CN107513411B - A kind of production method of wax polish - Google Patents
A kind of production method of wax polish Download PDFInfo
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- CN107513411B CN107513411B CN201610432871.XA CN201610432871A CN107513411B CN 107513411 B CN107513411 B CN 107513411B CN 201610432871 A CN201610432871 A CN 201610432871A CN 107513411 B CN107513411 B CN 107513411B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
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- C—CHEMISTRY; METALLURGY
- 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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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a kind of production methods of wax polish.The method of the present invention is using F-T synthetic product as raw material, through sweating, emulsification preparation purpose product.This method is on the basis of common sweating process, liquid composition is carried out to force separation solids fraction and liquid composition by wax layer using air-flow in sweating effort, and preferably the aqueous solution of raw material and the decomposable substance for generating gas is emulsified, it is also beneficial to the quick discharge of liquid composition, to produce the basic material without low-melting component；It is glazing wax product that basic material is emulsified with components such as silicone oil, native paraffin, the molten type auxiliary agents of oil again.The method of the present invention have many advantages, such as investment of production equipment is low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution, glazing wax product high temperature resistance it is good.
Description
Technical field
The invention belongs to daily chemical product production technical fields, more particularly to a kind of production method of wax polish, especially
It is the production method of the glazing wax product suitable for various hard surfaces (floor, furniture, automobile etc.).
Background technique
Glazing product is mainly the gloss for generating or restoring various surfaces (floor, furniture, automobile etc.), while being played clear
The effects of clean, wear-resistant, anticorrosion (exposing to the weather), waterproof, resistant to high temperatures, antiultraviolet, antistatic, scratch resistance.
Wax polish is different by mode of appearance, can be divided into the types such as solid, lotion, liquid.By decentralized medium difference, can be divided into
The types such as solvent dispersion, emulsion dispersion；From composition, wax polish includes volatile component and film-forming components and accessory ingredients
(emulsifier, grinding agent, thickener, antioxidant, UV resistant agent, essence etc.) three categories substance.Volatile component is (to solvent point
Dissipating class product is various organic solvents, is the substances such as water, alcohol, organic solvent to emulsion dispersion class product) it is intended, primarily, to improve
The workability of light wax；Film-forming components play the effects of glazing.It is (poly- that the film-forming components of wax polish generally comprise wax, silicone oil, resin
Carbonate resin, polyurethane resin, fluororesin, polyacrylate resin etc.) etc. hydrophobic substances.Wax used in wax polish mainly wraps
Include pertroleum wax (paraffin, microwax), native paraffin (beeswax, Chinese wax, Ka Naba wax, candelila wax, lignite wax, rice bran wax etc.),
Synthetic wax (polyethylene wax, polypropylene wax) etc..Emulsifying wax polish is easy to use, it is laborsaving to embrocate, therefore is widely used.
Some glazing wax products can encounter 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 when its solarization, 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, will will influence the appearance for needing glazing article under the gloss for making coating surface.
Various native paraffins and synthetic wax can generate preferable gloss and heat-resist, but price is high.
The general name of the pertroleum wax all kinds of wax products obtained that are crude oil after refining processing from wax-containing distillate, including liquid
Body paraffin, soap manufacturing paraffin, paraffin and microwax.Paraffin be in crude oil lube cut through dewaxing, de-oiling, purification and molding
Production, typically contain C20~C50The components such as n-alkane, isoparaffin and a small amount of cycloalkane, usual fusing point is 50 DEG C~
74℃.Microwax be decompression residuum after propane equal solvent depitching again through dewaxing, de-oiling, purification and molding and etc. production
, generally by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition, usual dropping point 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 the base oil wax below of oil content 2% is prepared using slack wax as raw material, and de-oiling technique mainly has solvent
De-oiling and sweating de-oiling.Through clay-filtered or hydrofinishing and molding, packaging and other steps, commodity stone can be obtained again in base oil wax
Oily wax.
Pertroleum wax is the hydrocarbon mixture of n-alkane, isoparaffin, cycloalkane of a variety of carbon numbers etc., carbon number distribution compared with
Width, therefore must wherein contain a certain number of low-melting components (oil and lower melting-point wax).Excessive use stone in wax polish
The pertroleum waxes such as wax, microwax will cause glazing film poor heat resistance.
Fischer-Tropsch (F-T) synthetic technology be nineteen twenty-three invention, mainly include high temperature synthesis techniques and low temperature synthesis technique,
F-T synthesis technology and catalyst all made breakthrough progress since nineteen nineties, and F-T sintetics is increasingly rich
It is rich.In F-T synthetic product chemical composition based on n-alkane, there is a small amount of isoparaffin, also contains more alkene and oxygen-containing
Compound, and carbon number distribution is very wide.F-T synthetic product is directly used in wax polish formula due to containing a large amount of low-melting components
In can also make glazing film poor heat resistance.
In terms of wax product production technology, the common manufacturing process that separates has distillation, solvent separation, sweating separation etc..
Distillation is to achieve the purpose that 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 distillation process needs raw material being heated to boiling point or more, consumes a large amount of energy.Such as
A kind of method for improving Fischer-Tropsch wax pour point of CN201410217632.3() it introduces raw material is removed into low boiling under high temperature high vacuum
Point substance, then the further distillation purification under extremely high vacuum, to prepare high melting-point wax product.Hydrocarbon of the fusing point at 70 DEG C or more simultaneously
The boiling point of class is more than 500 DEG C (normal pressures), and efficiency is greatly reduced when being separated using distillation.
Solvent fractionation method is that the property of the different solubility using components various in wax in a solvent carries out separating-purifying
, as CN200410043806.5(it is a kind of divide polyethylene wax method), a kind of separation polyethylene of CN201110351185.7(
The method of by-product polyethylene wax), its production that can be used for the products such as wax polish of gained high melting point polyethylene wax.Solvent separates work
Skill investment of production equipment is big；It needs largely to use solvent in production process, recycling design needs to consume a large amount of energy；In solvent
Benzene homologues are usually contained, environment can be impacted；Solvent is inflammable, be easy to cause production accident.
Sweating separation method carries out separating-purifying using components various in wax property with different melting points.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 biggish n-alkane of molecular weight
Fusing point is higher, and the fusing point of the lesser n-alkane of molecular weight is lower；When molecular weight is identical, the fusing point of isoparaffin and cycloalkane
To be lower than n-alkane, and isomery degree more high-melting-point is lower.
Compared with distillating method, since 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 does not use solvent, so sweating separation process is pacified
Entirely, energy conservation and on environment without influence.
Common sweating process mainly comprises the steps that (1) preparation: pad water is (with water full of sweatbox ware plate
Lower space) charge (raw material is heated to being packed into sweatbox when fusing point or more is in a liquid state) afterwards；(2) it crystallizes: by raw material with little
10 DEG C~20 DEG C of its fusing point or less are progressively cooled in the rate of temperature fall of 4 DEG C/h.In cooling procedure, various components by fusing point by
High to Low sequence successively crystallizes and forms solid；(3) it sweating: after wax layer temperature reaches preset cooling final temperature, puts
Fall to pad water；Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components are by fusing point by low
Successively be fused into liquid to high sequence and flow out the wax layer residue (on wax) finally obtained (under wax) be exactly high-melting-point, it is low
The wax of oil-containing；(4) it refines: collecting crude product and (continue to increase temperature after sweating effort, be taken out on wax with fusing, as slightly
Product), through clay-filtered (it be warming up to predetermined temperature after melting crude product, carclazyte is added and constant temperature was stirred to the predetermined time
Filtering) after, 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
O'clock in 70 DEG C or more of wax product.When common sweating process produces 40 DEG C~60 DEG C of soap manufacturing paraffin and low melt point paraffin, sweating
In journey although solids fraction (wax of higher melt) and liquid composition (oil and the wax compared with low melting point) two class components are respectively at solid
Two kinds of phases of body and liquid, but be also difficult to be kept completely separate.To make final products meet the requirements, extension sweating sessions are generallyd use
(reducing heating rate) and the method for improving sweating final temperature, but will lead to production cycle length and product yield decline in this way；
Experiments have shown that common sweating process production fusing point is in 70 DEG C or more of wax product, the carbon dispersion of distribution on sweating later period 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
It is improved with the decline of yield, fusing point is produced in the report of 70 DEG C or so of wax product with sweating process so so far there are no.
Compared with solvent separates, sweating process is intermittently operated, and product yield is lower, the production cycle is longer, but is sent out
Sweat technique has that small investment, production process is simple, operating cost is low, production process is safe, energy saving and no pollution to the environment etc. is excellent
Point still has part of the manufacturer producing soap manufacturing paraffin product using this method at present.
For many years, sweating method has obtained some development in equipment and process aspect, as CN89214332(vertical type square is more
Section partition sweat tank), CN94223980.6(ware type sudorific device), CN98233254.8(Paraffin sweating pot),
CN200920033500.X(novel paraffin sweating tank), a kind of Efficient paraffin sweatbox of CN201210508905.0(),
CN201320127680.4(tubular type paraffin deoiler) etc., it is improved in sweating equipment；CN91206202(is a kind of efficiently
Paraffin sweating pot) it is improved on sweating process, but these improvement cannot still produce wax product of the fusing point at 70 DEG C or more.
Sweating process is the unique solvent-free separation method being currently known for commercial scale wax product, green advocating
Color low-carbon, environmental protection and energy saving today, people is increasingly caused without the high melting-point wax product of low melting point using sweating process production
Concern, while while not influencing the performances such as wax polish high temperature resistant reduce glazing wax product production cost demand more
Add urgent.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of production methods of wax polish, including sweating, emulsification two
Part.Specifically using the F-T synthetic product that n-alkane weight content is 80% or more as sweating raw material, in common sweating
On the basis of technique, oil preferably is made in the aqueous solution of sweating paraffin and the decomposable substance for generating gas under stress
Sweating is carried out after water-in type emulsion, the gas and aqueous solution generated using decomposable substance decomposition forms small in wax layer
Space increases high temperature constant temperature process in crystallization process, is conducive to the discharge of sweating stage liquid component；And in sweating effort
Liquid composition is carried out to force separation solids fraction and liquid composition by wax layer using air-flow, separating effect is enhanced and adds
Fast separating rate；To produce the basic material without low-melting component；Again by basic material, synthetic wax, silicone oil, natural
Wax, the molten type auxiliary agent of oil are glazing wax product with deionized water emulsification under emulsifier effect.There is the method for the present invention production to set
It is standby to invest that low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution, glazing wax product high temperature resistance
The advantages that good.
A kind of production method of wax polish of the invention, including the following contents:
A: pre-emulsification
(A1) prepared by oil phase material: using F-T synthetic product as sweating raw material, heating fusing；W/o type emulsifier is added, stirs
It mixes uniformly, forms oil phase material；
(A2) prepared by water-phase material: under stress heating the aqueous solution of the decomposable substance for generating gas, is formed
Water-phase material；
(A3) prepared by emulsion: under pressure and stirring condition, the lower water-phase material for obtaining (A2) is added (A1) and obtains
Oil phase material, continue stirring 10~30 minutes after all adding to form emulsion；
B: sweating
(B1) preparation: the emulsion by the preparation of (A3) process is packed into sweatbox under stress；
(B2) it crystallizes: wax layer is cooled to by sweating raw material dropping point~dropping point+4 with 1.0 DEG C/h~3.0 DEG C/h rate
DEG C high temperature constant temperature temperature, and constant temperature is for a period of time；Wax layer is cooled to by sweating original with 2.0 DEG C/h~4.0 DEG C/h rate again
8 DEG C~15 DEG C of crystallization final temperature below drop fusing point；
(B3) it cryogenic thermostat: is crystallizing final temperature cryogenic thermostat for a period of time, while reducing pressure to normal pressure；
(B4) sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate；Wax layer reaches predetermined temperature and constant temperature for a period of time
After stop sweating；Wax layer is forced air flow through in sweating effort；
(B5) it refines: being wax polish basic material after refining on wax；
(C) production emulsification:
(C1) prepared by oil phase material: basic material and the molten type auxiliary agent heating of synthetic wax, silicone oil, native paraffin, oil being melted, stirred
It mixes uniformly, forms oil phase material；
(C2) prepared by water-phase material: O/W type emulsifier and deionized water being heated, water-phase material is formed；
(C3) prepared by emulsion: the oil phase material that (C1) is obtained is added in the water-phase material that (C2) is obtained under stiring,
Homogenized again after dispersion and emulsion is glazing wax product.
In method of the invention, F-T synthetic product described in step (A1), n-alkane weight content requires to be 80%
More than, preferably normal paraffin content be 90% or more F-T synthetic product as sweating raw material.
In method of the invention, sweating paraffin is generated into gas with decomposable in the presence of pressure and w/o type emulsifier
Substance aqueous solution emulsification after carry out sweating.W/o type emulsifier described in step (A1) be selected from nonionic surface active agent,
One or more of anionic surfactant, cationic surface active agent, amphoteric surfactant.The W/
O-shaped HLB value is 1~10, preferably 3~8.The freezing point or fusing point of the surfactant are lower than step (B4) sweating highest
Temperature (i.e. predetermined temperature described in step (B4)).
Wherein, it is stearic to be selected from sorbitan monooleate, anhydrous sorbitol list for the nonionic surface active agent
Acid esters, diethylene glycol aliphatic ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol list are stearic
One group of substance that acid esters, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester are constituted；Yin
Ionic surfactant is selected from fatty alcohol sulfate monoethanolamine salt, pareth sulfate, oleamide yl carboxylic acid
Sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurate, sodium butylnaphthalenesulfonate, Disodium sulfosuccinate, suitable succinate monoester
One group of substance that sodium sulfonate is constituted.The cationic surface active agent is selected from benzyl quaternary ammonium salt, dodecyl dimethyl benzyl
Ammonium chloride, dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride, three second
One group of substance that amide oleate is constituted；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 substance constituted at object.
In the present invention, the w/o type emulsifier is preferably the compound emulsifying agent that two or more surfactants are constituted.
In method of the invention, the substance of decomposable generation gas described in step (A2) is selected from carbonic acid, hydrogen peroxide, ammonia
One group of substance that water, chloric acid, hypochlorous acid are constituted, it is preferably water-soluble and itself and nontoxic, the non-stimulated smell of decomposition product
Carbonic acid, hydrogen peroxide etc..The concentration of the aqueous solution of the decomposable substance for generating gas is 0.1%~5.0%(mass, similarly hereinafter), preferably
It is 0.2%~2.0%.Using hydrogen peroxide aqueous solution when, it is inorganic strong that sodium hydroxide and/or potassium hydroxide etc. are added in hydrogen peroxide
Alkali accelerates the decomposition rate of hydrogen peroxide as catalyst, and uses nitrogen protection.The inorganic strong alkali is in hydrogen peroxide solution
Additional amount be 0.1~20.0 mg/Kg, preferably 0.2~8.0 mg/Kg.
In method of the invention, the proportion of emulsion obtained by step (A3) is general are as follows: and sweating paraffin 60.0%~
95.0%, it can decompose the aqueous solution 4.9%~30.0% for generating the substance of gas, w/o type emulsifier 0.1%~10.0%.It is preferred that emulsifying
The proportion of liquid are as follows: sweating paraffin 75.0%~89.0% can decompose the aqueous solution 10.0%~20.0% for generating the substance of gas, W/
O-shaped emulsifier 1.0%~5.0%.
Emulsion process described in step (A3) uses the ordinary skill in the art.Such as, the condition of the emulsification are as follows: at 90 DEG C
At~98 DEG C, 50~1500 revs/min of mixing speed mixes 5~60 minutes, is preferably stirred with 100~1000 revs/min
Speed is mixed to mix 10~30 minutes.Oil phase material and water-phase material are generally heated to 90 respectively in step (A1) and step (A2)
DEG C~95 DEG C and 90 DEG C~98 DEG C.
In method of the invention, the sweatbox is generally sweating ware, and added above dismountable close in wax layer
Envelope system and pressurizing device.Increase air pressure during step (A2), (A3), (B1) and (B2) to inhibit in water-phase material system
The gas that the decomposition and decomposition of decomposable substance generate during standby, emulsion preparation, preparation and crystallization etc. escapes wax layer.
The pressure (gauge pressure) is 0.5~50.0 atmospheric pressure, preferably 15.0~30.0 atmospheric pressure.
In method of the invention in method of the invention, the sweating ware in wax layer pressurizing device added above and/or
Increase vacuum plant below wax layer, wax layer is made to form pressure difference up and down.Wax layer is forced air flow through described in step (B4) to adopt
Increase pressure (air pressure) above wax layer and/or reduce pressure (air pressure) below wax layer, forms wax layer upper and lower (side)
Pressure difference is realized.The pressure difference is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force gas
Stream passes through wax layer.
In method of the invention, time of high-temperature constant temperature section described in step (B2) is 0.1~6.0 hour, preferably 0.5
~5.0 hours, more preferably 1.0~4.0 hours.
In method of the invention, time of cryogenic thermostat section described in step (B3) is 0.1~5.0h, preferably 0.5~
3.0h；Pressure is gradually decreased to normal pressure simultaneously.The rate of the pressure reduction is generally 0.1~150.0 atmospheric pressure/hour,
Preferably 5.0~50.0 atmospheric pressure/hour.
In method of the invention, the predetermined temperature (i.e. final temperature) of step (B4) described heating is basic material drip melt
- 10 DEG C of point~basic material dropping point.It is described be warming up to predetermined temperature after, solids fraction and liquid can be made by increasing the constant temperature stage
The separation of state component is more abundant, and the time in constant temperature stage is 0.1~10.0 hour, preferably 1.0~8.0 hours, most preferably 2.0
~6.0 hours.
In method of the invention, the heating rate and cooling rate of said wax layer can pass through air bath, water-bath, oil bath
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer heating is controlled using water-bath or oil bath mode
When rate and rate of temperature fall, collet can be increased outside sweating ware, collet is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function, the substances such as water or conduction oil are added as circulatory mediator in the circulatory system；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 method of the invention, wax layer is forced air flow through described in step (B4) can be real in sweating effort any stage
It applies, preferably implements at sweating initial stage.
In method of the invention, wax layer is forced air flow through described in step (B4) and is utilized in increase air pressure above wax layer
It realizes, can such as apply the gauge of 0.2~2.0 atmospheric pressure above wax layer, and remain normal pressure below wax layer.
In method of the invention, wax layer is forced air flow through described in step (B4) and is utilized in reduction air pressure below wax layer
It realizes, normal pressure can be such as kept above wax layer, and maintain the gauge of -0.2~-0.8 atmospheric pressure below wax layer.
In method of the invention, synthetic wax described in step (C1) can be one of silicon wax, oxidized polyethylene wax
Or mixtures thereof.The silicone oil can be methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, aminomethyl phenyl silicon
One of oil, methylchlorophenyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, amido silicon oil or
Its mixture.The native paraffin can be beeswax, Chinese wax, Ka Naba wax, candelila wax, lignite wax, one in rice bran wax
Or mixtures thereof kind.The described molten type auxiliary agent of oil 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, methylene chloride, ether, ethylene oxide, vinegar
Sour methyl esters, ethyl acetate, propyl acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, acetone, methyl fourth
Ketone, methylisobutylketone, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol ether acetate, ethylene glycol
Or mixtures thereof one of ether-ether, phenol, turpentine oil, tasteless kerosene.Preferably nontoxic, low smell, volatility be appropriate, price
D40, D60 low, source is wide, D80, No. 90, No. 120, No. 180, No. 190, No. 200, ExxsolD40, ExxsolD80,
ExxsolD110, ExxsolD130, ExxsolDSP80/100, propyl acetate, dimethyl succinate, in dimethyl glutarate
Or mixtures thereof one kind.
In method of the invention, O/W type emulsifier described in step (C2) can be anionic surfactant, such as
The dodecyl benzene sulfonic acid of the Lamepon A of high carboxylic acid's salt form or the lauryl sodium sulfate of sulfuric ester salt form or sulfonate type
Sodium, alkylolamides type triethanolamine, morpholine；It is also possible to nonionic surface active agent, such as the fatty alcohol of polyoxyethylene-type
The Span(sapn of polyoxyethylene ether (peregal) or polyol type) -60, Span(sapn) -80 and Tween-60, Tween-
80；It can also be one of non-ion fluorin carbon surface active agent, such as 0301 surfactant of LX or a variety of.
In the present invention, the condition of emulsification described in step (C3) are as follows: at 85 DEG C~98 DEG C, in 1000~10000 revs/min
Dispersion and emulsion 5~120 minutes under the mixing speed of clock.
In method of the invention, in terms of the quality of wax polish, the composition of wax polish described in step (C3) are as follows: basic material
5.0%~10.0%, synthetic wax 2.0%~6.0%, silicone oil 1.5%~6.0%, native paraffin 2.0%~8.0%, O/W type emulsifier 1.5%
~8.0%, the molten type auxiliary agent 6.0%~20.9% of oil, surplus are water；It preferably constitutes are as follows: basic material 5.0%~8.0%, synthetic wax
2.0%~4.0%, silicone oil 2.5%~4.0%, native paraffin 2.0%~5.0%, O/W type emulsifier 1.5%~5.0%, the molten type auxiliary agent of oil
6.0%~15.0 %, surplus are water.
Wherein, preservative, antioxidant, one in essence can also be added in wax polish described in step (C3) as needed
Kind or more be used as additive.The additional amount of the additive in mass are as follows: preservative 0.01~0.2%, preferably 0.01~
0.1%；Antioxidant 0.1~1.0%, preferably 0.2~1.0%；Essence 0.1~1.0%, preferably 0.2~0.5%.The preservative can
To be one of sodium benzoate and/or ammonium benzoate.The antioxidant is antioxidant BHT, antioxidant 1010, antioxidant
1076, antioxidant CA, antioxidant 1330, antioxidant 3114, antioxidant 164, irgasfos 168, antioxidant 264, antioxidant B215,
Or mixtures thereof one of antioxidant B225.
In method of the invention, the emulsion process of wax polish described in step (C3) are as follows: by basic material, synthetic wax,
Native paraffin, silicone oil, the molten type auxiliary agent of oil and antioxidant heating, which are melted and be uniformly mixed, is used as oil phase material；By surfactant with
And preservative is add to deionized water and heats and be uniformly mixed as water-phase material；High-speed stirred water-phase material and by oily phase material
Material is added in water-phase material and mixes dispersion and emulsion, then is homogenized and cooling, as glazing wax product after essence are added as needed.
Analysis shows not impurity such as sulfur-bearing, nitrogen, aromatic hydrocarbons in F-T synthetic product, are easy to reach very high pure by purification
Degree；In the chemical composition of low temperature F-T synthetic product based on n-alkane and distribution is very wide, and contain a small amount of alkene and oxygen-containing
Compound.Due to that can make the bad stability under high temperature there are olefin component, oxygenatedchemicals has special smell.A large amount of eutectics
Point component, which makes it be directly used as wax polish group timesharing, will lead to high temperature resistance variation.Therefore F-T synthetic product is not suitable for directly
With the allotment component of wax polish.
Sweating separation method is separated using various components property with different melting points.For the research of sweating effort
Show that liquid composition is gradually discharged along crystalline portion in sweating effort, the feelings flowed in capillary similar to liquid
Condition.But the high melting-point wax for fusing point at 70 DEG C or so causes crystals upon crystallization structure thin since raw material chemical composition is complicated
Small densification forms huge filter flow resistance power to the discharge of liquid composition, this results in the common sweating for only leaning on gravity natural separation
Solids fraction is difficult to be kept completely separate with liquid composition in the process, thus common sweating separating technology cannot 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 product to produce inexpensive high temperature resistant glazing wax product
Research, for F-T synthetic product contain a certain amount of alkene and oxygenatedchemicals (fusing point of these components is usually less than 65 DEG C,
Belong to low-melting component), also the low-melting component containing a large amount of alkanes is that F-T synthetic product is caused to be not suitable for being directly used in allotment
The reason of glazing wax product, removes these non-Suitable ingredients by using sweating method.By going deep into common sweating effort
Research, is difficult to the reason of separating with liquid composition for solids fraction, uses in sweating effort and forces air flow through wax layer, and
Increase the processes such as constant temperature stage in crystallization process and sweating effort, while further preferably by sweating raw material and can decompose generation gas
Sweating is carried out after the aqueous solution emulsification of substance, these measures effectively remove alkene in sweating raw material, oxygenatedchemicals and low
The non-Suitable ingredients such as fusing point alkane, make product be suitable as the basic material of wax polish.
It is difficult to the reason of separating with liquid composition for solids fraction in sweating effort, by using gas in sweating effort
Stream forces the separation of solids fraction and liquid composition by the method that wax layer carries out liquid composition, enhances separating effect and adds
Fast separating rate；Increasing the high temperature constant temperature stage in crystallization process can make the crystallization of wax bigger, be conducive in sweating effort
The discharge of liquid composition.For wax crystallization process studies have shown that the chemical composition of wax be determine crystal habit it is main because
Element, while the condition of cooling procedure also will affect crystal habit, especially near dropping point at a temperature of cooling condition pair
The influence of crystal habit is most obvious.For wax when being cooled near dropping point, the n-alkane of larger molecular weight has formed crystallization analysis
Out, this partially crystallizable body can be used as the nucleus for being subsequently formed crystallization, increases the high temperature constant temperature stage at this time, can enable nucleus
Sufficiently increase, larger sized crystal is formed, although this larger sized crystal is thick not as good as the crystallization of low melt point paraffin
Greatly, but the crystal structure of this increase is also highly beneficial to sweating stage discharge liquid composition.Simultaneously further preferably by raw material
It is emulsified under stress with the aqueous solution of the decomposable substance for generating gas, is formed after w/o type emulsion is used as and carry out sweating.
The aqueous solution that can decompose the substance of generation gas in emulsion is evenly distributed in raw material wax layer in the form of fine particle；Keep pressure
Emulsion is cooled to 8 DEG C~15 DEG C of dropping point or less under the conditions of power.It is applied during step (A2), (A3), (B1) and (B2)
The pressure for adding 0.5~50.0 atmospheric pressure (gauge pressure), can inhibit water-phase material prepare, emulsion preparation, preparation and
The gas that the decomposition and decomposition of decomposable substance generate during crystallization etc. escapes wax layer.Wax layer is cooled to constant temperature after predetermined temperature
0.1h~3.0h is so that wax layer crystallization is more abundant；Pressure is gradually decreased in thermostatic process to normal pressure simultaneously.Raw material is cooled to drop
Wax layer is in softer solid state in the time terminated after below fusing point to sweating effort, this can decompose substance gradually in the process
Decomposition releases gas, and equally distributed micro-bubble is formed in raw material wax layer；Pass through wax using air-flow in sweating effort
Layer, can carry out the aqueous solution of decomposable substance to form short space in wax layer, what these short spaces and bubble generated
Short space is easy to be formed in sweating effort several tiny channels in wax layer, is conducive to liquid composition in sweating effort
Discharge；Air-flow can also carry out liquid composition to force separation solids fraction and liquid composition simultaneously, to enhance separation effect
Fruit simultaneously accelerates separating rate.Selected surfactant fusing point or freezing point are lower than the maximum temperature of sweating effort, and contain official
It can roll into a ball, it is poor with the intermiscibility of paraffin, it can be discharged in sweating effort with liquid composition.It is aided with the cryogenic thermostat stage again
Keep solid crystal more abundant and to separate solids fraction and liquid composition the methods of more abundant the constant temperature stage of sweating effort,
Sweating process is allowed to produce the wax polish basic material without containing low-melting component.
The oil phase material that the components such as basic material, synthetic wax, native paraffin, silicone oil, the molten type auxiliary agent of oil are constituted adds under stiring
In the water-phase material for entering the components such as O/W type emulsifier and deionized water composition, dispersion and emulsion and be glazing wax product after cooling down.
This have the advantage that: by carrying out liquid composition using forcing air flow through wax layer in sweating effort
Method enhance the separating effect of solids fraction and liquid composition and accelerate separating rate；Crystal is increased using high temperature crystallization
Size, while being excluded using the aqueous solution that decomposable substance decomposition generates short space and decomposable substance that micro-bubble is formed
The short space generated afterwards is also beneficial to the quick discharge of liquid composition；And increase cryogenic thermostat stage and sweating effort
The processes such as constant temperature stage, so that sweating process be allow to produce the wax polish basic material without low-melting component；By base
Plinth material and synthetic wax, silicone oil, native paraffin, the molten type auxiliary agent of oil, emulsifier, deionized water and preservative, antioxidant, essence etc. are newborn
It is glazing wax product after change.Method of the invention have plant investment is low, production process is simple and operating cost is low, it is safe,
Energy saving and solvent-free pollution environment, the advantages that glazing wax product high temperature resistance is good.
Specific embodiment
The present invention is raw material by selecting suitable low temperature F-T synthetic product, on the basis of common sweating process, sweating
Ware top connects dismountable sealing device and connect with pressurized buffer tank and compressor, and/or connection subtracts in sweating ware lower part
Press surge tank and vacuum pump；Sweating raw material heating fusing simultaneously preferably generates under the conditions of pressure and w/o type emulsifier with decomposable
Sweating ware is packed into after the aqueous solution emulsification of the substance of gas；Wax layer heating-cooling speed is controlled with oil bath；Wax layer temperature is down to sweating
Raw material dropping point temperature nearby and high temperature constant temperature for a period of time；Continue to be cooled to preset temperature and cryogenic thermostat for a period of time；?
In sweating effort, start compressor in wax layer positive pressure formed above, and/or starting vacuum pump is with formed below negative in wax layer
Pressure, to force air flow through wax layer；Wax layer temperature reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；On wax
The wax polish basic material after refining；Basic material and synthetic wax, silicone oil, native paraffin, the molten type auxiliary agent of oil, O/W type are emulsified
It is glazing wax product after the emulsification such as agent, deionized water and preservative, antioxidant, essence.Method of the invention is thrown with device
Provide low, production process is simple and operating cost is low, safety, energy conservation and solvent-free pollution environment, glazing wax product heat resistance it is good
The advantages that.
1-4 illustrates the production method of wax polish of the present invention by the following examples.As related to below without especially indicating
And % is mass percent, the pressure is gauge pressure.
Embodiment 1
The present embodiment includes: A: pre-emulsification, B: sweating and C: production emulsification three parts.
A: pre-emulsification: this part includes the preparation of (A1) oil phase material, the preparation of (A2) water-phase material, (A3) emulsion preparation three
A step.
(A1) prepared by oil phase material
Take the wax oil product (normal paraffin content of Sinopec Group's low temperature F-T compound experiment device
For 95.50wt%；86.2 DEG C of dropping point；Needle penetration (25 DEG C) 55(10-1Mm)；Needle penetration (65 DEG C) > 200(10-1Mm).From 25
DEG C and 65 DEG C of needle penetration can be seen that and contain a large amount of low melting points in the wax oil product) 76.5Kg, be heated to 91 DEG C of fusings
Diethylene glycol aliphatic ester, the sorbitan monopalmitate of 0.7Kg and the oleoyl amido carboxylic of 0.4Kg of 2.4Kg are added afterwards
Sour sodium, stirs evenly.
(A2) prepared by water-phase material
By the CO of 0.10Kg under 20.2~20.4 atmospheric pressure2It is dissolved in the water of 19.9Kg, is heated to 95 DEG C.
(A3) prepared by emulsion
Oil phase material is forced into 20.2~20.4 atmospheric pressure, and with the stirring of the speed of 500r/ min；By water-phase material
It is added in oil phase material, continues to stir 25min, form w/o type emulsion.
B: sweating: this part includes (B1) preparation, (B2) cooling-high temperature constant temperature-decrease temperature crystalline, (B3) low temperature perseverance
Temperature, (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 is installed in sweating ware lower part
Tank simultaneously connects vacuum pump；Sweating ware collet and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；With
Conduction oil is heat medium；The heating function for starting the circulatory system, makes recycle oil be warming up to 95 DEG C.Pad below sweating ware ware plate
Water.The sealing system on sweating ware top is installed；Hair is added in the emulsion prepared in (A3) under 20.2~20.4 atmospheric pressure
Sweat ware.
(B2) cooling-high temperature constant temperature-decrease temperature crystalline
Start the refrigerating function of the circulatory system, controlling wax layer temperature declines wax layer temperature with the rate of temperature fall of 2.0 DEG C/h
To 89.0 DEG C and 3.0 hours progress high temperature constant temperatures of constant temperature, so that crystal sufficiently increases；Wax is made with the rate of temperature fall of 2.5 DEG C/h again
Layer temperature drops to 76.0 DEG C so that wax layer crystallizes to form solid.Close the refrigerating function of the circulatory system.
(B3) cryogenic thermostat
In 76.0 DEG C of constant temperature 2.0h so that wax layer crystallization is more abundant, while pressurized buffer tank internal pressure is controlled by emptying system
Power is gradually decrease to normal pressure with 30 atmospheric pressure/h rates.Close the refrigerating function of the circulatory system.
(3) heating-constant temperature sweating
Sweating ware is discharged and pads water.Sweating ware outlet connection intermediate storage tank (I) is to receive under wax；Start compressor and keeps adding
Pressure buffering pressure inside the tank is stablized keeps normal pressure below 1.6~1.8 atmospheric pressure, sweating ware ware plate；Start circulation system
Function makes wax layer temperature be increased to 85.0 DEG C with the heating rate of 1.5 DEG C/h.Stop compressor.
It opens vacuum pump and pressure-reducing cushioning pressure inside the tank is kept to stablize the air pressure above -0.4~-0.6 atmospheric pressure, wax layer
Keep normal pressure；Wax layer temperature is set to be increased to 88.0 DEG C and constant temperature 4.0 hours with the heating rate of 1.0 DEG C/h, so that in wax layer
Solids fraction and liquid composition are sufficiently separated.Stop vacuum pump, terminates sweating effort.
The outlet of sweating ware is changed to connection crude product storage tank (I) to receive on wax.Continue to increase the temperature of conduction oil to 115
DEG C, it is taken out on wax with fusing, as crude product (I).
(B5) it refines
Crude product (I) is basic material (I) after clay-filtered.
Basic material (I) property: 92.5 DEG C of dropping point；Needle penetration (25 DEG C) 2 (10-1Mm)；Needle penetration (65 DEG C) 46(10-1Mm).The oxygenatedchemicals such as alkene and alcohol, acid are not detected in chromatography-mass spectral analysis.Basic material (I) yield is 38.6%(phase
Wax oil is synthesized for sweating raw material F-T).
The oxygenatedchemicals such as alkene and alcohol, acid, which are not detected, from chromatography-mass spectral analysis can be seen that in basic material (I)
These substances have removed；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: production emulsification: this part includes the preparation of (C1) oil phase material, the preparation of (C2) water-phase material, the preparation of (C3) emulsion
Three steps.
(C1) prepared by oil phase material: weighing basic material (I) 5.0Kg, silicon wax tree rouge (DOW CORNING SW-8005 C30)
1.0Kg, 1.8 Kg, Ka Naba wax of oxidized wax (Sha Suo company A28) (3#, Brazil) 5.0Kg, hydroxy silicon oil (LX0301, road health
Rather) 3.5Kg, No. 120 solvent naphtha (Sinopec Nanjing branch company) 9.0Kg are stirred until homogeneous after being heated to 95 DEG C of meltings as oil
Phase materials；
(C2) prepared by water-phase material: weighing morpholine (the happy together safe chemical products Co., Ltd of Beijing's saliva) 1.3Kg, nonionic
Fluorocarbon surfactant (YM-313, Shanghai Yu Mu Chemical Co., Ltd.) 0.2Kg, water 73.2Kg is mixed and heated to 90 DEG C and stirs
It is uniformly water phase material；
(C3) prepared by emulsion:
Oil phase material low whipping speed by (C1) preparation is to be added in the water phase material of (C2) preparation under 1500 revs/min；
It is packed into and holds after being homogenized by the heat exchanger that inner tube contains ceramic ring by emulsion under 0.6 megapascal pressure and be cooled to 40 DEG C
Device is cooled to room temperature as emulsion-type glazing wax product (I).
Emulsion-type glazing wax product (I) property: high-temperature stability: qualified；Low-temperature stability: qualified；Glossiness value added
17.Meet GB/T 23437-2009 standard requirements.
Embodiment 2
The present embodiment includes: A: pre-emulsification, B: sweating and C: production emulsification three parts.
A: pre-emulsification: this part includes the preparation of (A1) oil phase material, the preparation of (A2) water-phase material, (A3) emulsion preparation three
A step.
(A1) prepared by oil phase material
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment device (with embodiment 1)
The sorbitan monostearate of 2.3Kg, the diethylene glycol list laurel of 1.0Kg is added after being heated to 92 DEG C of fusings in 78.2Kg
The triacetamide oleate of acid esters and 0.5Kg, stirs evenly.
(A2) prepared by water-phase material
By the CO of 0.20Kg under 24.6~24.8 atmospheric pressure2It is dissolved in the water of 17.8Kg, is heated to 96 DEG C.
(A3) prepared by emulsion
Oil phase material is forced into 24.6~24.8 atmospheric pressure, and with the stirring of the speed of 750r/ min；By water-phase material
It is added in oil phase material, continues to stir 20min, form w/o type emulsion.
B: sweating: this part includes (B1) preparation, (B2) cooling-high temperature constant temperature-decrease temperature crystalline, (B3) low temperature perseverance
Temperature, (B4) heating-constant temperature sweating, (B5) refine five steps.
Preparation staged pressure is with (A3), remaining is the same as embodiment 1.
Basic material (II) property of this part preparation: 92.7 DEG C of dropping point；Needle penetration (25 DEG C) 2 (10-1Mm)；Needle enters
Spend (65 DEG C) 47(10-1Mm).The oxygenatedchemicals such as alkene and alcohol, acid are not detected in chromatography-mass spectral analysis.Basic material (II) is received
Rate is 39.1%(relative to sweating raw material F-T synthesis wax oil).
The oxygenatedchemicals such as alkene and alcohol, acid, which are not detected, from chromatography-mass spectral analysis can be seen that in basic material (II)
These substances have removed；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: production emulsification: this part includes the preparation of (C1) oil phase material, the preparation of (C2) water-phase material, the preparation of (C3) emulsion
Three steps.
(C1) prepared by oil phase material: weighing basic material (II) 6.0Kg, silicon wax tree rouge (DOW CORNING SW-8005 C30)
1.0Kg, 2.2 Kg, Ka Naba wax of oxidized wax (Sha Suo company A28) (3#, Brazil) 2.6Kg, hydroxy silicon oil (LX0301, road health
Rather) 2.0Kg, phenyl silicone oil (RB-1558, Guangzhou thunder nation chemical industry) 2.0Kg, No. 120 solvent naphthas (Sinopec Nanjing branch company)
11.5Kg is stirred until homogeneous after being heated to 95 DEG C of meltings as oil phase material；
(C2) prepared by water-phase material: weighing triethanolamine (Guangzhou De Xu new material Co., Ltd) 2.5Kg, non-ionic fluorocarbon
Surfactant (YM-313, Shanghai Yu Mu Chemical Co., Ltd.) 0.2Kg, 70.0 Kg of water is mixed and heated to 90 DEG C and stirs equal
Even is water phase material；
(C3) prepared by emulsion:
Oil phase material low whipping speed by (C1) preparation is to be added in the water phase material of (C2) preparation under 1500 revs/min；
It is packed into and holds after being homogenized by the heat exchanger that inner tube contains ceramic ring by emulsion under 0.6 megapascal pressure and be cooled to 40 DEG C
Device is cooled to room temperature as emulsion-type glazing wax product (II).
Emulsion-type glazing wax product (II) property: high-temperature stability: qualified；Low-temperature stability: qualified；Glossiness value added
16.Meet GB/T 23437-2009 standard requirements.
Embodiment 3
The present embodiment includes: A: pre-emulsification, B: sweating and C: production emulsification three parts.
A: pre-emulsification: this part includes the preparation of (A1) oil phase material, the preparation of (A2) water-phase material, (A3) emulsion preparation three
A step.
(A1) prepared by oil phase material
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment device (with embodiment 1)
The sorbitan monooleate of 1.8Kg, the diethylene glycol mono laurate of 0.6Kg is added after being heated to 92 DEG C of fusings in 80.6Kg
The empgen BB of ester and 0.5Kg, stirs evenly.
(A2) prepared by water-phase material
With 27.5% H2O2Solution, solid NaOH and H2O, which is prepared, contains H2O2 0.8%, the aqueous solution of NaOH 6.0mg/Kg, takes
16.5Kg is forced into 18.4~18.6 atmospheric pressure under a nitrogen atmosphere, and is heated to 96 DEG C.
(A3) prepared by emulsion
Oil phase material is forced into 18.4~18.6 atmospheric pressure under a nitrogen atmosphere, and is stirred with the speed of 300r/ min
It mixes；Water-phase material is added in oil phase material, continues to stir 30min, forms w/o type emulsion.
B: sweating: this part includes (B1) preparation, (B2) cooling-high temperature constant temperature-decrease temperature crystalline, (B3) low temperature perseverance
Temperature, (B4) heating-constant temperature sweating, (B5) refine five steps.
The preparation stage controls pressure with nitrogen, and pressure is with (A3), remaining is the same as embodiment 1.
Basic material (III) property of this part preparation: 92.2 DEG C of dropping point；Needle penetration (25 DEG C) 2 (10-1Mm)；Needle enters
Spend (65 DEG C) 44(10-1Mm).The oxygenatedchemicals such as alkene and alcohol, acid are not detected in chromatography-mass spectral analysis.Basic material (III) is received
Rate is 39.5%(relative to sweating raw material F-T synthesis wax oil).
The oxygenatedchemicals such as alkene and alcohol, acid, which are not detected, from chromatography-mass spectral analysis can be seen that in basic material (III)
These substances have removed；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: production emulsification: this part includes the preparation of (C1) oil phase material, the preparation of (C2) water-phase material, the preparation of (C3) emulsion
Three steps.
(C1) prepared by oil phase material: weighing basic material (III) 7.0Kg, silicon wax tree rouge (DOW CORNING SW-8005 C30)
4.0Kg, Ka Naba wax (3#, Brazil) 1.8Kg, Chinese wax (Hebei Dongsheng beeswax factory) 1.2Kg hydroxy silicon oil (LX0301, road health
Rather) 1.0Kg, phenyl silicone oil (RB-1558, Guangzhou thunder nation chemical industry) 2.0Kg, No. 120 solvent naphthas (Sinopec Nanjing branch company)
6.6Kg is stirred until homogeneous after being heated to 95 DEG C of meltings as oil phase material；
(C2) prepared by water-phase material: it is (wide to weigh Span-80 (Guangzhou De Xu new material Co., Ltd) 1.8 Kg, Tween-80
Zhou Dexu new material Co., Ltd) 1.8 Kg, non-ion fluorin carbon surface active agent (Shanghai Yu Mu Chemical Co., Ltd.) 0.2Kg,
Water 72.6Kg is mixed and heated to 90 DEG C and is stirred for water phase material；
(C3) prepared by emulsion:
Oil phase material low whipping speed by (C1) preparation is to be added in the water phase material of (C2) preparation under 1500 revs/min；
It is packed into and holds after being homogenized by the heat exchanger that inner tube contains ceramic ring by emulsion under 0.6 megapascal pressure and be cooled to 40 DEG C
Device is cooled to room temperature as emulsion-type glazing wax product (III).
Emulsion-type glazing wax product (III) property: high-temperature stability: qualified；Low-temperature stability: qualified；Glossiness value added
18.Meet GB/T 23437-2009 standard requirements.
Embodiment 4
The present embodiment includes: A: pre-emulsification, B: sweating and C: production emulsification three parts.
A: pre-emulsification: this part includes the preparation of (A1) oil phase material, the preparation of (A2) water-phase material, (A3) emulsion preparation three
A step.
(A1) prepared by oil phase material
Take the wax oil product of Sinopec Group's low temperature F-T compound experiment device (with embodiment 1)
The diethylene glycol aliphatic ester of 1.6Kg, the anhydrous sorbitol monostearate of 0.6Kg is added after being heated to 94 DEG C of fusings in 83.0Kg
The polyoxyethylene fatty acid ester of ester and 0.3Kg, stirs evenly.
(A2) prepared by water-phase material
With 27.5% H2O2Solution, solid KOH and H2O, which is prepared, contains H2O2 1.2%, the aqueous solution of 3.0 mg/Kg of KOH, takes
14.5Kg is forced into 27.1~27.3 atmospheric pressure under a nitrogen atmosphere, and is heated to 97 DEG C.
(A3) prepared by emulsion
Oil phase material is forced into 27.1~27.3 atmospheric pressure under a nitrogen atmosphere, and is stirred with the speed of 900r/ min
It mixes；Water-phase material is added in oil phase material, continues to stir 15min, forms w/o type emulsion.
B: sweating: this part includes (B1) preparation, (B2) cooling-high temperature constant temperature-decrease temperature crystalline, (B3) low temperature perseverance
Temperature, (B4) heating-constant temperature sweating, (B5) refine five steps.
The preparation stage controls pressure with nitrogen, and pressure is with (A3), remaining is the same as embodiment 1.
Basic material (IV) property of this part preparation: 91.8 DEG C of dropping point；Needle penetration (25 DEG C) 2 (10-1Mm)；Needle enters
Spend (65 DEG C) 43(10-1Mm).The oxygenatedchemicals such as alkene and alcohol, acid are not detected in chromatography-mass spectral analysis.Basic material (IV) is received
Rate is 38.2%(relative to sweating raw material F-T synthesis wax oil).
The oxygenatedchemicals such as alkene and alcohol, acid, which are not detected, from chromatography-mass spectral analysis can be seen that in basic material (IV)
These substances have removed；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: production emulsification: this part includes the preparation of (C1) oil phase material, the preparation of (C2) water-phase material, the preparation of (C3) emulsion
Three steps.
(C1) prepared by oil phase material: weighing basic material (IV) 8.0Kg, silicon wax tree rouge (DOW CORNING SW-8005 C30)
1.0Kg, 1.4 Kg, Ka Naba wax of oxidized wax (Sha Suo company A28) (1#, Brazil) 2.4Kg, beeswax (Hebei Dongsheng beeswax factory)
0.6Kg, hydroxy silicon oil (DOW CORNING) 1.0Kg, phenyl silicone oil (RB-1558, Guangzhou thunder nation chemical industry) No. 120 solvent naphthas of 1.5Kg
This big Chemical Co., Ltd. is thought in (Sinopec Nanjing branch company) 6.0Kg, the Jiangsu antioxidant 1330() 0.4Kg, it is heated to 95 DEG C
It is stirred until homogeneous after melting as oil phase material；
(C2) prepared by water-phase material: weighing morpholine (the happy together safe chemical products Co., Ltd of Beijing's saliva) 1.2 Kg, tween-
The Guangzhou 80(De Xu new material Co., Ltd) 3.6 Kg, (YM-313, Shanghai rain wood chemical industry are limited for non-ion fluorin carbon surface active agent
Company) 0.2Kg, sodium benzoate (Zhengzhou Hong Wang Chemical Industry Science Co., Ltd) 0.2 Kg, water 72.2Kg be mixed and heated to 90 DEG C simultaneously
It is stirred for water phase material；
(C3) prepared by emulsion:
Oil phase material low whipping speed by (C1) preparation is to be added in the water phase material of (C2) preparation under 1500 revs/min；
Essence (vanilla flavored, Shenyang He Tian fragrance Co., Ltd) 0.3Kg is added, contains emulsion by inner tube under 0.6 megapascal pressure
There is the heat exchanger of ceramic ring to be homogenized and be packed into container after being cooled to 40 DEG C, is cooled to room temperature as emulsion-type glazing wax product
(IV).
Emulsion-type glazing wax product (IV) property: high-temperature stability: qualified；Low-temperature stability: qualified；Glossiness value added
16.Meet GB/T 23437-2009 standard requirements.
The production method that can be seen that wax polish of the invention by embodiment 1-4, by increasing pressurization and/or vacuum
The improvement to sweatbox such as facility；Micro-bubble and water-soluble is formed in wax layer using the decomposable substance decomposition for generating gas
The short space formed after liquid discharge, the constant temperature for forcing air flow through in sweating effort wax layer, increasing crystallization and sweating effort
The improvement to sweating process such as stage；It enhances the separating effect of solids fraction and liquid composition and accelerates separating rate, from
And lower-molecular-weight component in raw material has been effectively removed, so that sweating process is produced the basic material without low-melting component.
Basic material again with synthetic wax, silicone oil, native paraffin, the molten type auxiliary agent of oil, emulsifier, deionized water and preservative, antioxidant, perfume (or spice)
The emulsion dispersions such as essence are glazing wax product.Method of the invention is low with plant investment, production process is simple and operating cost
Low, safety, energy conservation and solvent-free pollution environment, the advantages that glazing wax product heat resistance is good.
Claims (31)
1. a kind of production method of wax polish, including the following contents:
A: pre-emulsification
(A1) prepared by oil phase material: using F-T synthetic product as sweating raw material, heating fusing；W/o type emulsifier is added, stirring is equal
It is even, form oil phase material；
(A2) prepared by water-phase material: under stress heating the aqueous solution of the decomposable substance for generating gas, forms water phase
Material；The decomposable substance for generating gas is selected from least one of carbonic acid, hydrogen peroxide, ammonium hydroxide, chloric acid, hypochlorous acid；
(A3) prepared by emulsion: the oily phase material that (A1) is obtained is added in the water-phase material that (A2) is obtained under pressure and stirring condition
Material, continues stirring 10~30 minutes to form emulsion after all adding；
B: sweating
(B1) preparation: the emulsion by the preparation of (A3) process is packed into sweatbox under stress；
(B2) it crystallizes: wax layer is cooled to by sweating raw material dropping point~+4 DEG C of dropping point with 1.0 DEG C/h~3.0 DEG C/h rate
High temperature constant temperature temperature, and constant temperature 0.1~6.0 hour；Wax layer is cooled to by sweating original with 2.0 DEG C/h~4.0 DEG C/h rate again
8 DEG C~15 DEG C of crystallization final temperature below drop fusing point；
(B3) cryogenic thermostat: in crystallization final temperature cryogenic thermostat 0.1~5.0 hour, while pressure is reduced to normal pressure；
(B4) sweating: with the heating of 0.5 DEG C/h~2.5 DEG C/h rate；Wax layer reaches predetermined temperature and constant temperature 0.1~10.0 hour
After stop sweating；Wax layer is forced air flow through in sweating effort；The predetermined temperature is basic material -10 DEG C~base of dropping point
Plinth material dropping point；
(B5) it refines: being wax polish basic material after refining on wax；
(C) production emulsification:
(C1) prepared by oil phase material: basic material and the molten type auxiliary agent heating of synthetic wax, silicone oil, native paraffin, oil being melted, stirring is equal
It is even, form oil phase material；
(C2) prepared by water-phase material: O/W type emulsifier and deionized water being heated, water-phase material is formed；
(C3) prepared by emulsion: under agitation, the oil phase material that (C1) is obtained is added in the water-phase material that (C2) is obtained,
Homogenized again after dispersion and emulsion is glazing wax product.
2. according to the method for claim 1, which is characterized in that the substance of the decomposable generation gas be selected from carbonic acid,
One kind of hydrogen peroxide or combinations thereof object.
3. according to the method for claim 2, which is characterized in that the quality of the aqueous solution of the decomposable substance for generating gas is dense
Degree is 0.1~5.0%.
4. according to the method for claim 2, which is characterized in that the substance of the decomposable generation gas is hydrogen peroxide.
5. according to the method for claim 4, which is characterized in that catalyst is added in hydrogen peroxide, the catalyst is
Inorganic strong alkali, additional amount of the catalyst in hydrogen peroxide solution are 0.1~20.0 mg/Kg.
6. according to the method for claim 5, which is characterized in that the inorganic strong alkali is sodium hydroxide and/or hydroxide
Potassium.
7. according to the method for claim 1, which is characterized in that w/o type emulsifier described in step (A1) is selected from nonionic
Type surfactant, anionic surfactant, cationic surface active agent, amphoteric surfactant constitute one group
Substance, the freezing point or fusing point of w/o type emulsifier are lower than the maximum temperature of step (B4) sweating.
8. according to the method for claim 7, which is characterized in that the nonionic surface active agent is selected from Sorbitan
Alcohol monoleate, sorbitan monostearate, diethylene glycol aliphatic ester, sorbitan monopalmitate, tetrem two
Alcohol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester constitute one group
Substance；The anionic surfactant be selected from fatty alcohol sulfate monoethanolamine salt, pareth sulfate,
Oleamide yl carboxylic acid sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurate, sodium butylnaphthalenesulfonate, Disodium sulfosuccinate,
The one group of substance constituted along succinate monoester sodium sulfonate；The cationic surface active agent is selected from benzyl quaternary ammonium salt, 12
Zephiran, dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl
One group of substance that ammonium chloride, triacetamide oleate are constituted；The amphoteric surfactant be selected from empgen BB,
Dodecyldimethyl ammonium oxide, aliphatic group imidazolidine derivatives, derivative of fatty acid, amphoteric modified epoxy ethane addition
One group of substance that object is constituted.
9. according to the method for claim 7, which is characterized in that the w/o type emulsifier is two or more surface-actives
The compound emulsifying agent that agent is constituted, the HLB value of w/o type emulsifier are 1~10.
10. according to the method for claim 1, which is characterized in that step (A3) obtains the composition of emulsion are as follows: sweating raw material
Mass percent be 60.0%~95.0%, can decompose generate gas substance aqueous solution mass percent be 4.9%~
30.0%, the mass percent of w/o type emulsifier is 0.1%~10.0%.
11. according to the method for claim 7, which is characterized in that the composition of the emulsion are as follows: sweating material quality percentage
Number is 75.0%~89.0%, and can decompose and generate the mass percent of the aqueous solution of substance of gas is 10.0%~20.0%, emulsification
The mass percent of agent is 1.0%~5.0%.
12. according to the method for claim 1, which is characterized in that apply during step (A2), (A3), (B1) and (B2)
Gauge be 0.5~50.0 atmospheric pressure air pressure, with inhibit water-phase material preparation, emulsion preparation, preparation and
It can decompose the decomposition of substance in crystallization process and decompose the gas generated and escape wax layer.
13. according to the method for claim 4, which is characterized in that use nitrogen protection when using hydrogen peroxide solution.
14. according to the method for claim 1, which is characterized in that force air flow through wax layer described in step (B4) and adopt
Increase air pressure above wax layer and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize, it is described
Pressure difference is 0.1~5.0 atmospheric pressure.
15. according to the method for claim 1, which is characterized in that gradually decreased while cryogenic thermostat in step (B3)
For pressure to normal pressure, rate of pressure reduction is 0.1~150.0 atmospheric pressure/hour.
16. according to the method for claim 1, which is characterized in that force air flow through wax layer described in step (B4) and sending out
Sweat initial stage implements.
17. according to the method for claim 14, which is characterized in that the wax layer that forces air flow through uses 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.
18. according to the method for claim 14, which is characterized in that the wax layer that forces air flow through uses under wax layer
Side reduces air pressure and realizes, air pressure keeps normal pressure above wax layer, and the table of -0.2~-0.8 atmospheric pressure is maintained below wax layer
Pressure pressure.
19. according to the method described in claim 1, which is characterized in that the positive structure in F-T synthetic product described in step (A1)
The weight content of alkane is 80% or more.
20. according to the method for claim 1, which is characterized in that sweatbox described in step (B1) is sweating ware.
21. according to the method for claim 1, which is characterized in that the composition of step (C3) described wax polish in mass are as follows:
Basic material 5.0%~10.0%, synthetic wax 2.0%~6.0%, silicone oil 1.5%~6.0%, native paraffin 2.0%~8.0%, O/W type cream
Agent 1.5%~8.0%, oil solubility aids 6.0%~20.9%, surplus are water.
22. according to the method for claim 21, which is characterized in that be additionally added in the wax polish preservative, antioxidant,
One or more of essence is used as additive；The additional amount of the additive in mass are as follows: preservative 0.01~0.2%, antioxygen
Agent 0.1~1.0%, essence 0.1~1.0%.
23. according to method described in claim 1,21 or 22, which is characterized in that the synthetic wax is selected from silicon wax tree rouge, oxygen
Change at least one of polyethylene wax.
24. according to method described in claim 1,21 or 22, which is characterized in that the 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.
25. according to method described in claim 1,21 or 22, which is characterized in that the native paraffin be selected from beeswax, Chinese wax,
At least one of Ka Naba wax, candelila wax, rice bran wax.
26. according to method described in claim 1,21 or 22, which is characterized in that the oil solubility aids 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 hexamethylene
Ketone, chlorobenzene, dichloro-benzenes, methylene chloride, ether, ethylene oxide, methyl acetate, ethyl acetate, propyl acetate, succinic acid diformazan
Ester, dimethyl glutarate, dimethyl adipate, acetone, espeleton, methylisobutylketone, glycol monoethyl ether, ethylene glycol list second
At least one of ether, ethylene glycol monobutyl ether, ethylene glycol ether acetate, glycol ether ester, phenol, turpentine oil, tasteless kerosene.
27. according to method described in claim 1,21 or 22, which is characterized in that the O/W type emulsifier is selected from Lei meter Bang
A, lauryl sodium sulfate, neopelex triethanolamine, morpholine, Span-60, Span-80, Tween-60,
At least one of Tween-80, peregal, LX0301.
28. according to the method for claim 22, which is characterized in that the preservative is sodium benzoate and/or benzoic acid
Ammonium, the antioxidant are selected from antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 1330, antioxidant
3114, one or more of antioxidant 164, irgasfos 168, antioxidant 264, antioxidant B215, antioxidant B225.
29. according to the method for claim 3, which is characterized in that the quality of the aqueous solution of the decomposable substance for generating gas
Concentration is 0.2~2.0%.
30. according to the method for claim 5, which is characterized in that additional amount of the catalyst in hydrogen peroxide solution be 0.2~
8.0 mg/Kg。
31. according to the method for claim 14, which is characterized in that the pressure difference is 0.2~2.0 atmospheric pressure.
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| CN110105880A (en) * | 2019-05-30 | 2019-08-09 | 周立华 | A kind of vehicle glazing protection wax and preparation method thereof |
| CN114806399A (en) * | 2022-04-28 | 2022-07-29 | 广东优贝科技股份有限公司 | Automobile paint surface glaze and preparation method thereof |
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