CN107513411A - A kind of production method of wax polish - Google Patents
A kind of production method of wax polish Download PDFInfo
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- CN107513411A CN107513411A CN201610432871.XA CN201610432871A CN107513411A CN 107513411 A CN107513411 A CN 107513411A CN 201610432871 A CN201610432871 A CN 201610432871A CN 107513411 A CN107513411 A CN 107513411A
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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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Abstract
The invention discloses a kind of production method of wax polish.The inventive method prepares purpose product using F T synthetic products as raw material, through sweating, emulsification.This 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, and the aqueous solution that raw material and decomposable asymmetric choice net are preferably generated to the material of gas emulsifies, 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 emulsifies with components such as silicone oil, native paraffin, the molten type auxiliary agents of oil 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 production method of 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, organic solvent to emulsion dispersion class product)It is intended, primarily, to improve
The workability of light wax;Film-forming components play the effect such as glazing.The film-forming components of wax polish generally comprise wax, silicone oil, resin(It is poly-
Carbonate resin, polyurethane resin, fluororesin, polyacrylate resin etc.)Deng hydrophobic substance.Wax mainly wraps used in wax polish
Include 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)Deng.Emulsifying wax polish is easy to use, it is laborsaving to embrocate, therefore is widely used.
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, will will influences to need the outward appearance of glazing article under the gloss that coating surface be made.
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), its production available for products such as wax polishs of gained high melting point polyethylene wax.Solvent separates work
Skill investment of production equipment is big;Need largely to use solvent in production process, recycling design needs to consume substantial amounts of energy;In solvent
Benzene homologues are usually contained, 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 production method of wax polish, including sweating, emulsification two
Part.It is sweating raw material specifically by more than 80% F-T synthetic products of n-alkane weight content, in common sweating
On the basis of technique, oil is made in the aqueous solution for the material that sweating paraffin and decomposable asymmetric choice net preferably are generated into gas under stress
Sweating is carried out after water-in type emulsion, is formed using gas caused by decomposable asymmetric choice net substance decomposition and the aqueous solution in wax layer small
Space, increase high temperature constant temperature process in crystallization process, be advantageous to the discharge of sweating stage liquid component;And in sweating effort
Liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow, separating effect is enhanced and adds
Fast separating rate;So as to produce the basic material for being free of 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 emulsifying agent effect.The inventive method is set with production
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 resistance to elevated temperatures
The advantages that good.
A kind of production method of wax polish of the present invention, including herein below:
A:Pre-emulsification
(A1)It is prepared by oil phase material:Using F-T synthetic products as sweating raw material, heating fusing;W/o type emulsifying agent is added, stirring is equal
It is even, form oil phase material;
(A2)It is prepared by water-phase material:The aqueous solution that decomposable asymmetric choice net is generated to the material of gas under stress heats, and forms aqueous phase
Material;
(A3)It is prepared by emulsion:It is lower to incite somebody to action under pressure and stirring condition(A2)Obtained water-phase material adds(A1)Obtained oil
Phase material, continue stirring after all adding 10~30 minutes to form emulsion;
B:Sweating
(B1)Preparation:Under stress will(A3)Emulsion prepared by process loads sweatbox;
(B2)Crystallization:Wax layer is cooled to by sweating raw material melt drop temperature~+4 DEG C of melt drop temperature with 1.0 DEG C/h~3.0 DEG C/h speed
High temperature constant temperature temperature, and constant temperature is for a period of time;Wax layer is cooled to by sweating raw material drop with 2.0 DEG C/h~4.0 DEG C/h speed again
8 DEG C~15 DEG C of crystallization final temperature below fusing point;
(B3)Cryogenic thermostat:In crystallization final temperature cryogenic thermostat for a period of time, while pressure is reduced to normal pressure;
(B4)Sweating:Heated up with 0.5 DEG C/h~2.5 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)Production emulsification:
(C1)It is prepared by oil phase material:Basic material and the molten type auxiliary agent heating of synthetic wax, silicone oil, native paraffin, oil are melted, stirring is equal
It is even, form oil phase material;
(C2)It is prepared by water-phase material:O/W types emulsifying agent and deionized water are heated, form water-phase material;
(C3)It is prepared by emulsion:Under agitation will(C1)Obtained oil phase material adds(C2)In obtained water-phase material, disperse
Homogenized again after emulsification is glazing wax product.
In the method for the present invention, step(A1)Described F-T synthetic products, the requirement of its n-alkane weight content are 80%
More than, the F-T synthetic products that preferably normal paraffin content is more than 90% are as sweating raw material.
In the method for the present invention, sweating paraffin is generated into gas in the presence of pressure and w/o type emulsifying agent with decomposable asymmetric choice net
Material the aqueous solution emulsification after carry out sweating.Step(A1)Described w/o type emulsifying agent be selected from nonionic surface active agent,
One or more in anionic surfactant, cationic surface active agent, amphoteric surfactant.Described W/
O-shaped HLB value is in 1~10, preferably 3~8.The freezing point or fusing point of the surfactant are less than step(B4)Sweating highest
Temperature(That is step(B4)Described in 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 w/o type emulsifying agent is preferably the compound emulsifying agent that two or more surfactants are formed.
In the method for the present invention, step(A2)The material of described decomposable asymmetric choice net generation gas is selected from carbonic acid, hydrogen peroxide, ammonia
One group of material that water, chloric acid, hypochlorous acid are formed, it is preferably water-soluble and itself and nontoxic, the non-stimulated smell of catabolite
Carbonic acid, hydrogen peroxide etc..The concentration of the aqueous solution of the material of decomposable asymmetric choice net generation gas is 0.1%~5.0%(Quality, similarly hereinafter), preferably
For 0.2%~2.0%.Using hydrogen peroxide the aqueous solution when, it is inorganic strong that sodium hydroxide and/or potassium hydroxide etc. are added in hydrogen peroxide
Alkali, to accelerate the decomposition rate of hydrogen peroxide, and is protected as catalyst using nitrogen.The inorganic strong alkali is in hydrogen peroxide solution
Addition be 0.1~20.0 mg/Kg, preferably 0.2~8.0 mg/Kg.
In the method for the present invention, step(A3)The proportioning of resulting emulsion is generally:Sweating paraffin 60.0%~
95.0%, the aqueous solution 4.9%~30.0% of the material of decomposable asymmetric choice net generation gas, w/o type emulsifying agent 0.1%~10.0%.It is preferred that emulsify
The proportioning of liquid is:Sweating paraffin 75.0%~89.0%, the aqueous solution 10.0%~20.0% of the material of decomposable asymmetric choice net generation gas, W/
O-shaped emulsifying agent 1.0%~5.0%.
Step(A3)Described emulsion process uses the ordinary skill in the art.Such as, the condition of the emulsification is: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.Step(A1)And step(A2)In oil phase material and water-phase material are typically heated to 90 respectively
DEG C~95 DEG C and 90 DEG C~98 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(A2)、(A3)、(B1)With(B2)During increase air pressure to suppress in water-phase material system
Gas effusion wax layer caused by the decomposition and decomposition of decomposable asymmetric choice net material during standby, emulsion preparation, preparation and crystallization etc..
Described pressure(Gauge pressure)For 0.5~50.0 atmospheric pressure, preferably 15.0~30.0 atmospheric pressure.
In the method for the present invention in method of the invention, described sweating ware in wax layer pressue device added above and/or
Increase vacuum plant below wax layer, wax layer is formed pressure differential up and down.Step(B4)The described wax layer that forces air flow through is adopted
Increase pressure above wax layer(Air pressure)And/or pressure is reduced below wax layer(Air pressure), make wax layer upper and lower(Side)Formed
Pressure differential is realized.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force gas
Stream passes through wax layer.
In the method for the present invention, step(B2)Described in high-temperature constant temperature section time be 0.1~6.0 hour, preferably 0.5
~5.0 hours, more preferably 1.0~4.0 hours.
In the method for the present invention, step(B3)Described in time of cryogenic thermostat section be 0.1~5.0h, preferably 0.5~
3.0h;Pressure is gradually reduced simultaneously to normal pressure.The speed that the pressure reduces is generally 0.1~150.0 atmospheric pressure/hour,
Preferably 5.0~50.0 atmospheric pressure/hour.
In the method for the present invention, step(B4)The predetermined temperature of the heating(That is final temperature)Based on material drip melt
- 10 DEG C of point~basic material melt drop temperature.It is described be warming up to predetermined temperature after, the increase constant temperature stage can make solids fraction and liquid
The separation of state component is more abundant, and the time in constant temperature stage is 0.1~10.0 hour, preferably 1.0~8.0 hours, most preferably 2.0
~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~-0.8 atmospheric pressure is maintained below wax layer.
In the method for the present invention, step(C1)Described in synthetic wax can be one kind in silicon wax, OPE
Or its mixture.Described silicone oil can be methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, aminomethyl phenyl silicon
Oil, methylchlorophenyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, one kind in amido silicon oil or
Its mixture.Described native paraffin can be one in beeswax, Chinese wax, Ka Naba waxes, candelila wax, lignite wax, rice bran wax
Kind or its mixture.Described oily molten type auxiliary agent 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, 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
One kind or its mixture in ether-ether, phenol, turpentine oil, tasteless kerosene.Preferably nontoxic, low smell, volatility are appropriate, price
D40, D60 low, source is wide, D80, No. 90, No. 120, No. 180, No. 190, No. 200, ExxsolD40, ExxsolD80,
In ExxsolD110, ExxsolD130, ExxsolDSP80/100, propyl acetate, dimethyl succinate, dimethyl glutarate
A kind of or its mixture.
In the method for the present invention, step(C2)Described in O/W types emulsifying agent can be anionic surfactant, such as
The Lamepon A or the lauryl sodium sulfate of sulfuric ester salt form or the DBSA of sulfonate type of high carboxylic acid's salt form
Sodium, alkylolamides type triethanolamine, morpholine;Can also be nonionic surface active agent, such as the fatty alcohol of polyoxyethylene-type
APEO(Peregal)Or the Span of polyol type(Sapn)-60、Span(Sapn)- 80 and Tween-60, Tween-
80;It can also be non-ion fluorin carbon surface active agent, the one or more in such as surfactants of LX 0301.
In the present invention, step(C3)Described in the condition that emulsifies be: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 the method for the present invention, in terms of the quality of wax polish, step(C3)Described in the composition of wax polish be: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 types emulsifying agent 1.5%
~8.0%, the molten type auxiliary agent 6.0%~20.9% of oil, surplus are water;Preferably constitute for: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 types emulsifying agent 1.5%~5.0%, the molten type auxiliary agent of oil
6.0%~15.0 %, surplus are water.
Wherein, step(C3)Described in wax polish can also add as needed in preservative, antioxidant, essence one
Additive is used as more than kind.The addition of the additive is in mass: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%.Described preservative can
To be one kind in sodium benzoate and/or ammonium benzoate.Described antioxidant is antioxidant BHT, antioxidant 1010, antioxidant
1076th, antioxidant CA, antioxidant 1330, antioxidant 3114, antioxidant 164, irgasfos 168, antioxidant 264, antioxidant B215,
One kind or its mixture in antioxidant B225.
In the method for the present invention, step(C3)Described in the emulsion process of wax polish be:By basic material, synthetic wax,
Native paraffin, silicone oil, the molten type auxiliary agent of oil and antioxidant heating, which are melted and be well mixed, is used as oil phase material;By surfactant with
And preservative is added in deionized water to heat and be well mixed and is used as water-phase material;High-speed stirred water-phase material and by oil phase material
Material adds in water-phase material and mixes dispersion and emulsion, then is homogenized and is cooled down after adding essence as needed, as glazing wax product.
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.By going deep into common sweating effort
Research, the reason for being difficult to separate with liquid composition for solids fraction, used in sweating effort and force air flow through wax layer, and
In the process such as crystallization process and sweating effort increase constant temperature stage, while sweating raw material and decomposable asymmetric choice net are further preferably generated into gas
Sweating is carried out after the aqueous solution emulsification of material, these measures effectively removes alkene in sweating raw material, oxygenatedchemicals and low
The non-Suitable ingredients such as fusing 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;Increasing the high temperature constant temperature stage in crystallization process can make the crystallization of wax bigger, be advantageous in sweating effort
The discharge of liquid composition.Research for wax crystallization process shows, the chemical composition of wax be determine crystal habit it is main because
Element, while the condition of cooling procedure can also influence crystal habit, the especially cooling condition pair at the temperature near melt drop temperature
The influence of crystal habit is most obvious.For wax when being cooled near melt drop temperature, the n-alkane of larger molecular weight has formed crystallization analysis
Go out, this partially crystallizable body can now increase the high temperature constant temperature stage, can enable nucleus as the nucleus for being subsequently formed crystallization
Fully increase, larger sized crystal is formed, although this larger sized crystal is thick not as the crystallization of low melt point paraffin
Greatly, but this increase crystal structure to the sweating stage discharge liquid composition be also highly beneficial.Simultaneously further preferably by raw material
Emulsified under stress with the aqueous solution of the material of decomposable asymmetric choice net generation gas, formed after w/o type emulsion is used as and carry out sweating.
The aqueous solution of the material of decomposable asymmetric choice net generation gas is evenly distributed in the form of fine particle in raw material wax layer in emulsion;Keep pressure
Emulsion is cooled to below melt drop temperature 8 DEG C~15 DEG C under the conditions of power.In step(A2)、(A3)、(B1)With(B2)During apply
Add 0.5~50.0 atmospheric pressure(Gauge pressure)Pressure, can suppress water-phase material prepare, emulsion prepare, preparation and
Gas effusion wax layer caused by the decomposition and decomposition of decomposable asymmetric choice net material during crystallization etc..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 reduced in thermostatic process simultaneously to normal pressure.Raw material is cooled to drop
Wax layer is in softer solid state in the time terminated after below fusing point to sweating effort, and decomposable asymmetric choice net material is gradual during this
Decomposition discharges 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 asymmetric choice net material to form short space in wax layer, caused by these short spaces and bubble
Short space is easy to form some tiny passages in wax layer in sweating effort, is advantageous to liquid composition in sweating effort
Discharge;Air-flow can also carry out liquid composition to force to separate solids fraction and liquid composition simultaneously, so as to enhance separation effect
Fruit simultaneously accelerates separating rate.Selected surfactant fusing point or freezing point are less 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
Make solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction and liquid composition separate the methods of more abundant,
Sweating process is allowd to produce the wax polish basic material for not 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 formed adds under agitation
It is glazing wax product after dispersion and emulsion and cooling in the water-phase material for entering the components such as O/W types emulsifying agent and deionized water composition.
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 the aqueous solution for the short space and decomposable asymmetric choice net material for producing micro-bubble formation using decomposable asymmetric choice net substance decomposition excludes
Caused short space afterwards, it 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 can produce the wax polish basic material without low-melting component;By base
Plinth material and the breast such as synthetic wax, silicone oil, native paraffin, oil molten type auxiliary agent, emulsifying agent, deionized water and preservative, antioxidant, essence
It is glazing wax product after change.The present invention method have plant investment is low, production process is simple and operating cost is low, it is safe,
Energy-conservation and solvent-free pollution 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 simultaneously generates preferably under the conditions of pressure and w/o type emulsifying agent with decomposable asymmetric choice net
Load sweating ware after the aqueous solution emulsification of the material of gas;Wax layer heating-cooling speed is controlled with oil bath;Wax layer temperature is down to sweating
Raw material melt drop temperature temperature nearby and high temperature constant temperature for a period of time;Continue to be cooled to preset temperature and cryogenic thermostat for a period of time;
In sweating effort, start compressor with wax layer malleation formed above, and/or start vavuum pump with 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 refined;Basic material and synthetic wax, silicone oil, native paraffin, the molten type auxiliary agent of oil, O/W types are emulsified
It is glazing wax product after the emulsification such as agent, deionized water and preservative, antioxidant, essence.The method of the present invention has device throwing
Provide that low, production process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution environment, glazing wax product heat resistance are good
The advantages that.
1-4 illustrates the production method of wax polish of the present invention by the following examples.As without especially indicating, related to below
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(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three
Individual step.
(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).From 25 DEG C
It can be seen that with 65 DEG C of needle penetration and contain a large amount of low melting points in the wax oil product)76.5Kg, after being heated to 91 DEG C of fusings
Add 2.4Kg diethylene glycol fatty acid ester, 0.7Kg sorbitan monopalmitate and 0.4Kg oleamide yl carboxylic acid
Sodium, stir.
(A2)It is prepared by water-phase material
By 0.10Kg CO under 20.2~20.4 atmospheric pressure2It is dissolved in 19.9Kg water, is heated to 95 DEG C.
(A3)It is prepared by emulsion
Oil phase material is forced into 20.2~20.4 atmospheric pressure, and stirred with 500r/ min speed;Water-phase material is added
Into oil phase material, continue 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 is permanent
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 tank is installed simultaneously in sweating ware bottom
Connect vavuum pump;Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware;With heat conduction
Oil is heating medium;Start the heating function of the circulatory system, recycle oil is warming up to 95 DEG C.Pad water below sweating ware ware plate.Peace
Fill the sealing system on sweating ware top;Will under 20.2~20.4 atmospheric pressure(A3)The emulsion of middle preparation adds sweating ware.
(B2)Cooling-high temperature constant temperature-decrease temperature crystalline
Start the refrigerating function of the circulatory system, control wax layer temperature drops to wax layer temperature with 2.0 DEG C/h rate of temperature fall
89.0 DEG C and 3.0 hours progress high temperature constant temperatures of constant temperature, so that crystal fully increases;Wax layer is made with 2.5 DEG C/h rate of temperature fall again
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 it is more abundant, while by emptying system control pressurized buffer pressure inside the tank with
30 atmospheric pressure/h speed is gradually decrease to normal pressure.Close the refrigerating function of the circulatory system.
(3)Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank(Ⅰ)To receive under wax;Start compressor and keep pressurization slow
Rush the stable holding normal pressure below 1.6~1.8 atmospheric pressure, sweating ware ware plate of pressure inside the tank;Start circulation system function,
Wax layer temperature is set to be increased to 85.0 DEG C with 1.5 DEG C/h heating rate.Stop compressor.
Open vavuum pump and keep the stable air pressure above -0.4~-0.6 atmospheric pressure, wax layer of pressure-reducing cushioning pressure inside the tank
Keep normal pressure;Wax layer temperature is set to be increased to 88.0 DEG C of simultaneously constant temperature 4.0 hours with 1.0 DEG C/h heating rate, so that in wax layer
Solids fraction and liquid composition are sufficiently separated.Stop vavuum pump, terminate sweating effort.
The outlet of sweating ware is changed to connect crude product storage tank(Ⅰ)To receive on wax.Continue to raise the temperature of conduction oil to 115
DEG C, taken out with fusing on wax, as crude product(Ⅰ).
(B5)It is refined
Crude product(Ⅰ)It is basic material after clay-filtered(Ⅰ).
Basic material(Ⅰ)Property:92.5 DEG C of melt drop temperature;Needle penetration(25℃)2 (10-1mm);Needle penetration(65℃)46(10-1mm).Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.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 is not detected from chromatogram-mass spectral analysis can be seen that basic material(Ⅰ)In
These materials 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(C1)Oil phase material preparation,(C2)Water-phase material preparation,(C3)It is prepared by emulsion
Three steps.
(C1)It is prepared by oil phase material:Weigh basic material(Ⅰ)5.0Kg, silicon wax tree fat(DOW CORNING SW-8005 C30)
1.0Kg, oxidized wax(Sha Suo companies A28)1.8 Kg, Ka Naba waxes(3#, Brazil)5.0Kg, hydroxy silicon oil(LX0301, road health
Rather)3.5Kg, No. 120 solvent naphthas(Sinopec Nanjing branch company)9.0Kg, it is stirred until homogeneous after being heated to 95 DEG C of meltings as oil
Phase materials;
(C2)It is prepared by water-phase material:Weigh morpholine(The happy together safe chemical products Co., Ltd in Beijing Tianjin)1.3Kg, non-ionic fluorocarbon
Surfactant(YM-313, Shanghai Yu Mu Chemical Co., Ltd.s)0.2Kg, water 73.2Kg are mixed and heated to 90 DEG C and stirred
For aqueous phase material;
(C3)It is prepared by emulsion:
Will(C1)The oil phase material low whipping speed of preparation is to be added under 1500 revs/min(C2)In the aqueous phase material of preparation;0.6
It is under MPa that heat exchanger that emulsion contains ceramic ring by inner tube is homogenizing and be cooled to after 40 DEG C and load container, cool down
It is emulsion-type glazing wax product to normal temperature(Ⅰ).
Emulsion-type glazing wax product(Ⅰ)Property:High-temperature stability:It is qualified;Low-temperature stability:It is qualified;Glossiness value added
17.Meet the requirement of GB/T 23437-2009 standards.
Embodiment 2
The present embodiment includes:A:Pre-emulsification, B:Sweating and C:Production emulsification three parts.
A:Pre-emulsification:This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three
Individual step.
(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)78.2Kg,
Be heated to adding after 92 DEG C of fusings 2.3Kg sorbitan monostearate, 1.0Kg diethylene glycol monolaurate and
0.5Kg triacetamide oleate, stirs.
(A2)It is prepared by water-phase material
By 0.20Kg CO under 24.6~24.8 atmospheric pressure2It is dissolved in 17.8Kg water, is heated to 96 DEG C.
(A3)It is prepared by emulsion
Oil phase material is forced into 24.6~24.8 atmospheric pressure, and stirred with 750r/ min speed;Water-phase material is added
Into oil phase material, continue 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 is permanent
Temperature,(B4)Heating-constant temperature sweating,(B5)Refine five steps.
Preparation staged pressure is same(A3), remaining is the same as embodiment 1.
Basic material prepared by this part(Ⅱ)Property:92.7 DEG C of melt drop temperature;Needle penetration(25℃)2 (10-1mm);Pin enters
Degree(65℃)47(10-1mm).Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material(Ⅱ)Receive
Rate is 39.1%(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 basic material(Ⅱ)In
These materials 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(C1)Oil phase material preparation,(C2)Water-phase material preparation,(C3)It is prepared by emulsion
Three steps.
(C1)It is prepared by oil phase material:Weigh basic material(Ⅱ)6.0Kg, silicon wax tree fat(DOW CORNING SW-8005 C30)
1.0Kg, oxidized wax(Sha Suo companies A28)2.2 Kg, Ka Naba waxes(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, it is stirred until homogeneous after being heated to 95 DEG C of meltings as oil phase material;
(C2)It is prepared by water-phase material:Weigh triethanolamine(Guangzhou De Xu new materials Co., Ltd)2.5Kg, non-ion fluorin carbon surface
Activating agent(YM-313, Shanghai Yu Mu Chemical Co., Ltd.s)0.2Kg, the Kg of water 70.0 are mixed and heated to 90 DEG C and are stirred for
Aqueous phase material;
(C3)It is prepared by emulsion:
Will(C1)The oil phase material low whipping speed of preparation is to be added under 1500 revs/min(C2)In the aqueous phase material of preparation;0.6
It is under MPa that heat exchanger that emulsion contains ceramic ring by inner tube is homogenizing and be cooled to after 40 DEG C and load container, cool down
It is emulsion-type glazing wax product to normal temperature(Ⅱ).
Emulsion-type glazing wax product(Ⅱ)Property:High-temperature stability:It is qualified;Low-temperature stability:It is qualified;Glossiness value added
16.Meet the requirement of GB/T 23437-2009 standards.
Embodiment 3
The present embodiment includes:A:Pre-emulsification, B:Sweating and C:Production emulsification three parts.
A:Pre-emulsification:This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three
Individual step.
(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)80.6Kg,
Be heated to adding after 92 DEG C of fusings 1.8Kg sorbitan monooleate, 0.6Kg diethylene glycol monolaurate and
0.5Kg empgen BB, stirs.
(A2)It is prepared by water-phase material
With 27.5% H2O2Solution, solid NaOH and H2O, which is prepared, contains H2O2 0.8%th, the NaOH 6.0mg/Kg aqueous solution, takes
16.5Kg, 18.4~18.6 atmospheric pressure are forced under a nitrogen atmosphere, and be heated to 96 DEG C.
(A3)It is prepared by emulsion
Oil phase material is forced into 18.4~18.6 atmospheric pressure under a nitrogen atmosphere, and stirred with 300r/ min speed;Will
Water-phase material is added in oil phase material, is continued to stir 30min, is formed w/o type emulsion.
B:Sweating:This part includes(B1)Preparation,(B2)Cooling-high temperature constant temperature-decrease temperature crystalline,(B3)Low temperature is permanent
Temperature,(B4)Heating-constant temperature sweating,(B5)Refine five steps.
The preparation stage is same with nitrogen control pressure, pressure(A3), remaining is the same as embodiment 1.
Basic material prepared by this part(Ⅲ)Property:92.2 DEG C of melt drop temperature;Needle penetration(25℃)2 (10-1mm);Pin enters
Degree(65℃)44(10-1mm).Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material(Ⅲ)Receive
Rate is 39.5%(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 basic material(Ⅲ)In
These materials 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(C1)Oil phase material preparation,(C2)Water-phase material preparation,(C3)It is prepared by emulsion
Three steps.
(C1)It is prepared by oil phase material:Weigh basic material(Ⅲ)7.0Kg, silicon wax tree fat(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, it is stirred until homogeneous after being heated to 95 DEG C of meltings as oil phase material;
(C2)It is prepared by water-phase material:Weigh Span-80(Guangzhou De Xu new materials Co., Ltd)1.8 Kg, Tween-80(Guangzhou moral
Rising sun new material Co., Ltd)1.8 Kg, non-ion fluorin carbon surface active agent(Shanghai Yu Mu Chemical Co., Ltd.s)0.2Kg, water
72.6Kg is mixed and heated to 90 DEG C and is stirred for aqueous phase material;
(C3)It is prepared by emulsion:
Will(C1)The oil phase material low whipping speed of preparation is to be added under 1500 revs/min(C2)In the aqueous phase material of preparation;0.6
It is under MPa that heat exchanger that emulsion contains ceramic ring by inner tube is homogenizing and be cooled to after 40 DEG C and load container, cool down
It is emulsion-type glazing wax product to normal temperature(Ⅲ).
Emulsion-type glazing wax product(Ⅲ)Property:High-temperature stability:It is qualified;Low-temperature stability:It is qualified;Glossiness value added
18.Meet the requirement of GB/T 23437-2009 standards.
Embodiment 4
The present embodiment includes:A:Pre-emulsification, B:Sweating and C:Production emulsification three parts.
A:Pre-emulsification:This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three
Individual step.
(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,
Be heated to adding after 94 DEG C of fusings 1.6Kg diethylene glycol fatty acid ester, 0.6Kg sorbitan monostearate and
0.3Kg polyoxyethylene fatty acid ester, stirs.
(A2)It is prepared by water-phase material
With 27.5% H2O2Solution, solid KOH and H2O, which is prepared, contains H2O2 1.2%th, the mg/Kg of KOH 3.0 aqueous solution, takes
14.5Kg, 27.1~27.3 atmospheric pressure are forced under a nitrogen atmosphere, and be heated to 97 DEG C.
(A3)It is prepared by emulsion
Oil phase material is forced into 27.1~27.3 atmospheric pressure under a nitrogen atmosphere, and stirred with 900r/ min speed;Will
Water-phase material is added in oil phase material, is continued to stir 15min, is formed w/o type emulsion.
B:Sweating:This part includes(B1)Preparation,(B2)Cooling-high temperature constant temperature-decrease temperature crystalline,(B3)Low temperature is permanent
Temperature,(B4)Heating-constant temperature sweating,(B5)Refine five steps.
The preparation stage is same with nitrogen control pressure, pressure(A3), remaining is the same as embodiment 1.
Basic material prepared by this part(Ⅳ)Property:91.8 DEG C of melt drop temperature;Needle penetration(25℃)2 (10-1mm);Pin enters
Degree(65℃)43(10-1mm).Chromatogram-mass spectral analysis, the oxygenatedchemicals such as alkene and alcohol, acid is not detected.Basic material(Ⅳ)Receive
Rate is 38.2%(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 basic material(Ⅳ)In
These materials 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(C1)Oil phase material preparation,(C2)Water-phase material preparation,(C3)It is prepared by emulsion
Three steps.
(C1)It is prepared by oil phase material:Weigh basic material(Ⅳ)8.0Kg, silicon wax tree fat(DOW CORNING SW-8005 C30)
1.0Kg, oxidized wax(Sha Suo companies A28)1.4 Kg, Ka Naba waxes(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
(Sinopec Nanjing branch company)6.0Kg, antioxidant 1330(Think this big Chemical Co., Ltd. in Jiangsu)0.4Kg, it is heated to 95 DEG C
It is stirred until homogeneous after melting as oil phase material;
(C2)It is prepared by water-phase material:Weigh morpholine(The happy together safe chemical products Co., Ltd in Beijing Tianjin)1.2 Kg, Tween-80
(Guangzhou De Xu new materials Co., Ltd)3.6 Kg, non-ion fluorin carbon surface active agent(YM-313, the limited public affairs of Shanghai rain wood chemical industry
Department)0.2Kg, sodium benzoate(Zhengzhou Hong Wang Chemical Industry Science Co., Ltd)0.2 Kg, water 72.2Kg are mixed and heated to 90 DEG C and stirred
Mix is uniformly aqueous phase material;
(C3)It is prepared by emulsion:
Will(C1)The oil phase material low whipping speed of preparation is to be added under 1500 revs/min(C2)In the aqueous phase material of preparation;Add
Essence(Vanilla flavored, Shenyang He Tian spices Co., Ltd)0.3Kg, emulsion is contained into porcelain by inner tube under 0.6 MPa
The heat exchanger of ring is homogenizing and loads container after being cooled to 40 DEG C, and it is emulsion-type glazing wax product to be cooled to normal temperature(Ⅳ).
Emulsion-type glazing wax product(Ⅳ)Property:High-temperature stability:It is qualified;Low-temperature stability:It is qualified;Glossiness value added
16.Meet the requirement of GB/T 23437-2009 standards.
The production method of the wax polish of the present invention is can be seen that 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 substance decomposition of decomposable asymmetric choice net generation gas
The short space that is formed after liquid discharge, the constant temperature for forcing air flow through in sweating effort wax layer, increase crystallization and sweating effort
The improvement to sweating process such as stage;Enhance the separating effect of solids fraction and liquid composition and accelerate separating rate, from
And lower-molecular-weight component in raw material is effectively eliminated, sweating process is produced the basic material without low-melting component.
Basic material again with synthetic wax, silicone oil, native paraffin, oil molten type auxiliary agent, emulsifying agent, deionized water and preservative, antioxidant, perfume (or spice)
The emulsion dispersions such as essence are glazing wax product.The method of the present invention has that plant investment is low, 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 (32)
1. a kind of production method of wax polish, including herein below:
A:Pre-emulsification
(A1)It is prepared by oil phase material:Using F-T synthetic products as sweating raw material, heating fusing;W/o type emulsifying agent is added, stirring is equal
It is even, form oil phase material;
(A2)It is prepared by water-phase material:The aqueous solution that decomposable asymmetric choice net is generated to the material of gas under stress heats, and forms aqueous phase
Material;
(A3)It is prepared by emulsion:Will under pressure and stirring condition(A2)Obtained water-phase material adds(A1)Obtained oil phase material
Material, continues stirring 10~30 minutes to form emulsion after all adding;
B:Sweating
(B1)Preparation:Under stress will(A3)Emulsion prepared by process loads sweatbox;
(B2)Crystallization:Wax layer is cooled to by sweating raw material melt drop temperature~+4 DEG C of melt drop temperature with 1.0 DEG C/h~3.0 DEG C/h speed
High temperature constant temperature temperature, and constant temperature is for a period of time;Wax layer is cooled to by sweating raw material drop with 2.0 DEG C/h~4.0 DEG C/h speed again
8 DEG C~15 DEG C of crystallization final temperature below fusing point;
(B3)Cryogenic thermostat:In crystallization final temperature cryogenic thermostat for a period of time, while pressure is reduced to normal pressure;
(B4)Sweating:Heated up with 0.5 DEG C/h~2.5 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)Production emulsification:
(C1)It is prepared by oil phase material:Basic material and the molten type auxiliary agent heating of synthetic wax, silicone oil, native paraffin, oil are melted, stirring is equal
It is even, form oil phase material;
(C2)It is prepared by water-phase material:O/W types emulsifying agent and deionized water are heated, form water-phase material;
(C3)It is prepared by emulsion:Under agitation, will(C1)Obtained oil phase material adds(C2)In obtained water-phase material,
Homogenized again after dispersion and emulsion is glazing wax product.
2. in accordance with the method for claim 1, it is characterised in that step(A2)The material choosing of described decomposable asymmetric choice net generation gas
From carbonic acid, hydrogen peroxide, ammoniacal liquor, chloric acid, hypochlorous acid, water and itself and nontoxic, the non-stimulated smell of catabolite are preferably soluble in
One kind or its composition of carbonic acid, hydrogen peroxide.
3. in accordance with the method for claim 2, it is characterised in that the quality of the aqueous solution of the material of decomposable asymmetric choice net generation gas is dense
Spend for 0.1~5.0%, preferably 0.2~2.0%.
4. in accordance with the method for claim 2, it is characterised in that the material of described decomposable asymmetric choice net generation gas is hydrogen peroxide.
5. in accordance with the method for claim 4, it is characterised in that catalyst is added in hydrogen peroxide, described catalyst is
Inorganic strong alkali, addition of the catalyst in hydrogen peroxide solution are 0.1~20.0 mg/Kg, preferably 0.2~8.0 mg/Kg.
6. in accordance with the method for claim 5, it is characterised in that described inorganic strong alkali is sodium hydroxide and/or hydroxide
Potassium.
7. in accordance with the method for claim 1, it is characterised in that step(A1)Described w/o type emulsifying agent is selected from nonionic
Type surfactant, anionic surfactant, cationic surface active agent, amphoteric surfactant form one group
Material, the freezing point or fusing point of surfactant are less than step(B4)The maximum temperature of sweating.
8. in accordance with the method for claim 7, 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.
9. in accordance with the method for claim 7, it is characterised in that described w/o type emulsifying agent is two or more surface-actives
The compound emulsifying agent that agent is formed, the HLB value of w/o type emulsifying agent is 1~10.
10. in accordance with the method for claim 1, it is characterised in that step(A3)The composition for obtaining emulsion is:Sweating raw material
Mass percent is 60.0%~95.0%, the mass percent of the aqueous solution of the material of decomposable asymmetric choice net generation gas for 4.9%~
30.0%, the mass percent of w/o type emulsifying agent is 0.1%~10.0%.
11. in accordance with the method for claim 7, it is characterised in that the composition of the emulsion is:Sweating material quality percentage
Number is 75.0%~89.0%, and the mass percent of the aqueous solution of the material of decomposable asymmetric choice net generation gas is 10.0%~20.0%, emulsification
The mass percent of agent is 1.0%~5.0%.
12. in accordance with the method for claim 1, it is characterised in that step(A2)、(A3)、(B1)With(B2)During apply
Gauge is the air pressure of 0.5~50.0 atmospheric pressure, with suppress prepared by water-phase material, prepared by emulsion, preparation and
Gas caused by the decomposition and decomposition of decomposable asymmetric choice net material escapes wax layer in crystallization process.
13. in accordance with the method for claim 4, it is characterised in that use nitrogen to protect using during hydrogen peroxide solution.
14. 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.
15. in accordance with the method for claim 1, it is characterised in that step(B2)Described in time of high-temperature constant temperature section be
0.1~6.0 hour.
16. in accordance with the method for claim 1, it is characterised in that step(B3)Described in constant temperature time for 0.1~
5.0h。
17. in accordance with the method for claim 16, it is characterised in that pressure is gradually reduced while cryogenic thermostat to normal
Pressure, rate of pressure reduction is 0.1~150.0 atmospheric pressure/hour.
18. 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.
19. in accordance with the method for claim 1, it is characterised in that step(B4)Described in constant temperature time for 0.1~
10.0 hours.
20. 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.
21. in accordance with the method for claim 14, 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.
22. in accordance with the method for claim 14, it is characterised in that the described wax layer that forces air flow through is used under wax layer
Side reduces air pressure and realized, air pressure keeps normal pressure above wax layer, and the table of -0.2~-0.8 atmospheric pressure is maintained below wax layer
Pressure pressure.
23. according to the method described in claim 1, it is characterised in that step(A1)Positive structure in described F-T synthetic products
The weight content of alkane is more than 80%.
24. in accordance with the method for claim 1, it is characterised in that step(B1)Described sweatbox is sweating ware.
25. in accordance with the method for claim 1, it is characterised in that step in mass(C3)The composition of the wax polish is:
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 types breast
Agent 1.5%~8.0%, oil solubility aids 6.0%~20.9%, surplus are water.
26. in accordance with the method for claim 25, it is characterised in that be additionally added in described wax polish preservative, antioxidant,
One or more of essence is used as additive;The addition of the additive is in mass:Preservative 0.01~0.2%, antioxygen
Agent 0.1~1.0%, essence 0.1~1.0%.
27. according to the method described in claim 1,25 or 26, it is characterised in that described synthetic wax is selected from silicon wax tree fat, oxygen
Change at least one of Tissuemat E.
28. according to the method described in claim 1,25 or 26, 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.
29. according to the method described in claim 1,25 or 26, it is characterised in that described native paraffin be selected from beeswax, Chinese wax,
At least one of Ka Naba waxes, candelila wax, rice bran wax.
30. according to the method described in claim 1,25 or 26, it is characterised in that described 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, dichloromethane, ether, oxirane, 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.
31. according to the method described in claim 1,25 or 26, it is characterised in that described O/W types emulsifying agent 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.
32. in accordance with the method for claim 26, it is characterised in that described preservative is sodium benzoate and/or benzoic acid
Ammonium, described antioxidant are selected from antioxidant BHT, antioxidant 1010, antioxidant 1076, antioxidant CA, antioxidant 1330, antioxidant
3114th, one or more of antioxidant 164, irgasfos 168, antioxidant 264, antioxidant B215, antioxidant B225.
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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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