CN107523350A - A kind of sweating and the method for preparing emery wheel processing wax - Google Patents
A kind of sweating and the method for preparing emery wheel processing wax Download PDFInfo
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- CN107523350A CN107523350A CN201710444667.4A CN201710444667A CN107523350A CN 107523350 A CN107523350 A CN 107523350A CN 201710444667 A CN201710444667 A CN 201710444667A CN 107523350 A CN107523350 A CN 107523350A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/36—Recovery of petroleum waxes from other compositions containing oil in minor proportions, from concentrates or from residues; De-oiling, sweating
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/42—Refining of petroleum waxes
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Abstract
The invention discloses a kind of sweating and the method for preparing emery wheel processing wax.The inventive method is on the basis of common sweating process, oil soluble emulsifying agent and oil-soluble acid are dissolved in sweating raw material as oil phase material, using inorganic salt solution as water-phase material, sweating is carried out after emulsification, short space is formed after being discharged using the bubble and salting liquid of oil-soluble acid and inorganic salt reaction generation, the passage of discharge liquid composition is formed in favor of the quick discharge of liquid composition, while liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow in sweating effort.The inventive method has the advantages that equipment investment is low, preparation process is simple and operating cost is low, safety, energy-conservation and solvent-free pollution, products therefrom can be used as emery wheel releasing agent.
Description
Technical field
The invention belongs to Wax special production technical field, more particularly to a kind of sweating and the side of emery wheel processing wax is prepared
Method.
Background technology
Paraffin is the auxiliary agent commonly used in machining, one of them is just used as various materials as a kind of oil product
Emery wheel releasing agent.
Emery wheel is being designed with manufacturing process, and mould and releasing agent are all essential.Releasing agent is as a kind of coating
With low-down surface energy, when on applied to the matrix material for manufacturing emery wheel production mould, can be formed good heat-staple
Film layer, it and die surface form chemical bonds, abrasive wheel forming part can be allowed quickly to come off easily.Good releasing agent can produce
Stripping result without dirt, thus yield rate is improved, production cost is reduced, shortens the production cycle, ensures the one of wheel face quality
Cause property.Traditional emery wheel releasing agent is generally external application type, i.e., coated in cavity surface.Exterior-applied mold lubricant can be divided into it is inorganic, have
Machine and polymerization species.Conventional inorganic releasing agent mainly has talcum powder, mica powder etc., they the shortcomings that be easily to leave mold deposit and trace
Mark;Organic release agent includes soaps, paraffin etc., they the shortcomings that be also that mold deposit is more, soaps releasing agent also has to corrode to mould to be made
With;Polymerization species have polytetrafluoroethylene (PTFE), silicone oil etc., and stripping result is good, but expensive.
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℃。
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.
In terms of paraffin production technology, conventional separation manufacturing process mainly 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.
Solvent fractionation method is to reach separating-purifying using n-alkane and the different solubility of isoparaffin in a solvent
Purpose, solvent separating technology investment of production equipment is big;Need largely to use solvent in production process, recycling design needs to consume
Substantial amounts of energy;Benzene homologues are usually contained in solvent, environment can be impacted;Solvent is inflammable, 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.So sweating separation method can reduce the distribution of product carbon
Width and can changes normal paraffin content.
Compared with distillating method, because the melting temperature of various hydro carbons is far below boiling temperature, so sweating separation process
Energy consumption be far below separated;Compared with solvent fractionation method, sweating separation process is without using solvent, so sweating separated
Cheng Anquan, energy-conservation 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 fusing point has the soap of thick flaky crystal structure under 40 DEG C~60 DEG C of solid-state
With wax and low melt point paraffin, but for common sweating method, the solids fraction in sweating effort(The wax of higher melt)And liquid
State component(Oil and the wax compared with low melting point)Although being respectively at two kinds of phases of solid and liquid, it also is difficult to be kept completely separate.For
The oil content of final products is set to meet the requirements, generally use extends sweating sessions(Reduce programming rate)Temperature is terminated with sweating is improved
The method of degree, but can so cause production cycle length and product yield decline.
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 production equipment and process aspect(Vertical type square
Shape multipul sections spacer diaphoresis 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 production equipment;CN91206202(It is a kind of
High-efficient sweat pot for paraffin wax)Improved on sweating process, but there are still the shortcoming such as the production cycle is long, product yield is low.
Sweating process is to be currently known unique solvent-free separation method for commercial scale wax product, green advocating
Color low-carbon, today of environmental protection and energy saving, the concern that high-quality emery wheel releasing agent is increasingly subject to people is prepared using sweating process.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of sweating and the method for preparing emery wheel processing wax.Specifically
It is to use sweatbox, on the basis of common sweating process, oil soluble emulsifying agent and oil-soluble acid preferably are dissolved in into hair that ground, which is said,
Using inorganic salt solution as water-phase material, sweating is carried out after emulsification as oil phase material for sweat raw material, using oil-soluble acid with it is inorganic
Short space is formed after the bubble of reactant salt generation and salting liquid discharge, forms the passage of discharge liquid composition in favor of liquid group
The quick discharge divided, while utilize air-flow, to force to separate solids fraction and liquid composition, to increase by wax layer in sweating effort
Strong separating effect simultaneously accelerates separating rate;And increase the constant temperature stage of sweating effort, make this solvent-free separation side of sweating
Method can prepare the higher emery wheel processing wax of carbon narrow distribution, melt viscosity.The inventive method has investment of production equipment
Low, production process is simple and operating cost is low, safety, energy-conservation and the advantages that solvent-free pollution.
The sweating of the present invention and the method for preparing emery wheel processing wax, including herein below:
A:Emulsification
(A1)It is prepared by oil phase material:Using fusing point as 50 DEG C~72 DEG C, the paraffin less than 2.0% is former for sweating in mass for oil content
Material, oil soluble emulsifying agent and oil-soluble acid are added after heating fusing, is stirred, forms oil phase material;
(A2)It is prepared by water-phase material:Inorganic salts are dissolved in water, with or without heating, form water-phase material;
(A3)It is prepared by emulsion:Will(A2)Obtained water-phase material adds under agitation(A1)In obtained oil phase material,
Continue stirring 5~60 minutes, to form emulsion;
B:Sweating
(B1)Preparation:Will(A3)Emulsion prepared by process loads sweatbox;
(B2)Crystallization:First with 5.0 DEG C/h~50.0 DEG C/h speed by emulsion be cooled to+2 DEG C~fusing point of sweating raw material fusing point+
15 DEG C, then it is cooled to 1.0 DEG C/h~4.0 DEG C/h speed 5 DEG C~20 DEG C below sweating raw material fusing point of predetermined temperature;
(B3)Sweating:Heated up with 0.5 DEG C/h~3.0 DEG C/h speed, when wax layer reaches one section of first predetermined temperature and constant temperature
Between, continue to be warming up to second predetermined temperature with 0.5 DEG C/h~2.5 DEG C/h speed and constant temperature stops sweating afterwards for a period of time;
Wax layer is forced air flow through in sweating effort;Continue heating to melt and take out on wax;
(B4)It is refined:Purpose component is emery wheel processing wax product after refined.
In the method for the present invention, described paraffin is that fusing point is 50~72 DEG C, and oil content is less than 2.0%(Quality)It is common
The paraffin of paraffin, preferably fusing point at 54~64 DEG C.
In the method for the present invention, sweating raw material is emulsified in the presence of oil soluble emulsifying agent and oil-soluble acid with water-phase material
After carry out sweating.Step(A1)Described oil soluble emulsifying agent is selected from nonionic surface active agent, anionic surface activity
One or more in agent, cationic surface active agent, amphoteric surfactant.The HLB value of oil soluble emulsifying agent be 1~
10, preferably 3~8;The freezing point or fusing point of the surfactant are less than step(B3)First predetermined temperature of sweating.Institute
The oil soluble emulsifying agent stated is preferably the compound emulsifying agent that two or more surfactants are formed.
Wherein, it is stearic to be selected from sorbitan monooleate, anhydrous sorbitol list for described nonionic surface active agent
Acid esters, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol list are stearic
One group of material that acid esters, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester are formed;It is cloudy
Ionic surfactant is selected from fatty alcohol sulfate monoethanolamine salt, pareth sulfate, oleamide yl carboxylic acid
Sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurates, sodium butylnaphthalenesulfonate, Disodium sulfosuccinate, suitable succinate monoester
One group of material that sodium sulfonate is formed.Described cationic surface active agent is selected from benzyl quaternary ammonium salt, dodecyl dimethyl benzyl
Ammonium chloride, DTAC, cetyl trimethylammonium bromide, OTAC, three second
One group of material that acid amides oleate is formed;Amphoteric surfactant is selected from empgen BB, dodecyl dimethyl oxygen
Change ammonium, aliphatic group imidazolidine derivatives, alkyl imidazoline derivatives, derivative of fatty acid, amphoteric modified epoxy ethane to add
The one group of material formed into thing.
In the method for the present invention, step(A1)Described oil-soluble acid is soluble in sweating raw material and energy and step(A2)Institute
The organic acid for the inorganic salt reaction generation gas stated, selected from positive tenth of the twelve Earthly Branches acid, n-capric acid, positive undecanoic acid, laurate, positive tridecanoic acid, meat
Myristic acid, positive pentadecanoic acid, palmitic acid, pearly-lustre resin acid, stearic acid, positive nonadecanoic acid, arachidic acid, positive heneicosoic acid, behenic acid, positive two
Tridecanoic acid, lignoceric acid, positive neocerotic acid, cerinic acid, positive carboceric acid, montanic acid, positive motanic acid, melissic acid, positive myricinic acid,
One group of material that lacceroic acid, leaf lice acid, linoleic acid, palmitoleic acid, oleic acid, erucic acid, selacholeic acid are formed.Preferably without special gas
Taste, nonhazardous, it is easy to get and price is low, fusing point is less than the organic acid of first predetermined temperature of sweating, including linoleic acid, palm oil
Acid, oleic acid, erucic acid, selacholeic acid, n-capric acid, positive undecanoic acid, laurate, positive tridecanoic acid, myristic acid, the one of positive pentadecanoic acid composition
Group material.
In the method for the present invention, step(A2)Described inorganic salts are can be with step(A1)Described oil-soluble acid reaction
Generate the water-soluble inorganic salt of gas.The inorganic salts are in carbonate, bicarbonate, sulphite, bisulfites
It is one or more of;Preferably cheap, wide material sources, itself and reaction product are nontoxic, the sodium carbonate, the carbon that have no irritating odor
One kind in the bicarbonates such as one kind and its mixture and/or sodium acid carbonate, saleratus in the carbonate such as sour potassium and its
One group of material that mixture is formed.The concentration of described inorganic salt solution(Quality %, similarly hereinafter)For 0.1%~10.0%, preferably
For 0.5%~5.0%.
In the method for the present invention, step(A3)The composition of resulting emulsion is:Sweating raw material 55.0%~90.0%, aqueous phase
Material 9.8%~29.0%, oil soluble emulsifying agent 0.1%~6.0%, oil-soluble acid 0.1%~10.0%.Emulsion preferably constitutes
For:Sweating raw material 66.0%~83.0%, water-phase material 15.0%~25.0%, oil soluble emulsifying agent 1.8%~4.0%, oil-soluble acid
0.2%~5.0%.
Described emulsification uses the ordinary skill in the art.The condition of emulsification is:At 70 DEG C~98 DEG C, with 50~5000
Rev/min mixing speed mix 5~60 minutes;Preferably at 75 DEG C~95 DEG C, with 100~1000 revs/min of stirring
Speed mixes 10~30 minutes.
In the method for the present invention, step(B2)During preferred hair is first cooled to 5.0 DEG C/h~30.0 DEG C/h speed
In the range of+8 DEG C of+3 DEG C~fusing point of sweat raw material fusing point, then with 1.5 DEG C/h~3.5 DEG C/h speed be cooled to sweating raw material fusing point with
Lower 8 DEG C~15 DEG C of predetermined temperature.
In the method for the present invention, the preferred sweating ware of described sweatbox, and in wax layer pressue device added above and/or
Increase vacuum plant below wax layer, in step(B3)During make wax layer up and down form pressure differential.Described pressure gas
Stream is used by wax layer increases pressure above wax layer(Air pressure)And/or pressure is reduced below wax layer(Air pressure), make in wax layer,
Lower section(Side)Pressure differential is formed to realize.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 big
Air pressure, to force air flow through wax layer.
In the method for the present invention, step(B3)Described in heating rate before first predetermined temperature be preferably 1.0
DEG C/h~2.5 DEG C/h, it is preferably 0.5 DEG C/h~2.0 DEG C/h after first predetermined temperature.First described predetermined temperature
For purpose component fusing point -5 DEG C~purpose component fusing point;Second described predetermined temperature is purpose component fusing point~purpose component
+ 5 DEG C of fusing point.It is described be warming up to predetermined temperature after, the increase constant temperature stage can make solids fraction and liquid composition separate and more fill
Point, the time in constant temperature stage is 0.1~10.0 hour, preferably 1.0~8.0 hours, most preferably 2.0~5.0 hours.
In the method for the present invention, the programming rate and cooling rate of said wax layer, air bath, water-bath, oil bath can be passed through
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer is controlled to heat up using water-bath or oil bath mode
When speed and rate of temperature fall, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, the circulatory system
With program cooling/heating function, the circulatory system adds the material such as water or conduction oil as circulatory mediator;Coil pipe is soaked after charging
Not and be fixed in wax layer, can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature.
In the method for the present invention, step(B3)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(B3)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(B3)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(B4)Described purpose component refers under two waxes, i.e. step(B3)In sweating effort
First time constant temperature terminates product under the wax collected into second of constant temperature terminal procedure.
When releasing agent is applied on the matrix material of manufacture emery wheel production mould, good heat-staple film layer can be formed, can
To allow abrasive wheel forming part quickly to come off easily.Good releasing agent can produce the stripping result without dirt, thus improve yield rate, drop
Low production cost, shorten the production cycle, ensure the uniformity of wheel face quality.
The releasing agent used in emery wheel processing at present is substantially common paraffin.Research shows, presently commercially available commodity
Paraffin usually contains alkane more than 20 carbon numbers, and carbon number distribution is wider, and oil content is generally the mass %'s of 0.8 mass %~2.0
Higher level.Result of the test shows, when the common paraffin that carbon number distribution is wide, oil content is high is used as into the releasing agent of emery wheel processing,
When cavity surface is coated in emery wheel process, there is that uniformity is bad, keeps that demoulding time is not long, has to product appearance
The deficiencies of adverse effect.Because the crystallization of common paraffin is thicker, and it is inadequate with mould adhesion strength, it is easily transferred to emery wheel
On, typically 2~3 production cycles can only be run by playing a wax, influence production efficiency;The product made of waxing for the first time speckles with more
The wax of amount, hardness is partially soft after emery wheel product hardens out, plays the wax of excess or even can cause film.These are all common paraffinized
Caused by learning composition, therefore common paraffin needs to reduce the carbon dispersion of distribution and oil content and properly increases isomery hydrocarbon content, just changes
It is apt to its performance, improves emery wheel product quality and production efficiency.
Sweating separation method is separated using the different property of various component fusing points, but solid in sweating effort
State component is difficult to be kept completely separate with liquid composition, and this is due to wax and oily two kinds of components are all nonpolar hydrocarbon molecules, molecule
Intermolecular forces are larger;The wax crystallization of solid-state forms capillary pipe structure simultaneously, has stronger suction-operated to oil, this results in only leaning on
Wax and oil are difficult to be kept completely separate in the common sweating effort of gravity natural separation.Generally use extends sweating sessions, improves sweating
The methods of final temperature, makes the oil content of final products meet the requirements, but this can cause the production cycle to extend again, wax product is received
Rate reduces.These have impact on the extensive use of sweating separation method.
The present invention is in order to prepare emery wheel processing wax, by associating for the composition to common paraffin and performance, it is determined that
Common paraffin carbon wider distribution, oil content are higher, relatively low isomery hydrocarbon content is the reason for influenceing emery wheel quality, by using sweating
Method reduces oil content and the carbon dispersion of distribution, improves isomery hydrocarbon content.By the further investigation to common sweating effort, for solid
State component is difficult to separate reason with liquid composition, is used in sweating effort and forces air flow through wax layer, and in sweating effort
Increase the constant temperature stage, sweating raw material is further preferably mixed into oil-soluble acid and oil soluble emulsifying agent W/O is made with inorganic salt solution again
Sweating is carried out after type emulsion, these measures are effectively improved the performance that product is used as emery wheel processing wax.
The present invention is by the further investigation to common sweating effort, the original that is difficult to separate for solids fraction and liquid composition
Cause, the method for carrying out liquid composition by wax layer using air-flow in sweating effort force solids fraction and point of liquid composition
From enhancing separating effect and accelerate separating rate;Inorganic salt solution is uniformly divided in the form of fine particle in emulsion simultaneously
Cloth is in raw material wax layer;Because the acidity of selected oil-soluble acid is weaker and is respectively at inorganic salts in oil phase and aqueous phase,
The reaction for generating gas is carried out with slower speed;In the time that sweating raw material terminates after being cooled to below fusing point to sweating effort
Wax layer is in softer solid state, and oil-soluble acid gradually occurs to chemically react and discharges gas with inorganic salts during this,
Equally distributed micro-bubble is formed in raw material wax layer;On the one hand it can be carried by wax layer using air-flow in sweating effort
Go out inorganic salt solution to form short space in wax layer, space caused by these short spaces and bubble is easy in sweating effort
In forming some tiny passages in wax layer, be advantageous to the discharge of liquid composition in sweating effort;On the other hand separation is forced
Solids fraction and liquid composition, so as to enhance separating effect and accelerate separating rate.Selected oil-soluble acid and surface-active
The fusing point of agent is less than first predetermined temperature of sweating, and all belongs to polar molecule, poor with the intermiscibility of sweating raw material, can be in sweating
During discharged with liquid composition.Being aided with the constant temperature stage of sweating effort again makes solids fraction and liquid composition separate and more fill
Grade method so that the excellent emery wheel processing wax of sweating process more efficiently processability.
This have the advantage that:By the side for carrying out liquid composition by wax layer using air-flow in sweating effort
Method enhances the separating effect of solids fraction and liquid composition and accelerates separating rate;Utilize oil-soluble acid and inorganic salts simultaneously
The space and inorganic salt solution that reaction generation micro-bubble is formed produce short space after discharging and form some tiny passages,
It is also beneficial to the quick discharge of liquid composition;And increase the processes such as the constant temperature stage of sweating effort, so as to more efficiently prepare
High-quality emery wheel processing wax.The present invention method have plant investment is low, production process is simple and operating cost is low, it is safe,
The advantages that energy-conservation and solvent-free pollution environment.
Embodiment
The present invention is by being sweating raw material from suitable common paraffin, 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 connects and depressurize in sweating ware bottom
Surge tank and vavuum pump;The heating of sweating raw material is melted and is preferably added to oil-soluble acid and emulsifying agent, after being emulsified with inorganic salt solution
Load sweating ware;Wax layer heating-cooling speed is controlled with water-bath;When wax layer heating reaches one section of first preset temperature and constant temperature
Between, continue to be warming up to second preset temperature and constant temperature stops sweating effort afterwards for a period of time;In sweating effort, start compression
Machine is with wax layer malleation formed above, and/or starts vavuum pump with wax layer negative pressure formed below, to force air flow through wax
Layer;Purpose component is emery wheel processing wax product after refined.
The method that 1-4 illustrates the sweating of the present invention and prepares emery wheel processing wax by the following examples.Such as without spy
Not Zhu Ming, it is mass percent to be related to % below, and the pressure is gauge pressure.
Embodiment 1
The present embodiment includes:A:Emulsification and B:Sweating two parts.
A:Emulsification
This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three steps.
(A1)It is prepared by oil phase material:Take 60#Semi-refined wax(Dalian branch company of CNPC, 60.8 DEG C of fusing point, oil content
1.62%, isoparaffin content 37.25%)70.0Kg, 2.0Kg anhydrous sorbitol monostearates are added after being heated to 78 DEG C of fusings
Ester, 0.9Kg diethylene glycols monolaurate, 0.5Kg empgen BBs and 2.5Kg linoleic acid, stir.
(A2)It is prepared by water-phase material:Compound concentration is 3.7% KHCO3Solution, take 24.1Kg and be heated to 82 DEG C.
(A3)It is prepared by emulsion:Stirred with 450 revs/min of speed(A1)Oil phase material prepared by process, and will(A2)
Water-phase material prepared by process is added in oil phase material, is continued to stir 25min, is formed water-in-oil type emulsion.
B:Sweating
This part includes(B1)Preparation,(B2)Crystallization,(B3)Heating-constant temperature-heating-constant temperature sweating,(B4)Refined four
Individual step.
(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;Using water as
Heat medium;Start the heating function of the circulatory system, recirculated water is warming up to 65 DEG C.Pad water below sweating ware ware plate.Will(A3)
Emulsion prepared by process adds sweating ware.The sealing system of sweating ware is installed.
(B2)Crystallization
Emulsion stands the refrigerating function of the startup circulatory system after 1.0h, and control wax layer temperature is with 3.0 DEG C/h rate of temperature fall
50.0 DEG C are down to so that wax layer crystallizes to form solid;Close the refrigerating function of the circulatory system.
(B3)Heating-constant temperature-heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank(Ⅰ)To receive under wax;Start compressor and keep pressurization slow
Rush the stable holding normal pressure below 1.4~1.6 atmospheric pressure, sweating ware ware plate of pressure inside the tank;Start circulation system function,
Wax layer temperature is increased to 57.5 DEG C and constant temperature 3.5 hours with 2.5 DEG C/h heating rate so that solids fraction in wax layer with
Liquid composition is sufficiently separated.Stop compressor.
The outlet of sweating ware is changed to connect crude product storage tank(Ⅰ)To receive under two waxes, both crude products(Ⅰ);Start vavuum pump simultaneously
The stable air pressure above -0.3~-0.5 atmospheric pressure, wax layer of pressure-reducing cushioning pressure inside the tank is kept to keep normal pressure;With 1.0 DEG C/h's
Heating rate makes wax layer temperature be increased to 62.5 DEG C and constant temperature 4.0 hours so that solids fraction and liquid composition in wax layer are abundant
Separation;Stop vavuum pump, terminate sweating effort.
The outlet of sweating ware is changed to connect intermediate storage tank(Ⅱ);Continue heat cycles water and be warming up to 80 DEG C with fusing taking-up wax
On.
(B4)It is refined
Crude product(Ⅰ)It is emery wheel processing wax product after clay-filtered(Ⅰ).
Emery wheel processing wax product(Ⅰ)Property:60.5 DEG C of fusing point;Oil content 0.47%, isoparaffin content 49.26%.Sand
Take turns processing wax product(Ⅰ)Yield is 53.3%(Relative to raw material 60#Semi-refined wax).
Embodiment 2
The present embodiment includes:A:Emulsification and B:Sweating two parts.
A:Emulsification
This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three steps.
(A1)It is prepared by oil phase material:Take 60#Semi-refined wax(With embodiment 1)82.0Kg, added after being heated to 90 DEG C of fusings
1.5Kg sorbitan monooleates, 0.5Kg tetraethylene glycols monostearate, 0.2Kg sodium alkyl benzene sulfonates and 1.0Kg are just
Tridecanoic acid, stir.
(A2)It is prepared by water-phase material:Compound concentration is 1.6% Na2CO3Solution, take 14.8Kg and be heated to 94 DEG C.
(A3)It is prepared by emulsion:Stirred with 900 revs/min of speed(A1)Oil phase material prepared by process, and will(A2)
Water-phase material prepared by process is added in oil phase material, is continued to stir 10min, is formed water-in-oil type emulsion.
B:Sweating
With embodiment 1.
Emery wheel processing wax product manufactured in the present embodiment(Ⅱ)Property:60.3 DEG C of fusing point;Oil content 0.45%, isomeric alkane
Hydrocarbon content 48.69%.Emery wheel processing wax product(Ⅱ)Yield is 52.1%(Relative to raw material 60#Semi-refined wax).
Embodiment 3
The present embodiment includes:A:Emulsification and B:Sweating two parts.
A:Emulsification
This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three steps.
(A1)It is prepared by oil phase material:Take 60#Semi-refined wax(With embodiment 1)74.0Kg, added after being heated to 82 DEG C of fusings
2.1Kg sorbitan monostearates, 0.6Kg polyoxyethylene fatty acid esters, 0.3Kg triacetamides oleate and 2.0Kg
Oleic acid, stir.
(A2)It is prepared by water-phase material:Compound concentration is 1.8% Na2CO3Solution, take 21.0Kg and be heated to 85 DEG C.
(A3)It is prepared by emulsion:Stirred with 650 revs/min of speed(A1)Oil phase material prepared by process, and will(A2)
Water-phase material prepared by process is added in oil phase material, is continued to stir 20min, is formed water-in-oil type emulsion.
B:Sweating
With embodiment 1.
Emery wheel processing wax product manufactured in the present embodiment(Ⅲ)Property:60.6 DEG C of fusing point;Oil content 0.42%, isomeric alkane
Hydrocarbon content 50.07%.Emery wheel processing wax product(Ⅲ)Yield is 52.8%(Relative to raw material 60#Semi-refined wax).
Embodiment 4
The present embodiment includes:A:Emulsification and B:Sweating two parts.
A:Emulsification
This part includes(A1)Oil phase material preparation,(A2)Water-phase material preparation,(A3)Emulsion prepares three steps.
(A1)It is prepared by oil phase material:Take 60#Semi-refined wax(With embodiment 1)78.0Kg, added after being heated to 86 DEG C of fusings
1.8Kg sorbitan monooleates, 0.3Kg diethylene glycols monolaurate, 0.5Kg sorbitan mono-laurates and
1.5Kg positive undecanoic acid, stirs.
(A2)It is prepared by water-phase material:Compound concentration is 3.1% K2CO3Solution, take 17.9Kg and be heated to 90 DEG C.
(A3)It is prepared by emulsion:Stirred with 300 revs/min of speed(A1)Oil phase material prepared by process, and will(A2)
Water-phase material prepared by process is added in oil phase material, is continued to stir 30min, is formed water-in-oil type emulsion.
B:Sweating
With embodiment 1.
Emery wheel processing wax product manufactured in the present embodiment(Ⅳ)Property:60.8 DEG C of fusing point;Oil content 0.40%, isomeric alkane
Hydrocarbon content 48.87%.Emery wheel processing wax product(Ⅳ)Yield is 53.6%(Relative to raw material 60#Semi-refined wax).
Comparative example 1
With 60#Semi-refined wax(With embodiment 1)For raw material, sweating ware is added after heating fusing;Wax is made with 2.0 DEG C/h rate of temperature fall
Layer temperature drops to 50.0 DEG C;Wax layer temperature is set to be increased to 57.5 DEG C with 2.0 DEG C/h heating rate again;Then with 1.0 DEG C/h
Heating rate wax layer temperature is increased to 62.5 DEG C;Make under two waxes collected between 57.5 DEG C~62.5 DEG C after clay-filtered
For emery wheel processing wax product(Ⅴ).
Emery wheel processing wax product(Ⅴ)Property:61.5 DEG C of fusing point;Oil content 0.88%, isoparaffin content 41.63%.Receive
Rate is 41.5%(Relative to raw material 60#Semi-refined wax).
The product and 60 prepared with embodiment 1-4, comparative example 1#Semi-refined wax(Property is the same as embodiment 1)It is stripped as emery wheel
Agent, emery wheel raw material are liquid phenolic resin(Wetting agent)And powdered phenol-formaldehyde resin, liquid powder is than 1:3, sand is carried out using cold-press process
Pilot production is taken turns, as a result see the table below.
Product(Ⅰ) | Product(Ⅱ) | Product(Ⅲ) | Product(Ⅳ) | Product(Ⅴ) | 60#Semi-refined wax | |
Number of run | 6 | 7 | 7 | 7 | 4 | 3 |
Yield rate, % | 98 | 99 | 98 | 99 | 94 | 92 |
Above-mentioned result of the test shows that the product prepared using embodiment 1-4 is used as emery wheel releasing agent, production run number and production
Product yield rate is substantially improved;And comparative example properties of product improve unobvious.
The method that can be seen that the sweating of the present invention by embodiment 1-4 and prepare emery wheel processing wax, added by increase
The improvement to sweatbox such as pressure and/or vacuum facility;By the way that sweating raw material is mixed into oil-soluble acid and given birth to inorganic salt reaction
Into gas formed in wax layer micro-bubble and salting liquid discharge after formed short space, air-flow is forced in sweating effort
Pass through the improvement to sweating process such as wax layer, the constant temperature stage for increasing sweating effort;Enhance solids fraction and liquid composition
Separating effect simultaneously accelerates separating rate.With comparative example 1(Conventional sweating)Compare, embodiment 1-4 is very fast in cooling, heating rate
In the case of, the oil content of product have dropped 0.41 percentage point, 0.43 percentage point, 0.46 percentage point and 0.48 respectively
Percentage point;Isoparaffin content adds 7.63 percentage points, 7.06 percentage points, 8.44 percentage points and 7.24 hundred respectively
Branch;Yield has been respectively increased 11.8 percentage points, 10.6 percentage points, 11.3 percentage points and 12.1 percentage points), make hair
Sweat technique more efficiently prepares high-quality emery wheel processing wax product(In the case where number of run increases by 2~3 times, yield rate
Improve 4~5 percentage points).
Claims (22)
1. a kind of sweating and the method for preparing emery wheel processing wax, including herein below:
A:Emulsification
(A1)It is prepared by oil phase material:Using fusing point as 50 DEG C~72 DEG C, the paraffin less than 2.0% is former for sweating in mass for oil content
Material, oil soluble emulsifying agent and oil-soluble acid are added after heating fusing, is stirred, forms oil phase material;
(A2)It is prepared by water-phase material:Inorganic salts are dissolved in water, form water-phase material;
(A3)It is prepared by emulsion:Will(A2)Obtained water-phase material adds under agitation(A1)In obtained oil phase material,
Continue stirring 5~60 minutes, to form emulsion;
B:Sweating
(B1)Preparation:Will(A3)Emulsion prepared by process loads sweatbox;
(B2)Crystallization:Emulsion is cooled to by sweating raw material+2 DEG C~fusing point+15 of fusing point with 5.0 DEG C/h~50.0 DEG C/h speed
DEG C, then it is cooled to 1.0 DEG C/h~4.0 DEG C/h speed 5 DEG C~20 DEG C below sweating raw material fusing point of predetermined temperature;
(B3)Sweating:Heated up with 0.5 DEG C/h~3.0 DEG C/h speed, when wax layer reaches one section of first predetermined temperature and constant temperature
Between, continue to be warming up to second predetermined temperature with 0.5 DEG C/h~2.5 DEG C/h speed and constant temperature stops sweating afterwards for a period of time;
Wax layer is forced air flow through in sweating effort;Continue heating to melt and take out on wax;
(B4)It is refined:Purpose component is emery wheel processing wax product after refined.
2. in accordance with the method for claim 1, it is characterised in that step(A1)Described oil soluble emulsifying agent is selected from nonionic
Type surfactant, anionic surfactant, cationic surface active agent, amphoteric surfactant form one group
Material, the HLB value of oil soluble emulsifying agent is 1~10, and the freezing point or fusing point of the surfactant are less than step(B3)Sweating
First predetermined temperature.
3. in accordance with the method for claim 2, it is characterised in that described nonionic surface active agent is selected from Sorbitan
Alcohol monoleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, Sorbitan
Alcohol monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, polyoxy second
One group of material that alkene fatty acid ester is formed;Described anionic surfactant be selected from fatty alcohol sulfate monoethanolamine salt,
Pareth sulfate, oleamide yl carboxylic acid sodium, sodium alkyl benzene sulfonate, N- methyl oleoyl taurates, dibutyl naphthalene
Sodium sulfonate, Disodium sulfosuccinate, the one group of material formed along succinate monoester sodium sulfonate;Described cationic surfactant
Agent is selected from benzyl quaternary ammonium salt, dodecyl benzyl dimethyl ammonium chloride, DTAC, cetyl trimethyl
One group of material that ammonium bromide, OTAC, triacetamide oleate are formed;Described amphoteric surfactants
Agent is selected from empgen BB, OA-12, aliphatic group imidazolidine derivatives, alkyl imidazoline and derived
One group of material that thing, derivative of fatty acid, amphoteric modified epoxy ethane additive product are formed.
4. in accordance with the method for claim 2, it is characterised in that described oil soluble emulsifying agent is two or more surface-actives
The compound emulsifying agent that agent is formed.
5. in accordance with the method for claim 1, it is characterised in that step(A1)Described oil-soluble acid is former to dissolve in sweating
Expect and can be with(A2)The organic acid of described inorganic salt reaction generation gas.
6. in accordance with the method for claim 5, it is characterised in that described organic acid is selected from positive tenth of the twelve Earthly Branches acid, n-capric acid, positive 11
Acid, laurate, positive tridecanoic acid, myristic acid, positive pentadecanoic acid, palmitic acid, pearly-lustre resin acid, stearic acid, positive nonadecanoic acid, arachidic acid,
Positive heneicosoic acid, behenic acid, positive tricosanic acid, lignoceric acid, positive neocerotic acid, cerinic acid, positive carboceric acid, montanic acid, positive 20
Nine acid, melissic acid, positive myricinic acid, lacceroic acid, leaf lice acid, linoleic acid, palmitoleic acid, oleic acid, erucic acid, selacholeic acid are formed
One group of material.
7. in accordance with the method for claim 6, it is characterised in that described oil-soluble acid is selected from linoleic acid, palmitoleic acid, oil
At least one of acid, erucic acid, selacholeic acid, n-capric acid, positive undecanoic acid, laurate, positive tridecanoic acid, myristic acid, positive pentadecanoic acid.
8. in accordance with the method for claim 1, it is characterised in that step(A2)Described inorganic salts are selected from carbonate, carbonic acid
At least one of hydrogen salt, sulphite, bisulfites, metal sulfide.
9. in accordance with the method for claim 8, it is characterised in that described inorganic salts are selected from sodium carbonate, potassium carbonate, bicarbonate
At least one of sodium, saleratus.
10. in accordance with the method for claim 1, it is characterised in that the mass concentration of inorganic salts is in described water-phase material
0.1%~10.0%.
11. in accordance with the method for claim 1, it is characterised in that step(A3)Described in mixing speed be 50~1500
Rev/min.
12. in accordance with the method for claim 1, it is characterised in that step(A3)The composition of obtained emulsion is:Sweating is former
It is 55.0%~90.0% to expect mass percent, and the mass percent of water-phase material is 9.8%~29.0%, the matter of oil soluble emulsifying agent
It is 0.1%~6.0% to measure percentage, and the mass percent of oil-soluble acid is 0.1%~10.0%.
13. in accordance with the method for claim 12, it is characterised in that step(A3)The composition of obtained emulsion is:Sweating
Material quality percentage is 66.0%~83.0%, and the mass percent of water-phase material is 15.0%~25.0%, oil soluble emulsifying agent
Mass percent be 1.8%~4.0%, the mass percent of oil-soluble acid is 0.2%~5.0%.
14. in accordance with the method for claim 1, it is characterised in that step(B3)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(B3)Described in first predetermined temperature be mesh
- 5 DEG C of component fusing point~purpose component fusing point;Second described predetermined temperature is purpose component fusing point~purpose component fusing point
+5℃。
16. in accordance with the method for claim 1, it is characterised in that step(B3)Described in constant temperature time for 0.1~
10.0 hours.
17. in accordance with the method for claim 1, it is characterised in that step(B3)Described in the wax layer that forces air flow through exist
Sweating is implemented initial stage.
18. 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.
19. 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.
20. in accordance with the method for claim 1, it is characterised in that step(B4)Described in purpose component refer under two waxes,
That is step(B3)First time constant temperature terminates product under the wax collected into second of constant temperature terminal procedure in sweating effort.
21. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
22. in accordance with the method for claim 1, it is characterised in that the fusing point of described sweating starting paraffin is 54 DEG C~64
℃。
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Cited By (1)
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CN114540101A (en) * | 2022-01-24 | 2022-05-27 | 华中光电技术研究所(中国船舶重工集团公司第七一七研究所) | Mold release agent for processing high-precision resin grinding wheel and use method thereof |
Citations (2)
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US5015357A (en) * | 1988-01-04 | 1991-05-14 | Amoco Corporation | Wax sweating |
CN1218094A (en) * | 1998-09-14 | 1999-06-02 | 薛世峰 | Preparation of fundamental oil of lubricant oil |
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2017
- 2017-06-13 CN CN201710444667.4A patent/CN107523350B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5015357A (en) * | 1988-01-04 | 1991-05-14 | Amoco Corporation | Wax sweating |
CN1218094A (en) * | 1998-09-14 | 1999-06-02 | 薛世峰 | Preparation of fundamental oil of lubricant oil |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114540101A (en) * | 2022-01-24 | 2022-05-27 | 华中光电技术研究所(中国船舶重工集团公司第七一七研究所) | Mold release agent for processing high-precision resin grinding wheel and use method thereof |
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