for the present invention, process（C）Described in silicone oil can be methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, methyl
Containing hydrogen silicone oil, methyl phenyl silicone oil, methylchlorophenyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl Silicon Containing Hydrogen
Oil, one kind in amido silicon oil or its mixture.The native paraffin can be beeswax, Chinese wax, Ka Naba waxes, candelila wax,
One kind or its mixture in lignite wax, rice bran wax.The solvent can be pentane, n-hexane, normal octane, D40, D60,
D80, No. 90, No. 120, No. 180, No. 190, No. 200, ExxsolD40, ExxsolD80, ExxsolD110, ExxsolD130,
ExxsolDSP80/100, benzene,toluene,xylene, hexamethylene, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichloro-benzenes, dichloromethane,
Ether, oxirane, methyl acetate, ethyl acetate, propyl acetate, dimethyl succinate, dimethyl glutarate, adipic acid diformazan
Ester, acetone, espeleton, methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol ethyl ether
One kind or its mixture in acetate, glycol ether ester, phenol, turpentine oil, tasteless kerosene.The solvent is preferably nontoxic,
Low smell, volatility are appropriate, price is low, source is wide D40, D60, D80, No. 90, No. 120, No. 180, No. 190, No. 200,
ExxsolD40, ExxsolD80, ExxsolD110, ExxsolD130, ExxsolDSP80/100, propyl acetate, succinic acid diformazan
One kind or its mixture in ester, dimethyl glutarate.
In the method for the present invention, step in mass（C3）Described in the composition of wax polish be：Basic material 5.0%~
29.0%th, silicone oil 0.1%~6.0%, native paraffin 1.0%~15.0%, solvent 50.0%~93.9%；Preferably composition is：Basic material
10.0%~25.0%, silicone oil 1.0%~5.0%, native paraffin 4.0%~10.0%, solvent 60.0%~85.0%.
Wherein, step（C3）Described in wax polish can also add one or more of antioxidant, essence as needed
As additive.Using the addition of additive described in glazing wax gauge as：Antioxidant 0.1~1.0%, preferably 0.1~0.5%；
Essence 0.1~1.0%, preferably 0.2~0.5%.
Described antioxidant can be antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant
1330th, antioxidant 3114, antioxidant 164, irgasfos 168, antioxidant 264, antioxidant B215, one kind in antioxidant B225 or
Its mixture.
Analysis shows, the not impurity such as sulfur-bearing, nitrogen, aromatic hydrocarbons in F-T synthetic products, easily reach very high pure by refined
Degree；In the chemical composition of low temperature F-T synthetic products based on n-alkane and distribution is very wide, and contain a small amount of alkene and oxygen-containing
Compound.Bad stability under high temperature can be made due to olefin component be present, oxygenatedchemicals has special smell.A large amount of eutectics
Point component makes it resistance to elevated temperatures can be caused to be deteriorated when being directly used as wax polish component.Therefore F-T synthetic products are not suitable for directly
With the allotment component of wax polish.
Sweating separation method is separated using the different property of various component fusing points.For the research of sweating effort
Show, liquid composition is gradually discharged along crystalline portion in sweating effort, the feelings flowed similar to liquid in capillary
Condition.But for high melting-point wax of the fusing point at 70 DEG C or so, 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 70 DEG C with
On wax product.
The present invention passes through going deep into for the composition to F-T synthetic products to produce the high temperature resistant glazing wax product of low cost
Research, contains a certain amount of alkene and oxygenatedchemicals for F-T synthetic products（The fusing point of these components is usually less than 65 DEG C,
Belong to low-melting component）, the low-melting component also containing a large amount of alkanes is to cause F-T synthetic products to be not suitable for being directly used in allotment
The reason for glazing wax product, these non-Suitable ingredients are removed by using sweating method, then with silicone oil, native paraffin, oil miscible solvent
Glazing wax product is produced in symphysis.
By the further investigation to common sweating effort, the reason for being difficult to separate with liquid composition for solids fraction,
Used in sweating effort and force air flow through wax layer, while sweating paraffin and two kinds can further preferably be reacted to the group of generation gas
Sweating is carried out after dividing emulsification and effectively removes sweating raw material with increase constant temperature stage, these measures in sweating effort crystallizing
The non-Suitable ingredients such as middle alkene, oxygenatedchemicals and low melting point alkane, make product be suitable for use as the basic material of wax polish.
The reason for being difficult to separate with liquid composition for solids fraction in sweating effort, by using gas in sweating effort
Stream carries out method pressure solids fraction and the separation of liquid composition of liquid composition by wax layer, enhances separating effect and adds
Fast separating rate；Simultaneously further preferably by sweating paraffin and two kinds can react generate gas component emulsify respectively after form W/
O-shaped emulsion, then carry out sweating after mixing under stress.The aqueous solution in mix emulsion fluid is uniform in the form of fine particle
It is distributed in raw material wax layer；Due to being w/o type emulsion, reactive two kinds of components are because the buffer action of oil film is without reacting
Or with slower speed responsing；Emulsion is cooled to below fusing point 5 DEG C~30 DEG C under stress, in step（B1）With
（B2）During apply pressure more than wax layer, can suppress preparation and crystallization etc. during react generation gas ease
Go out wax layer.Increasing the high temperature constant temperature stage in temperature-fall period can make the crystallization of wax bigger, be advantageous to liquid group in sweating effort
The discharge divided.Research for wax crystallization process shows that the chemical composition of wax is to determine the main factor of crystal habit, simultaneously
The condition of cooling procedure can also influence crystal habit, and especially the cooling condition at the temperature near melt drop temperature is to crystal habit
Influence it is most obvious.When being cooled near melt drop temperature, the n-alkane of larger molecular weight has formed crystallization and separated out wax, this part
Crystalline solid can now increase the high temperature constant temperature stage, nucleus can be enable fully to increase as the nucleus for being subsequently formed crystallization,
Larger sized crystal is formed, it is this although this larger sized crystal is thick not as the crystallization of low melt point paraffin
It is also highly beneficial that the crystal structure of increase discharges liquid composition to the sweating stage.After sweating raw material is cooled to below melt drop temperature
Wax layer is in softer solid state in the time terminated to sweating effort, and two kinds of reactive components gradually occur during this
Chemically react and discharge gas, equally distributed micro-bubble is formed in raw material wax layer；Air-flow is utilized in sweating effort
By wax layer, on the one hand can carry out can reactive material the aqueous solution to form short space in wax layer, these short spaces
With bubble caused by short space be easy to form some tiny passages in wax layer in sweating effort, be advantageous to sweating effort
The discharge of middle liquid composition；Another aspect air-flow can carry out liquid composition to force to separate solids fraction and liquid composition, from
And enhance separating effect and accelerate separating rate.Selected surfactant fusing point or freezing point are less than the highest of sweating effort
Temperature, and contain functional group, it is poor with the intermiscibility of sweating raw material, it can be discharged in sweating effort with liquid composition.Again
Being aided with the constant temperature stage after crystallization makes solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction and liquid group
The methods of separation is more abundant so that sweating process can produce the wax polish basic material for not containing low-melting component.
Melting mixing is uniform in proportion with silicone oil, native paraffin, solvent for basic material, is glazing wax product after cooling.
It is an advantage of the invention that：By using the side for forcing air flow through wax layer and carrying out liquid composition in sweating effort
Method enhances the separating effect of solids fraction and liquid composition and accelerates separating rate；Increase the constant temperature stage of crystallization process,
And using can reactive material produce micro-bubble formed short space and the aqueous solution discharge after produce short space in sweating
Some thin channels are formed in journey, are also beneficial to the quick discharge of liquid composition；Simultaneously increase crystallization after the constant temperature stage and
The processes such as the constant temperature stage of sweating effort, so that sweating process can produce the wax polish basis without low-melting component
Material；Melting mixing is uniformly wax polish to basic material in proportion with silicone oil, native paraffin, solvent and antioxidant, essence again
Product.The method of the present invention has that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free dirt
Contaminate environment, the advantages that glazing wax product resistance to elevated temperatures is good.
Embodiment
The present invention is by being raw material from suitable low temperature F-T synthetic products, 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；Sweating raw material heating fusing and the group that generation gas can be reacted with two kinds preferably under the conditions of emulsifying agent
Point the aqueous solution emulsify respectively again under stress be well mixed after load sweating ware；With oil bath control wax layer heating-cooling speed
Degree；Increase the constant temperature stage in crystallization process；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 perseverance
Stop sweating effort after warm a period of time；On wax after refined wax polish basic material；Basic material again with silicone oil, natural
It is glazing wax product after other component melts mixing such as wax, solvent.The method of the present invention has that plant investment is low, production process
Simple and operating cost is low, safety, energy-conservation and solvent-free pollution environment, the advantages that glazing wax product resistance to elevated temperatures is good.
The method that 1-4 illustrates the production wax polish of the present invention by the following examples.As without especially dated, following institute
The % being related to is mass percent, and the pressure is gauge pressure.
Embodiment 1
The present embodiment includes：（A）Emulsification,（B）Sweating,（C）Allocate three parts.
（A）Emulsification：Including（A1）Oil phase material preparation,（A2）Water-phase material preparation,（A3）Emulsion prepares three steps.
（A1）It is prepared by oil phase material：
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（Normal paraffin content is
95.50wt%；86.2 DEG C of melt drop temperature；Needle penetration（25℃）55（10-1mm）；Needle penetration（65℃）＞ 200（10-1mm））68.0Kg,
2.5Kg diethylene glycols fatty acid ester, 0.7Kg tetraethylene glycols monostearate and 0.4Kg 12 are added after being heated to 95 DEG C of fusings
Alkyl betaine, two parts are divided into after stirring.
It can be seen that from the needle penetration of 25 DEG C and 65 DEG C and contain a large amount of low melting points in the wax oil product.
（A2）It is prepared by water-phase material
Component（Ⅰ）It is prepared by water-phase material：Compound concentration is 0.8% HCl solution, takes 13.2Kg and is heated to 98 DEG C；
Component（Ⅱ）It is prepared by water-phase material：Compound concentration is 1.2% Na2CO3Solution, take 13.2Kg and be heated to 98 DEG C.
（A3）It is prepared by emulsion
Component（Ⅰ）It is prepared by emulsion：Portion in foregoing oil phase material is stirred with 450 r/min speed, and by component（Ⅰ）
Water-phase material is slowly added into oil phase material, is continued to stir 25min, is formed the component of water-in-oil type（Ⅰ）Emulsion.
Component（Ⅱ）It is prepared by emulsion：Another in foregoing oil phase material is stirred with 900r/min speed, and by group
Point（Ⅱ）Water-phase material is slowly added into oil phase material, is continued to stir 10min, is formed the component of water-in-oil type（Ⅱ）Emulsification
Liquid.
（B）Sweating：Including（B1）Preparation,（B2）Cooling-high temperature constant temperature-decrease temperature crystalline,（B3）Cryogenic thermostat,
（B4）Heating-constant temperature sweating,（B5）Refine five steps.
（B1）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, conduction oil is warming up to 91 DEG C.Pad water below sweating ware ware plate.Peace
The sealing system on dress sweating ware top is simultaneously forced into 21.2~21.4 atmospheric pressure；Will under 21.2~21.4 atmospheric pressure（A3）
The component of middle preparation（Ⅰ）Emulsion and component（Ⅱ）Emulsion it is well mixed after add sweating ware.
（B2）Cooling-high temperature constant temperature-decrease temperature crystalline
Under 21.2~21.4 atmospheric pressure, emulsion stands 1.0h.Start the refrigerating function of the circulatory system, start the circulatory system
Refrigerating function, wax layer temperature is dropped to 88.5 DEG C and constant temperature 3.0h with 2.0 DEG C/h rate of temperature fall and carry out high temperature constant temperatures, with
Crystal is set fully to increase；Again with 3.0 DEG C/h rate of temperature fall make wax layer temperature drop to 76.0 DEG C so that wax layer crystallize to be formed it is solid
Body.
（B3）Cryogenic thermostat
In 76.0 DEG C of constant temperature 1.0h so that wax layer crystallization it is more abundant, while by emptying system control pressurized buffer pressure inside the tank with
35 atmospheric pressure/h speed is gradually decrease to normal pressure.Close the refrigerating function of the circulatory system.
（B4）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 1.4~1.6 atmospheric pressure, sweating ware ware plate of pressure inside the tank；Start circulation system function,
Wax layer temperature is set to be increased to 86.0 DEG C with 3.0 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 90.0 DEG C of simultaneously constant temperature 5.0 hours with 1.0 DEG C/h heating rate, so that in wax layer
Solids fraction is sufficiently separated with liquid composition；Stop vavuum pump, terminate sweating effort.
Sweating ware exports changing-over crude product storage tank（Ⅰ）To receive on wax；Continue the temperature of rise conduction oil to 110 DEG C, with
Fusing is taken out on wax, as crude product（Ⅰ）.
（B5）It is refined
Crude product（Ⅰ）It is basic material after clay-filtered（Ⅰ）.
Basic material（Ⅰ）Property：95.8 DEG C of melt drop temperature；Needle penetration（25℃）2 （10-1mm）；Needle penetration（65℃）42（10-1mm）.Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material（Ⅰ）Yield is 34.6%（Phase
Wax oil is synthesized for sweating raw material F-T）.
The oxygenatedchemicals such as alkene and alcohol, acid is not detected from chromatogram-mass spectral analysis can be seen that these materials in raw material
Remove；It can be seen that low melting point has removed substantially in sweating product from 25 DEG C and 65 DEG C of needle penetrations.
（C）Allotment
（C1）Weigh basic material（Ⅰ）2.5Kg, Ka Naba wax（3#, Brazil）1.0Kg, stirred after being heated to 110 DEG C of meltings to equal
It is even；
（C2）Weigh D80（Qingjian River petrochemical industry Co., Ltd）3.0 Kg, No. 120 solvent naphthas（Qingjian River petrochemical industry is limited
Responsible company）3.1 Kg, silicone oil（300, Beijing boat apple silicon wound chemical industry）0.3 Kg, alkyl-silicone oil（Silok -2300, this Lip river, Guangzhou
Ke Huaxue）0.1Kg, it is heated to 35 DEG C and stirs；
（C3）Will（C2）Component is prepared to add（C1）Component is prepared, stirs and loads container after being cooled to 70 DEG C, be cooled to
Normal temperature is glazing wax product（Ⅰ）.
Glazing wax product（Ⅰ）Property：High-temperature stability：It is qualified；Low-temperature stability：It is qualified；Glossiness value added：14.Symbol
Close the requirement of GB/T 23437-2009 standards.
Embodiment 2
The present embodiment includes：（A）Emulsification,（B）Sweating,（C）Allocate three parts.
（A）Emulsification：Including（A1）Oil phase material preparation,（A2）Water-phase material preparation,（A3）Emulsion prepares three steps.
（A1）It is prepared by oil phase material：
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（With embodiment 1）80.0Kg,
1.7Kg sorbitan monostearates, 0.6Kg tetraethylene glycols monostearate and 0.3Kg are added after being heated to 92 DEG C of fusings
Sodium alkyl benzene sulfonate, two parts are divided into after stirring.
（A2）It is prepared by water-phase material
Component（Ⅰ）It is prepared by water-phase material：Compound concentration is 1.9% H2SO4Solution, take 8.7Kg and be heated to 95 DEG C；
Component（Ⅱ）It is prepared by water-phase material：Compound concentration is 2.8% NaHCO3Solution, take 8.7Kg and be heated to 95 DEG C.
（A3）It is prepared by emulsion
Component（Ⅰ）It is prepared by emulsion：Portion in foregoing oil phase material is stirred with 500 r/min speed, and by component（Ⅰ）
Water-phase material is slowly added into oil phase material, is continued to stir 20min, is formed the component of water-in-oil type（Ⅰ）Emulsion.
Component（Ⅱ）It is prepared by emulsion：Another in foregoing oil phase material is stirred with 750r/min speed, and by group
Point（Ⅱ）Water-phase material is slowly added into oil phase material, is continued to stir 15min, is formed the component of water-in-oil type（Ⅱ）Emulsification
Liquid.
（B）Sweating：Including（B1）Preparation,（B2）Cooling-high temperature constant temperature-decrease temperature crystalline,（B3）Cryogenic thermostat,
（B4）Heating-constant temperature sweating,（B5）Refine five steps.
（B1）Preparation and（B2）Pressure is 29.3~29.5 atmospheric pressure in crystallization process, and remaining is the same as embodiment 1.
The basic material of the present embodiment production（Ⅱ）Property：96.3 DEG C of melt drop temperature；Needle penetration（25℃）2 （10-1mm）；Pin
In-degree（65℃）39（10-1mm）.Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material（Ⅱ）
Yield is 35.4%（Wax oil is synthesized relative to sweating raw material F-T）.
The oxygenatedchemicals such as alkene and alcohol, acid is not detected from chromatogram-mass spectral analysis can be seen that these materials in raw material
Remove；It can be seen that low melting point has removed substantially in sweating product from 25 DEG C and 65 DEG C of needle penetrations.
（C）Allotment
（C1）Weigh basic material（Ⅱ）2.2Kg, Chinese wax（Hebei Dongsheng beeswax factory）0.8Kg, stirred after being heated to 110 DEG C of meltings
Mix to uniform；
（C2）Weigh D60（Qingjian River petrochemical industry Co., Ltd）3.4Kg, No. 200 solvent naphthas（Sinopec Nanjing branch company）
3.3Kg, silicone oil（300, Beijing boat apple silicon wound chemical industry）0.2Kg, silicone oil（3000, Beijing boat apple silicon wound chemical industry）0.1Kg, it is heated to
35 DEG C and stir；
（C3）Will（C2）Component is prepared to add（C1）Component is prepared, stirs and loads container after being cooled to 70 DEG C, be cooled to
Normal temperature is glazing wax product（Ⅱ）.
Glazing wax product（Ⅱ）Property：High-temperature stability：It is qualified；Low-temperature stability：It is qualified；Glossiness value added：12.Symbol
Close the requirement of GB/T 23437-2009 standards.
Embodiment 3
The present embodiment includes：（A）Emulsification,（B）Sweating,（C）Allocate three parts.
（A）Emulsification：Including（A1）Oil phase material preparation,（A2）Water-phase material preparation,（A3）Emulsion prepares three steps.
（A1）It is prepared by oil phase material：
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（With embodiment 1）83.0Kg,
Addition 1.4Kg diethylene glycols monolaurate, 0.4Kg sorbitan monooleates and 0.2Kg gather after being heated to 95 DEG C of fusings
Oxypropylene stearate, two parts are divided into after stirring.
（A2）It is prepared by water-phase material
Component（Ⅰ）It is prepared by water-phase material：Compound concentration is 1.9% H2SO4Solution, take 7.5Kg and be heated to 98 DEG C；
Component（Ⅱ）It is prepared by water-phase material：Compound concentration is 4.2% KHCO 3Solution, take 7.5Kg and be heated to 98 DEG C.
（A3）It is prepared by emulsion
Component（Ⅰ）It is prepared by emulsion：Portion in foregoing oil phase material is stirred with 500 r/min speed, and by component（Ⅰ）
Water-phase material is slowly added into oil phase material, is continued to stir 25min, is formed the component of water-in-oil type（Ⅰ）Emulsion.
Component（Ⅱ）It is prepared by emulsion：Another in foregoing oil phase material is stirred with 1000r/min speed, and by group
Point（Ⅱ）Water-phase material is slowly added into oil phase material, is continued to stir 10min, is formed the component of water-in-oil type（Ⅱ）Emulsification
Liquid.
（B）Sweating：Including（B1）Preparation,（B2）Cooling-high temperature constant temperature-decrease temperature crystalline,（B3）Cryogenic thermostat,
（B4）Heating-constant temperature sweating,（B5）Refine five steps.
（B1）Preparation and（B2）Pressure is 34.0~34.2 atmospheric pressure in crystallization process, and remaining is the same as embodiment 1.
The basic material of the present embodiment production（Ⅲ）Property：95.5 DEG C of melt drop temperature；Needle penetration（25℃）2 （10-1mm）；Pin
In-degree（65℃）38（10-1mm）.Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material（Ⅲ）
Yield is 38.8%（Wax oil is synthesized relative to sweating raw material F-T）.
The oxygenatedchemicals such as alkene and alcohol, acid is not detected from chromatogram-mass spectral analysis can be seen that these materials in raw material
Remove；It can be seen that low melting point has removed substantially in sweating product from 25 DEG C and 65 DEG C of needle penetrations.
（C）Allotment
（C1）Weigh basic material（Ⅲ）2.2Kg, beeswax（Hebei Dongsheng beeswax factory）0.8Kg, stirred after being heated to 110 DEG C of meltings
To uniform；
（C2）Weigh ExxsolD80（Exxon Mobil）3.4Kg、ExxsolD130（Exxon Mobil）3.3Kg, silicone oil（300,
Beijing boat apple silicon wound chemical industry）0.2Kg, phenyl silicone oil（RB-1558, Guangzhou thunder nation chemical industry）0.1Kg, it is heated to 35 DEG C and stirs equal
It is even；
（C3）Will（C2）Component is prepared to add（C1）Component is prepared, stirs and loads container after being cooled to 70 DEG C, be cooled to
Normal temperature is glazing wax product（Ⅲ）.
Glazing wax product（Ⅲ）Property：High-temperature stability：It is qualified；Low-temperature stability：It is qualified；Glossiness value added：15.Symbol
Close the requirement of GB/T 23437-2009 standards.
Embodiment 4
The present embodiment includes：（A）Emulsification,（B）Sweating,（C）Allocate three parts.
（A）Emulsification：Including（A1）Oil phase material preparation,（A2）Water-phase material preparation,（A3）Emulsion prepares three steps.
（A1）It is prepared by oil phase material：
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（With embodiment 1）73.0Kg,
1.9Kg sorbitan monostearates, 0.7Kg diethylene glycols monolaurate and 0.4Kg are added after being heated to 92 DEG C of fusings
Triacetamide oleate, two parts are divided into after stirring.
（A2）It is prepared by water-phase material
Component（Ⅰ）It is prepared by water-phase material：Compound concentration is 1.3% H2SO4Solution, take 12.0Kg and be heated to 95 DEG C；
Component（Ⅱ）It is prepared by water-phase material：Compound concentration is 1.9% K2CO3Solution, take 12.0Kg and be heated to 95 DEG C.
（A3）It is prepared by emulsion
Component（Ⅰ）It is prepared by emulsion：Portion in foregoing oil phase material is stirred with 300r/min speed, and by component（Ⅰ）Water
Phase material is slowly added into oil phase material, is continued to stir 30min, is formed the component of water-in-oil type（Ⅰ）Emulsion.
Component（Ⅱ）It is prepared by emulsion：Another in foregoing oil phase material is stirred with 800r/min speed, and by group
Point（Ⅱ）Water-phase material is slowly added into oil phase material, is continued to stir 15min, is formed the component of water-in-oil type（Ⅱ）Emulsification
Liquid.
（B）Sweating：Including（B1）Preparation,（B2）Cooling-high temperature constant temperature-decrease temperature crystalline,（B3）Cryogenic thermostat,
（B4）Heating-constant temperature sweating,（B5）Refine five steps.
（B1）Preparation and（B2）Pressure is 25.4~25.6 atmospheric pressure in crystallization process, and remaining is the same as embodiment 1.
The basic material of the present embodiment production（Ⅳ）Property：96.1 DEG C of melt drop temperature；Needle penetration（25℃）2 （10-1mm）；Pin
In-degree（65℃）44（10-1mm）.Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material（Ⅳ）
Yield is 36.1%（Wax oil is synthesized relative to sweating raw material F-T）.
The oxygenatedchemicals such as alkene and alcohol, acid is not detected from chromatogram-mass spectral analysis can be seen that these materials in raw material
Remove；It can be seen that low melting point has removed substantially in sweating product from 25 DEG C and 65 DEG C of needle penetrations.
（C）Allotment
（C1）Weigh basic material（Ⅳ）1.6Kg, Ka Naba wax（1#, Brazil's production）0.5Kg, antioxidant 1010（BASF）0.04
Kg, it is stirred until homogeneous after being heated to 110 DEG C of meltings；
（C2）Weigh No. D60（Panjin great achievement petro-chemical corporation）3.80Kg, No. 200（Sinopec Nanjing branch company）3.72Kg, silicone oil
（300, Beijing boat apple silicon wound chemical industry）0.2Kg, phenyl silicone oil（Silok -2540, Guangzhou Si Luoke chemistry）0.1Kg, it is heated to
35 DEG C and stir；
（C3）Will（C2）Component is prepared to add（C1）Component is prepared, is stirring evenly and then adding into essence（Vanilla flavored, Shenyang standing grain field spices
Co., Ltd）0.04 Kg simultaneously loads container after being cooled to 70 DEG C, and it is glazing wax product to be cooled to normal temperature（Ⅳ）.
Glazing wax product（Ⅳ）Property：High-temperature stability：It is qualified；Low-temperature stability：It is qualified；Glossiness value added：15.Symbol
Close the requirement of GB/T 23437-2009 standards.
The method that present invention production wax polish is can be seen that by embodiment 1-4, set by increasing pressurization and/or vacuum
The improvement to sweatbox such as apply；By the way that sweating raw material and reactive two kinds of components are emulsified respectively, given birth to using reaction
Into gas formed in wax layer micro-bubble and the aqueous solution discharge after formed short space, air-flow is forced in sweating effort
The improvement to sweating process such as constant temperature stage by wax layer, increase crystallization and sweating effort；Enhance solids fraction and liquid
The separating effect of component simultaneously accelerates separating rate, so as to effectively eliminate lower-molecular-weight component in raw material, so that sweating work
Skill can produce the basic material without low-melting component.Basic material melts with other components such as silicone oil, native paraffin, solvent again
Melt after mixing is glazing wax product.The present invention method have plant investment is low, production process is simple and operating cost is low, peace
Entirely, energy-conservation and solvent-free pollution environment, the advantages that glazing wax product resistance to elevated temperatures is good.
Claims (30)
1. a kind of method for producing wax polish, including herein below：
（A）Emulsification：Comprise the following steps：
（A1）It is prepared by oil phase material：Using F-T synthetic products as sweating raw material, heating fusing；Oil soluble emulsifying agent is added, stirring is equal
It is even, form light wood material phase；
（A2）It is prepared by water-phase material：By component（Ⅰ）And component（Ⅱ）Water is dissolved in respectively and is heated, and forms component（Ⅰ）Aqueous phase material
Material and component（Ⅱ）Water-phase material；
（A3）It is prepared by emulsion：By component（Ⅰ）Water-phase material and component（Ⅱ）Water-phase material respectively under agitation plus
Enter into oil phase material, continue stirring 5~60 minutes, to form component（Ⅰ）Emulsion and component（Ⅱ）Emulsion；
（B）Sweating：Comprise the following steps：
（B1）Preparation：Will（A3）Component prepared by process（Ⅰ）Emulsion and component（Ⅱ）Emulsion in pressure condition
It is lower well mixed, then mix emulsion fluid is loaded into sweatbox；
（B2）Crystallization：Mix emulsion fluid is first cooled to by sweating original with 1.0 DEG C/h~10.0 DEG C/h speed under stress
+ 4 DEG C of gob fusing point~+8 DEG C of melt drop temperature；Wax layer is cooled to by sweating raw material melt drop temperature with 1.0 DEG C/h~3.0 DEG C/h speed again
+ 4 DEG C of~melt drop temperature and constant temperature are for a period of time；Wax layer is cooled to by sweating raw material drip melt with 2.0 DEG C/h~4.0 DEG C/h speed again
Following 5 DEG C~30 DEG C cooling final temperature of point；
（B3）Constant temperature：In crystallization final temperature constant temperature for a period of time, while pressure is reduced to normal pressure；
（B4）Sweating：Heated up with 0.5 DEG C/h~3.5 DEG C/h speed；Wax layer reaches predetermined temperature and constant temperature stops afterwards for a period of time
Only sweating；Wax layer is forced air flow through in sweating effort；
（B5）It is refined：After refined it is wax polish basic material on wax；
（C）Allotment：By basic material, proportionally melting mixing is uniform with silicone oil, native paraffin, solvent, is wax polish after cooling
Product.
2. in accordance with the method for claim 1, it is characterised in that described oil soluble emulsifying agent is lived selected from non-ionic surface
Property agent, anionic surfactant, cationic surface active agent, amphoteric surfactant form one group of material；Oil
The HLB value of soluble emulsification agent is 1~10, and the freezing point or fusing point of surfactant are less than step（B4）The maximum temperature of sweating.
3. in accordance with the method for claim 2, it is characterised in that described nonionic surface active agent is selected from Sorbitan
Alcohol monoleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, Sorbitan
Alcohol monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, polyoxy second
One group of material that alkene fatty acid ester is formed；Described anionic surfactant be selected from fatty alcohol sulfate monoethanolamine salt,
Pareth sulfate, oleamide yl carboxylic acid sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurates, dibutyl naphthalene
Sodium sulfonate, Disodium sulfosuccinate, the one group of material formed along succinate monoester sodium sulfonate；Described cationic surfactant
Agent is selected from benzyl quaternary ammonium salt, dodecyl benzyl dimethyl ammonium chloride, DTAC, cetyl trimethyl
One group of material that ammonium bromide, OTAC, triacetamide oleate are formed；Described amphoteric surfactants
Agent is selected from empgen BB, OA-12, aliphatic group imidazolidine derivatives, alkyl imidazoline and derived
One group of material that thing, derivative of fatty acid, amphoteric modified epoxy ethane additive product are formed.
4. in accordance with the method for claim 2, it is characterised in that described oil soluble emulsifying agent is two or more surface-actives
The compound emulsifying agent that agent is formed.
5. in accordance with the method for claim 1, it is characterised in that described component（Ⅰ）And component（Ⅱ）Water is soluble in, and
One group of tie substance of energy interreaction generation gas.
6. in accordance with the method for claim 5, it is characterised in that described component（Ⅰ）At least one in water soluble acid
Kind, component（Ⅱ）Selected from least one of carbonate, bicarbonate, sulphite, bisulfites, metal sulfide；Or
Person, component（Ⅰ）Selected from least one of inorganic base, component（Ⅱ）Selected from least one of inorganic ammonium salt；Or component
（Ⅰ）Selected from hydrochloric acid, component（Ⅱ）Selected from least one of perchlorate, chlorate, hypochlorite；Or component（Ⅰ）It is selected from
Hydrochloric acid, component（Ⅱ）Selected from urea.
7. in accordance with the method for claim 6, it is characterised in that described water soluble acid includes inorganic acid and/or organic acid.
8. in accordance with the method for claim 7, it is characterised in that described inorganic acid be selected from perchloric acid, hydroiodic acid, sulfuric acid,
One group of material that hydrobromic acid, hydrochloric acid, nitric acid, acid iodide, sulfurous acid, phosphoric acid, nitrous acid, hydrofluoric acid are formed；Described organic acid choosing
From methanesulfonic acid, benzene sulfonic acid, DBSA, trifluoromethanesulfonic acid, sulfamic acid, methyl-sulfinic acid, benzenesulfinic acid, thio second
Acid, methyl mercaptan, benzenethiol, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, positive enanthic acid, caprylic acid, oxalic acid, malonic acid, winestone
Acid, butanedioic acid, adipic acid, citric acid, acrylic acid, butenoic acid, oleic acid, fumaric acid, maleic acid, benzoic acid, phenylacetic acid, adjacent benzene two
Formic acid, terephthalic acid (TPA), salicylic acid, caffeic acid, glycolic, lactic acid, malic acid, chloroacetic acid, dichloroacetic acid, trichloroacetic acid,
One group of material that trifluoroacetic acid, perfluorobutyric acid, perfluoro caprylic acid are formed.
9. in accordance with the method for claim 8, it is characterised in that described component（Ⅰ）For at least one in hydrochloric acid, sulfuric acid
Kind, component（Ⅱ）Selected from least one of sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus.
10. in accordance with the method for claim 1, it is characterised in that described component（Ⅰ）And component（Ⅱ）The aqueous solution in group
Point（Ⅰ）And component（Ⅱ）Mass concentration be 0.1%~10.0%, preferably 1.0%~5.0%.
11. in accordance with the method for claim 1, it is characterised in that step（A3）Described in mixing speed be 50~5000
Rev/min, the temperature for preparing emulsion is 75 DEG C~99 DEG C.
12. in accordance with the method for claim 1, it is characterised in that step（B1）The composition of obtained mix emulsion fluid is：Hair
Sweat paraffin mass percent is 60.0%~90.0%, component（Ⅰ）The aqueous solution and component（Ⅱ）The aqueous solution quality percentage
Number sum is 9.9%~30.0%, and the mass percent of oil soluble emulsifying agent is 0.1%~10.0%.
13. in accordance with the method for claim 12, it is characterised in that step（B1）The composition of obtained mix emulsion fluid is：
Sweating paraffin mass percent is 65.0%~84.0%, component（Ⅰ）The aqueous solution and component（Ⅱ）The aqueous solution quality hundred
Fraction sum is 15.0%~30.0%, and the mass percent of oil soluble emulsifying agent is 1.0%~5.0%.
14. in accordance with the method for claim 1, it is characterised in that step（B1）With（B2）During apply above wax layer
Gauge is the air pressure of 5.0~50.0 atmospheric pressure, and the air pressure of preferably 20.0~35.0 atmospheric pressure is to suppress preparing
The gas effusion wax layer of generation is reacted in work and crystallization process.
15. in accordance with the method for claim 1, it is characterised in that step（B2）Described in constant temperature zone time for 0.1~
6.0 hour.
16. in accordance with the method for claim 1, it is characterised in that step（B2）Described in the predetermined temperature that cools be sweating
8 DEG C~20 DEG C below paraffin melt drop temperature.
17. in accordance with the method for claim 1, it is characterised in that step（B3）Described in constant temperature time be 0.1~5.0
Hour.
18. in accordance with the method for claim 17, it is characterised in that pressure is gradually reduced while constant temperature to normal pressure, drop
Pressure speed is 0.1~150.0 atmospheric pressure/hour.
19. in accordance with the method for claim 1, it is characterised in that step（B4）Described in based on the predetermined temperature that heats up
- 10 DEG C of material melt drop temperature~basic material melt drop temperature.
20. in accordance with the method for claim 1, it is characterised in that step（B4）Described in constant temperature time be 0.1~10.0
Hour.
21. in accordance with the method for claim 1, it is characterised in that step（B4）Described in force air flow through wax layer and sending out
Sweat is implemented initial stage.
22. in accordance with the method for claim 1, it is characterised in that step（B4）Described in the wax layer that forces air flow through adopt
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, it is described
Pressure differential is 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure.
23. in accordance with the method for claim 22, 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.
24. in accordance with the method for claim 22, 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~-1.0 atmospheric pressure is maintained below wax layer
Pressure pressure.
25. according to the method described in claim 1, it is characterised in that the weight of the n-alkane in described F-T synthetic products
It is more than 80% to measure content.
26. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
27. in accordance with the method for claim 1, it is characterised in that the composition of wax polish is in mass：Basic material 5.0%
~29.0%, silicone oil 0.1%~6.0%, native paraffin 1.0%~15.0%, solvent 50.0%~93.9%.
28. in accordance with the method for claim 27, it is characterised in that be additionally added in described wax polish in antioxidant, essence
More than one as additive；Using the addition of additive described in glazing wax gauge as：Antioxidant 0.1~1.0%, essence
0.1~1.0%.
29. according to the method described in claim 1,27 or 28, it is characterised in that described silicone oil is selected from methyl-silicone oil, ethyl
Silicone oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, methyl vinyl silicon oil, methyl hydroxyl
At least one of base silicone oil, ethyl containing hydrogen silicone oil, amido silicon oil；The native paraffin be selected from beeswax, Chinese wax, Ka Naba waxes,
At least one of candelila wax, lignite wax, rice bran wax；The solvent be selected from pentane, n-hexane, normal octane, D40, D60,
D80, No. 90, No. 120, No. 180, No. 190, No. 200, ExxsolD40, ExxsolD80, ExxsolD110, ExxsolD130,
ExxsolDSP80/100, benzene,toluene,xylene, hexamethylene, cyclohexanone, toluene cyclohexanone, chlorobenzene, dichloro-benzenes, dichloromethane,
Ether, oxirane, methyl acetate, ethyl acetate, propyl acetate, dimethyl succinate, dimethyl glutarate, adipic acid diformazan
Ester, acetone, espeleton, methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol ethyl ether
At least one of acetate, glycol ether ester, phenol, turpentine oil, tasteless kerosene.
30. in accordance with the method for claim 28, it is characterised in that described antioxidant is selected from antioxidant BHT, antioxidant
1010th, antioxidant 1076, antioxidant CA, antioxidant 1330, antioxidant 3114, antioxidant 164, irgasfos 168, antioxidant 264,
At least one of antioxidant B215, antioxidant B225.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016104330067 | 2016-06-17 | ||
| CN201610433006 | 2016-06-17 |
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| CN107523224B CN107523224B (en) | 2020-04-14 |
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|---|---|---|---|
| CN201710444763.9A Active CN107523224B (en) | 2016-06-17 | 2017-06-13 | Method for producing polishing wax |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111234710A (en) * | 2020-02-20 | 2020-06-05 | 广州赫厉狮森汽车用品有限公司 | Automobile paint surface protective wax and preparation method thereof |
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| CN101148565A (en) * | 2007-09-08 | 2008-03-26 | 李而淮 | Wax polish and preparation method thereof |
| CN102925214A (en) * | 2011-08-09 | 2013-02-13 | 苏喜红 | Fischer-Tropsch synthesis wax refinement method |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
| CN103773427A (en) * | 2012-10-26 | 2014-05-07 | 中国石油化工股份有限公司 | Method for preparing liquid wax |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA421565A (en) * | 1944-07-18 | Standard Oil Development Company | Wax sweating process | |
| GB687235A (en) * | 1950-03-24 | 1953-02-11 | Bataafsche Petroleum | Improvements in and relating to the treatment of paraffin wax |
| CN101148565A (en) * | 2007-09-08 | 2008-03-26 | 李而淮 | Wax polish and preparation method thereof |
| CN102925214A (en) * | 2011-08-09 | 2013-02-13 | 苏喜红 | Fischer-Tropsch synthesis wax refinement method |
| CN103102972A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation process for thermoinduction wax medium for automatic enrichment valve of motorcycle |
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| CN111234710A (en) * | 2020-02-20 | 2020-06-05 | 广州赫厉狮森汽车用品有限公司 | Automobile paint surface protective wax and preparation method thereof |
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