CN107513306A - The production method of ink wax - Google Patents
The production method of ink wax Download PDFInfo
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- CN107513306A CN107513306A CN201610432982.0A CN201610432982A CN107513306A CN 107513306 A CN107513306 A CN 107513306A CN 201610432982 A CN201610432982 A CN 201610432982A CN 107513306 A CN107513306 A CN 107513306A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/12—Printing inks based on waxes or bitumen
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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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- 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
- C10G73/44—Refining of petroleum waxes in the presence of hydrogen or hydrogen-generating compounds
Abstract
The invention discloses a kind of production method of ink wax.This method carries out hydro-conversion using F T synthetic products as raw material under catalyst action；Hydrogenation products prepare the component of suitable boiling range as sweating raw material through distillation；Again purpose product is produced through emulsification, sweating.The inventive method is on the basis of common sweating process, liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow in sweating effort, preferably sweating raw material and water or salting liquid are emulsified simultaneously, are also beneficial to the quick discharge of liquid composition.The inventive method has the advantages that equipment investment is low, preparation process is simple and operating cost is low, safe and solvent-free pollution；Products therefrom melting range is narrow, can be used as ink wax.
Description
Technical field
The invention belongs to Wax special production technical field, more particularly to a kind of production method of ink wax, in particular for the production method of the wax of hot melt printing ink.
Background technology
Ink is the important materials for printing, and it is shown pattern, word on stock by printing.Ink is widely used in the various printings such as books and periodicals, packing and decorating, building decoration and electronic circuit sheet material.As social demand increases, ink kind and yield also respective extension and growth.
Hot melt printing ink, or phase change ink or cold-set ink, it is at ambient temperature solid-state, is in a liquid state under the higher temperature of inkjet-printing device operation.When inkjet-printing device is run, liquid ink droplets are ejected, and when the surface of the direct or indirect contact history matrix of ink droplet, they solidify rapidly so as to form predetermined solidification ink droplet pattern.Hot melt printing ink has the advantages that to solidify the quality for improving round dot when ink droplet is contacting with matrix when being solid during storage and transport etc., can eliminate the reliability, the printing that improve inkjet printing due to spout blockage problem caused by the injection of liquid ink immediately, therefore is used widely.
Hot melt printing ink generally includes colouring agent and carrier, such as U.S.P. 3,653,932nd, U.S.P. 4,851,045, U.S.P. 5,372,852nd, in the formula of the patent introduction such as DE 4205636AL, CN200610163170.7, CN200810146002.6, CN201210025537.4, carrier material can include pertroleum wax（Such as paraffin, microwax）And synthetic wax（Such as Tissuemat E）And other wax materials.The carrier of narrow carbon number distribution is advantageous to improve print quality.
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 atoleine, soap manufacturing paraffin, paraffin and microwax.Paraffin typically contains C20~C50The component such as n-alkane, isoparaffin and a small amount of cycloalkane, usual fusing point is 50 DEG C~74 DEG C；Microwax is typically by C30~C60Isoparaffin and a small amount of n-alkane, cycloalkane composition, usual melt drop temperature be 65 DEG C~92 DEG C, there is the needle-like crystal structure more tiny than paraffin under solid-state.Pertroleum wax is the hydrocarbon mixture of the n-alkane, isoparaffin, cycloalkane of a variety of carbon numbers etc., and its carbon number distribution is wider.
Fischer-Tropsch（F-T）Synthetic technology is nineteen twenty-three invention, realizes industrialization in Germany within 1936.F-T synthetic technologys mainly include high temperature synthesis techniques and low temperature synthesis technique.Since nineteen nineties, F-T synthesis techniques and catalyst all achieve breakthrough progress, and F-T sinteticses become increasingly abundant.F-T sinteticses contain alkene and oxygenatedchemicals and the non-constant width of carbon number distribution.
Conventional Wax separation means have 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 width of product carbon distribution, such as CN201410217632.3 can effectively be reduced by reducing the boiling range of distillation（A kind of method for improving Fischer-Tropsch wax pour point）Introduce and raw material is removed into low-boiling point material under high temperature high vacuum, then further distillation is refined under XHV, to prepare high melting-point wax product.Still-process needs raw material being heated to more than boiling point, consumes substantial amounts of energy, while the boiling point of hydro carbons of the fusing point more than 70 DEG C is at 500 DEG C（Normal pressure）More than, efficiency is greatly reduced when being separated using distillation.
Solvent separation is the purpose that reaches separation using the different solubility of the alkane of different structure and molecular weight in a solvent, such as CN200410043806.5（A kind of method for splitting Tissuemat E）、CN201110351185.7（A kind of method of separating polyethylene byproduct polyethylene wax）.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 raw material.The molecular weight of various components Bu Tong can all make its fusing point different with structure.When being all n-alkane, the fusing point of the larger n-alkane of molecular weight 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 will be less than n-alkane, and isomery degree more high-melting-point is lower.So the width and can that sweating separation method can reduce the distribution of product carbon improves normal paraffin content.
Compared with distillating method, because the melting temperature of various hydro carbons is far below boiling temperature, so the energy consumption of sweating effort is far below distillation；Compared with solvent separates, sweating effort is without using solvent, so sweating effort is safe, saves and on environment without influence, and sweating method can reduce the width and can raising normal paraffin content of product carbon distribution.
Common sweating process mainly includes the following steps that：（1）Preparation：Pad water（Sweatbox ware plate lower space is full of with water）After feed（Load sweatbox when raw material is heated to more than fusing point being in a liquid state）；（2）Crystallization：Raw material is progressively cooled to below its fusing point 10~20 DEG C with the rate of temperature fall no more than 4 DEG C/h.In cooling procedure, various components are crystallized to form solid successively by the order of fusing point from high to low；（3）Sweating：After wax layer temperature reaches default cooling final temperature, pad water is bled off；Raw material is slowly heated to default sweating final temperature again.In sweating effort, various components are successively fused into liquid by the order of fusing point from low to high and flowed out（Under wax）, the wax layer residue that finally obtains（On wax）It is exactly high-melting-point, the wax of low 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, as crude product）, through clay-filtered（Predetermined temperature is warming up to after crude product is melted, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the scheduled time）Afterwards, reshaping, packaging are purpose product.
Common sweating process can produce soap manufacturing paraffin and low melt point paraffin with thick flaky crystal structure of the fusing point at 40 DEG C~60 DEG C, be not suitable for producing wax of the fusing point at 70 DEG C or so.Experiment shows, common sweating process produces fusing point in 70 DEG C or so of wax product, the carbon dispersion of distribution and normal paraffin content on sweating later stage wax is unrelated with yield, the carbon dispersion of distribution i.e. on wax does not decline with the decline of yield, normal paraffin content is not also improved with the decline of yield, and report of the fusing point in 70 DEG C or so of ink wax product is produced with sweating process so so far there are no.
Sweating process is intermittently operated, and product yield is relatively low, the production cycle is longer, but sweating process have the advantages that small investment, production process are simple, operating cost is low, production process is safe, energy-conservation and it is environmentally safe, still have at present part producer 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 square 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（A kind of high-efficient sweat pot for paraffin wax）Improved on sweating process, but these improvement can not still produce ink wax product of the fusing point at 70 DEG C or so.
Sweating process is to be currently known unique solvent-free separation method for commercial scale wax product, and in promotion green low-carbon, today of environmental protection and energy saving, the demand that ink wax product of the fusing point more than 70 DEG C is produced using sweating process is more urgent.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of production method of ink wax, including is hydrogenated with, distills, emulsifying, the part of sweating four.Specifically using suitable F-T synthetic products as hydrogenating materials, it is hydrogenated with catalyst action；Hydrogenation products produce the component of appropriate boiling range as sweating raw material through distillation；Sweatbox is used again, on the basis of common sweating process, is carried out sweating after sweating paraffin and water or salting liquid preferably are made into emulsion, is advantageous to the discharge of liquid composition；And liquid composition is carried out to force to separate solids fraction and liquid composition by wax layer using air-flow in sweating effort, enhance separating effect and accelerate separating rate；And increase the constant temperature stage of crystallization process and sweating effort, this solvent-free separation method of sweating is produced ink wax of the fusing point more than 70 DEG C.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.
A kind of production method of ink wax of oil of the invention, including herein below：
（One）Hydrogenation：F-T synthetic products are hydrogenated with hydrogenation catalyst effect, and alkene therein and oxygenatedchemicals are converted into n-alkane；
（Two）Distillation：Above-mentioned hydrogenated products therefrom is produced into the cut that initial boiling point is 450~480 DEG C, the end point of distillation is 490~520 DEG C in distilling apparatus, as sweating raw material；
（Three）Emulsification：Comprise the following steps：
（A1）It is prepared by oil phase material：With process（Two）It is raw material to distill the cut produced, heating fusing；Oil soluble emulsifying agent is added, is stirred, forms oil phase material；
（A2）It is prepared by water-phase material：Water or salting liquid are heated, form water-phase material；
（A3）It is prepared by emulsion：Water-phase material is added in oil phase material under agitation, continues stirring after all adding 5~60 minutes；
（Four）Sweating：Comprise the following steps：
（B1）Preparation：Will（A3）Emulsion prepared by process loads sweatbox；
（B2）Crystallization：First emulsion is cooled in the range of+10 DEG C of+4 DEG C~fusing point of sweating raw material fusing point with 5.0 DEG C/h~30.0 DEG C/h speed, then wax layer is cooled to by proper temperature with 0.5 DEG C/h~3.5 DEG C/h speed, high temperature constant temperature is for a period of time；5 DEG C~20 DEG C below sweating raw material fusing point of cooling final temperature is cooled to 0.5 DEG C/h~3.0 DEG C/h speed again, and cryogenic thermostat is for a period of time；
（B3 sweatings：Predetermined temperature is warming up to 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；
（B4）It is refined：It is ink wax after being refined on wax.
In the method for the present invention, described F-T synthetic products, its n-alkane weight content requirement is more than 85%, and the F-T synthetic products that preferably normal paraffin content is more than 95% are as raw material.
In the method for the present invention, described hydrogenation process uses the ordinary skill in the art, and its operating condition is：The h of volume space velocity 0.2~2.0 when 3~10MPa of reaction pressure, 150~300 DEG C of reaction temperature, liquid-1With hydrogen liquid volume ratio 100~1000：1, hydrogen liquid volume ratio is preferably 300~800：1.Hydrogenation catalyst can select Ni/Al2O3、W-Ni/Al2O3、Mo-Ni/Al2O3Or W-Mo-Ni/Al2O3Catalyst etc..Active metal component is using the weight content that oxide is counted as 20%~70% in catalyst.Hydrogenation catalyst can be prepared by this area conventional method.Reactive metal oxides can be reduced or vulcanized by this area conventional method as needed when using by catalyst, to improve catalyst activity.
In the method for the present invention, described distilling apparatus uses the conventional vacuum distilling apparatus of this area.
In the method for the present invention, the one or more in one group of material that described oil soluble emulsifying agent is formed selected from nonionic surface active agent, anionic surfactant, cationic surface active agent, amphoteric surfactant, response type surfactant active.The HLB value of oil soluble emulsifying agent is 1~10, preferably 3~8；The freezing point or fusing point of the surfactant are less than sweating heating maximum temperature（That is step（B3）In predetermined temperature）.
Wherein, described nonionic surface active agent is selected from one group of material that sorbitan monooleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester are formed；Anionic 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, the one group of material formed along succinate monoester sodium sulfonate.Described cationic surface active agent is selected from one group of material that benzyl quaternary ammonium salt, dodecyl benzyl dimethyl ammonium chloride, DTAC, cetyl trimethylammonium bromide, OTAC, triacetamide oleate are formed；Amphoteric surfactant is selected from one group of material that empgen BB, OA-12, aliphatic group imidazolidine derivatives, alkyl imidazoline derivatives, derivative of fatty acid, amphoteric modified epoxy ethane additive product are formed.
Described response type surfactant active can be reacted by organic acid and ammoniacal liquor, and added Organic Alcohol and be made.Specially：Organic acid and the ammoniacal liquor stirring reaction under conditions of 10~30 DEG C generate organic acid ammonium salt after 5~60 minutes；Under conditions of 60~70 DEG C, Organic Alcohol is added into the organic acid ammonium salt prepared, stirring makes it well mixed for 5~30 minutes.
Described organic acid is saturation and unsaturated acids of the carbon number 1~36, it is preferred that unitary organic acid of the carbon number 8~20, can be caprylic acid, acid of the positive tenth of the twelve Earthly Branches, n-capric acid, undecanoic acid, laurate, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, stearic acid, linoleic acid, oleic acid, nonadecanoic acid, one kind in arachidic acid or its mixture；It can also be multicomponent organic acid of the carbon number 2~8, can be one kind or its mixture in oxalic acid, malic acid, maleic acid, fumaric acid；It can also be the mixture of above-mentioned unitary organic acid and multicomponent organic acid.Described ammoniacal liquor mass concentration is 1%~28%, preferably 5%~15%.Described Organic Alcohol is saturated monohydroxy alcohol of the carbon number 1~12, one kind or its mixture preferably in methanol, ethanol.Described mixing speed is 50~1500r/min, preferably 100~1000r/min.Use in the sweating effort of reactive emulsifier and absorb ammonia by 2%~20% aqueous solution of the mass ratio of the acid such as sulfuric acid, nitric acid.
Described oil soluble emulsifying agent is preferably the compound emulsifying agent that two or more surfactants are formed.
In the method for the present invention, described salting liquid is any water-soluble salt solution, preferably chemical property is stable, nontoxic, non-corrosiveness, without special odor, salting liquid cheap and easy to get.Such as, salting liquid can be one kind or its mixture in sodium chloride solution, Klorvess Liquid, sodium carbonate liquor, solution of potassium carbonate, metabisulfite solution, potassium sulfate solution.The concentration of salting liquid is 1%~30%（Quality, similarly hereinafter）, preferably 5%~20%.
The proportioning of the emulsion is：Sweating paraffin 60.0%~90.0%, preferably 65.0%~84.0%；Water or salting liquid 9.9%~30.0%, preferably 15.0%~30.0%；Compound emulsifying agent 0.1%~10.0%, preferably 1.0%~5.0%.Described emulsification condition is at 80 DEG C~98 DEG C, is mixed 5~60 minutes with 50~1500 revs/min of mixing speed, preferably at 85 DEG C~95 DEG C, is mixed 10~30 minutes with 100~1000 revs/min of mixing speed.
In the method for the present invention, the preferred sweating ware of described sweatbox, and increase in wax layer pressue device added above and/or below wax layer vacuum plant.In step（B3）In sweating effort, the described wax layer that forces air flow through uses the 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 realizes.Described pressure differential is generally 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure, to force air flow through wax layer.
In the method for the present invention, in the temperature-fall period of the crystallization, preferred feedstock wax layer is first cooled in the range of+8 DEG C of+4 DEG C~fusing point of sweating raw material fusing point with 10.0 DEG C/h~25.0 DEG C/h speed；Thereafter the preferably 1.0 DEG C/h~3.0 DEG C/h of the rate of temperature fall before high-temperature constant temperature section.The proper temperature of described high-temperature constant temperature section is+4.0 DEG C of -1.0 DEG C~fusing point of sweating raw material fusing point, preferably raw material fusing point~+2.0 DEG C of fusing point.The time of high-temperature constant temperature section is 0.1~4.0 hour, preferably 0.5~4.0 hour, more preferably 1.0~4.0 hours.
In the method for the present invention, process（Four）Middle step（B2）Rate of temperature fall preferably 1.0 DEG C/h~2.5 DEG C/h of the crystallization after high-temperature constant temperature section.Described cooling final temperature is preferably 8 DEG C~15 DEG C below sweating raw material fusing point.It is described be cooled to final temperature after, the increase cryogenic thermostat stage, the time in cryogenic thermostat stage was 0.1~3.0 hour, preferably 0.5~3.0 hour, more preferably 1.0~3.0 hours so that solid crystal is more abundant.
In the method for the present invention, process（Four）Middle step（B3）Described heating rate preferably 1.0 DEG C/h~2.0 DEG C/h.The predetermined temperature of described sweating effort is less than 1 DEG C~10 DEG C of purpose product fusing point.It is described be warming up to predetermined temperature after, the increase constant temperature stage can make solids fraction and liquid composition separates more abundant, and the time in constant temperature stage is 0.1~5.0 hour, preferably 0.5~5.0 hour, more preferably 1.0~5.0 hours.
In the method for the present invention, the programming rate and cooling rate of said wax layer, it can be controlled by air bath, water-bath, oil bath or other feasible modes, it is preferred to use water-bath or oil bath.When controlling wax layer heating rate and rate of temperature fall using water-bath or oil bath mode, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, chuck, coil pipe etc. can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature；The circulatory system has program cooling/heating function, and the circulatory system adds the material such as water or conduction oil as circulatory mediator.
In the method for the present invention, process（Four）Middle step（B3）It is described to force air flow through wax layer and implement in sweating effort any stage, preferably implement initial stage in sweating.
In the method for the present invention, the described wax layer that forces air flow through is utilized in what increase air pressure above wax layer was realized, can such as apply 0.2~2.0 atmospheric pressure above wax layer（Gauge pressure）Pressure, and wax layer below remain normal pressure.
In the method for the present invention, the described wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized, and normal pressure can be such as kept above wax layer, and -0.2~-1.0 atmospheric pressure are maintained below wax layer（Gauge pressure）Pressure.
Many hot melt printing inks, especially pigment base hot melt printing ink, the problems such as tendency of oil seepage, this seepage can cause the mixing of color in excessive ink cleaning volume, nozzle to make printing effect variation thereafter in the printhead of inkjet-printing device be present.As print speed is more and more prominent to high speed development, these problems.Research shows, these phenomenons be the fusion range of wax material used it is wide caused by, can effectively solve these problems using the wax of " narrow melting range ", and ink rapid curing in the application can be made, the requirement of flying print can be met.The end temp of phase transition process and the difference of initial temperature represent melting range in conventional DSC curve, and general melting range could meet the requirement of " the narrow melting range " needed for hot melt printing ink wax when being less than 10 DEG C.
The melting range of the products such as common paraffin, microwax, Tissuemat E is all more than 15 DEG C, it is impossible to meets the requirement of ink wax " narrow melting range ".Chemically composition on analyze, be exactly these products carbon number distribution it is wide caused by, the requirement of hot melt printing ink wax " narrow melting range " could be met by only reducing the width of the carbon number distribution of these wax products.
F-T synthetic products are mainly n-alkane, but also contain a certain amount of alkene and oxygenatedchemicals, and the non-constant width of carbon number distribution, can not be directly used as hot melt printing ink wax.But containing a small amount of methyl chains in the high-carbon array point of F-T synthetic products, this structure makes it have low melt viscosity and suitable hardness and toughness, and this is beneficial with wax to ink.So the alkene in F-T synthetic products and oxygenatedchemicals are converted into by n-alkane by hydrogenation mode, then can the excellent hot melt printing ink wax of production performance through fine separation.
Sweating separation method is to carry out separation production wax product using the different property of various component fusing points.Research shows that liquid composition is gradually discharged along crystalline portion in sweating effort, situation about being flowed similar to liquid in capillary.For high melting-point wax product of the fusing point at 70 DEG C or so, because chemical composition is complicated, cause the more tiny densification of crystals upon crystallization structure, discharge to liquid composition forms huge filter flow resistance power, this results in only being difficult to be kept completely separate with liquid composition by solids fraction in the common sweating effort of gravity natural separation, therefore common sweating process can not produce wax product of the fusing point more than 70 DEG C.
The present invention in order to produce high performance ink wax, by ink with wax performance and its chemical composition associate and the further investigation of the composition of F-T synthetic products, the high low temperature F-T synthetic products of selection normal paraffin content are hydrogenating materials；Contain a certain amount of alkene and oxygenatedchemicals for low temperature F-T synthetic products, and the non-constant width of carbon number distribution is the reason for causing it to meet ink wax product requirement, by selecting appropriate catalyst and reaction condition, the non-Suitable ingredients such as the alkene in low temperature F-T synthetic products and oxygenatedchemicals are converted into n-alkane；And purpose component is enriched with by being evaporated under reduced pressure；Carbon number distribution width is reduced so that the performance of product meets the requirement of ink wax " narrow melting range " by sweating again.
The present invention is difficult to liquid composition separate reason by the further investigation to common sweating effort, for solids fraction, by using forcing air flow through wax layer, and increasing the processes such as constant temperature stage in crystallization process and sweating effort in sweating effort；Further preferably sweating raw material and water or salting liquid are made emulsion and carry out sweating again simultaneously, these measures significantly reduce the width of product carbon distribution, the performance of product is disclosure satisfy that the requirement of ink wax.
The reason for being difficult to separate with liquid composition for solids fraction in sweating effort, by carrying out method pressure solids fraction and the separation of liquid composition of liquid composition by wax layer using air-flow in sweating effort, enhance separating effect and accelerate separating rate；Increasing the high temperature constant temperature stage in temperature-fall period can make the crystallization of wax bigger, be advantageous to the discharge of liquid composition in sweating effort.Research for wax crystallization process shows that the chemical composition of wax is to determine the main factor of crystal habit, while the condition of cooling procedure can also influence crystal habit, and especially influence of the cooling condition at the temperature near fusing point to crystal habit is most obvious.Wax is when being cooled near fusing point, the n-alkane of larger molecular weight has formed crystallization and separated out, this partially crystallizable body can be as the nucleus for being subsequently formed crystallization, now increase the high temperature constant temperature stage, nucleus can be enable fully to increase, larger sized crystal is formed, although this larger sized crystal is thick not as the crystallization of low melt point paraffin, it is also highly beneficial that the crystal structure of this increase discharges liquid composition to the sweating stage.Raw material and water or salting liquid are further preferably formed into w/o type emulsion under the compound emulsifying agent effect of appropriate HLB value simultaneously, water or salting liquid is evenly distributed in the form of fine particle in sweating raw material；Pass through wax layer using air-flow in sweating effort, on the one hand water outlet or salting liquid can be carried to form short space in wax layer, these short spaces are easy to form some tiny passages in wax layer in sweating effort, are advantageous to the discharge of liquid composition in sweating effort；Another aspect air-flow can carry out liquid composition to force to separate solids fraction and liquid composition, so as to enhance separating effect and accelerate separating rate.From salting liquid as aqueous phase, aqueous phase and the difference in specific gravity of oil phase are increased, the velocity of discharge of the aqueous phase in sweating effort can be accelerated, to form the passage of discharge liquid composition as early as possible.Selected surfactant fusing point or freezing point are less than the maximum temperature of sweating effort, and contain functional group, poor with the intermiscibility of sweating paraffin, can be discharged in sweating effort with liquid composition.Being aided with the cryogenic thermostat stage of crystallization process again makes solid crystal more abundant, and the constant temperature stage of sweating effort makes solids fraction separate the methods of more abundant with liquid composition so that sweating process can produce the ink wax of " narrow melting range " of the fusing point more than 70 DEG C.
This have the advantage that：By selecting appropriate catalyst and reaction condition, the alkene in F-T synthetic products and oxygenatedchemicals are converted into n-alkane by hydrogenation process, while other impurity will not be produced；Purpose component is enriched with by distilling；The method for being carried out liquid composition by wax layer using air-flow in sweating effort is enhanced the separating effect of solids fraction and liquid composition and accelerates separating rate；Dispersed short space is formed in wax layer using water or salting liquid, is also beneficial to the quick discharge of liquid composition；And increase the process such as the constant temperature stage of crystallization process and the constant temperature stage of sweating effort, so as to produce ink wax.The present invention method have the advantages that plant investment is low, production process is simple and operating cost is low, safety, energy-conservation and it is solvent-free pollution environment.
Embodiment
For the present invention by being hydrogenating materials from suitable low temperature F-T synthetic products, the technical process such as hydrogenated, distillation, emulsification, sweating produces ink wax of the fusing point more than 70 DEG C.Specially low temperature F-T synthetic products are hydrogenated with catalyst action；Hydrogenation products produce 470~500 DEG C of cuts as sweating raw material in distilling apparatus；Sweating raw material after water or salting liquid emulsification with loading sweating ware；Sweating ware top connects dismountable sealing device and is connected with pressurized buffer tank and compressor, and/or connects pressure-reducing cushioning tank and vavuum pump in sweating ware bottom；Wax layer heating-cooling speed is controlled with water-bath；Wax layer temperature be down to sweating raw material melting temperature nearby and high temperature constant temperature for a period of time；Continue to be cooled to final temperature and cryogenic thermostat for a period of time；Wax layer heating reaches preset temperature and constant temperature stops sweating effort afterwards for a period of time；In sweating effort, start compressor with wax layer malleation formed above, and/or start vavuum pump with wax layer negative pressure formed below, to force air flow through wax layer；Purpose product is ink wax product after refined.
1-4 illustrates the production method of the ink wax of the present invention by the following examples.Unless otherwise instructed, involved % is mass percent below.
Comparative example
1
This comparative example includes：（One）Hydrogenation,（Two）Distillation,（Three）Sweating three parts.
（One）Hydrogenation
With the wax oil product of Sinopec Group's low temperature F-T compound experiment devices（Normal paraffin content is 95.50wt%）For raw material, in FHJ-2 catalyst（A kind of Ni/Al2O3Commercial catalysts, Fushun Petrochemical Research Institute's development and production, active metallic content is counted as 40% using oxide, catalyst carries out conventional reduction processing before use）Under effect, in reaction pressure 5.0MPa, 200 DEG C of reaction temperature, volume space velocity 1.0h-1
With hydrogen liquid volume ratio 500：It is hydrogenated with conditions of 1 to convert alkene and oxygenatedchemicals therein.
Hydrogenation products n-alkane weight content 97.36%；Chromatogram-mass spectral analysis, the materials such as alkene, alcohol, acid are not detected, it can be seen that alkene and oxygenatedchemicals in raw material have removed.
（Two）Distillation
By above-mentioned hydrogenated conversion products therefrom in vacuum distillation apparatus, between 13.3Pa ~ 133Pa under pressure condition, 470 DEG C~500 DEG C of cut is prepared.470 DEG C~500 DEG C 69.7 DEG C of cut fusing points, 18.32 DEG C of melting range, yield 5.50%（Relative to hydrogenation products）.
（Three）Sweating
This part includes：（1）Preparation,（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization（3）Heating-constant temperature sweating,（4）The process such as refined.
（1）Preparation
Pad water below sweating ware ware plate.The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects 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 heating medium, start the heating function of the circulatory system, recirculated water is warming up to 72 DEG C.
With（Two）470 DEG C~500 DEG C cuts prepared by part distillation are raw material, and sweating ware is added after being heated to 72 DEG C of fusings.
（2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Start the refrigerating function of the circulatory system, wax layer temperature is dropped to 70.5 DEG C and 2.0 hours progress high temperature constant temperatures of constant temperature with 2.0 DEG C/h rate of temperature fall, so that crystallization fully increases；Wax layer temperature is set to drop to 58.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature with 1.5 DEG C/h rate of temperature fall again, so that crystallization is more abundant.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；The sealing system on sweating ware top is installed；Start compressor and keep pressurized buffer pressure inside the tank stable in 1.3~1.5 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system function, wax layer temperature is increased to 66.0 DEG C with 1.5 DEG C/h heating rate；Stop compressor.
Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.5~-0.7 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Wax layer temperature is set to be increased to 74.0 DEG C and constant temperature 4.0 hours so that the solids fraction in wax layer is sufficiently separated with liquid composition with 1.0 DEG C/h heating rate；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 circulating water temperature to 90 DEG C, taken out with fusing on wax, as crude product（Ⅰ）.
（4）It is refined
Crude product（Ⅰ）It is ink wax product after clay-filtered（Ⅰ）.Ink wax product（Ⅰ）Property：75.2 DEG C of fusing point, 8.36 DEG C of melting range.Ink wax product（Ⅰ）Yield be 8.16%（Relative to 470 DEG C~500 DEG C cuts of raw material）.
Embodiment
1
The present embodiment includes：（One）Hydrogenation,（Two）Distillation,（Three）Emulsification,（Four）The part of sweating four.
（One）Hydrogenation
With comparative example 1.
（Two）Distillation
With comparative example 1.
（Three）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（Two）470 DEG C~500 DEG C cut 80.0Kg prepared by part distillation, sorbitan monostearate 1.0Kg, diethylene glycol fatty acid ester 0.5Kg, tetraethylene glycol monostearate 1.5Kg are added after being heated to 90 DEG C of fusings, is stirred.
（A2）It is prepared by water-phase material
17.0Kg water is heated to 95 DEG C.
（A3）It is prepared by emulsion
Stirred with 500r/min speed（A1）The oil phase material of middle preparation, and will（A2）The water-phase material of middle preparation is slowly added into oil phase material, is continued to stir 30min, is formed water-in-oil type emulsion.
（Four）Sweating
This part includes（B1）Preparation,（B2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization,（B3）Heating-constant temperature sweating,（B4）Refine four steps.
（B1）Preparation
The sealing system of sweating ware and pressurized buffer tank and compressor are connected；Pressure-reducing cushioning tank is installed in sweating ware bottom and connects vavuum pump；Sweating ware chuck and removable coil pipe are connected with the circulatory system, coil pipe is fixed on sweating ware；By medium of water using water to heat medium, start the heating function of the circulatory system, recirculated water is warming up to 75 DEG C.Pad water below sweating ware ware plate.Will（A3）The emulsion of middle preparation adds sweating ware.
（B2）Cooling-high temperature constant temperature-cooling-cryogenic thermostat crystallization
Emulsion stands the refrigerating function of the startup circulatory system after 1.0h, wax layer temperature is dropped to 70.5 DEG C and 2.0 hours progress high temperature constant temperatures of constant temperature with 2.0 DEG C/h rate of temperature fall, so that crystallization fully growth；Wax layer temperature is set to drop to 58.0 DEG C and 2.0 hours progress cryogenic thermostats of constant temperature with 1.5 DEG C/h rate of temperature fall again, so that crystallization is more abundant.Close the refrigerating function of the circulatory system.
（B3）Heating-constant temperature sweating
Discharge sweating ware pad water.Sweating ware outlet connection intermediate storage tank（Ⅱ）To receive under wax；The sealing system on sweating ware top is installed；Start compressor and keep pressurized buffer pressure inside the tank stable in 1.3~1.5 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start circulation system function, wax layer temperature is increased to 66.0 DEG C with 1.5 DEG C/h heating rate；Stop compressor.
Start vavuum pump and keep pressure-reducing cushioning pressure inside the tank stable in -0.5~-0.7 atmospheric pressure（Gauge pressure）, wax layer top air pressure holding normal pressure；Wax layer temperature is set to be increased to 74.0 DEG C and constant temperature 4.0 hours so that the solids fraction in wax layer is sufficiently separated with liquid composition with 1.0 DEG C/h heating rate；Stop vavuum pump, terminate sweating effort.
The outlet of sweating ware is changed to connect crude product storage tank（Ⅱ）To receive on wax.Continue to raise circulating water temperature to 90 DEG C, taken out with fusing on wax, as crude product（Ⅱ）.
（B4）It is refined
Crude product（Ⅱ）It is ink wax product after clay-filtered（Ⅱ）.Ink wax product（Ⅱ）Property：74.9 DEG C of fusing point, 5.03 DEG C of melting range.Ink wax product（Ⅱ）Yield be 10.8%（Relative to 470 DEG C~500 DEG C cuts of raw material）.
Embodiment
2
The present embodiment includes：（One）Hydrogenation,（Two）Distillation,（Three）Emulsification,（Four）The part of sweating four.
（One）Hydrogenation
With comparative example 1.
（Two）Distillation
With comparative example 1.
（Three）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（Two）470 DEG C~500 DEG C cut 80.0Kg prepared by part distillation, sorbitan monooleate 1.5Kg, diethylene glycol monolaurate 1.0Kg, DTAC 0.5Kg are added after being heated to 90 DEG C of fusings, is stirred.
（A2）It is prepared by water-phase material
1.5Kg KCl is dissolved in 15.5Kg water, and is heated to 95 DEG C.
（A3）It is prepared by emulsion
Stirred with 700r/min speed（A1）The oil phase material of middle preparation, and will（A2）The water-phase material of middle preparation is slowly added into oil phase material, is continued to stir 15min, is formed water-in-oil type emulsion.
（Four）Sweating
With embodiment 1.
The ink wax product of the present embodiment production（Ⅲ）Property：75.1 DEG C of fusing point, 4.96 DEG C of melting range.Ink wax product（Ⅲ）Yield be 11.5%（Relative to 470 DEG C~500 DEG C cuts of raw material）.
Embodiment
3
The present embodiment includes：（One）Hydrogenation,（Two）Distillation,（Three）Emulsification,（Four）The part of sweating four.
（One）Hydrogenation
With embodiment 1.
（Two）Distillation
With embodiment 1.
（Three）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（Two）470 DEG C~500 DEG C cut 80.0Kg prepared by part distillation, diethylene glycol fatty acid ester 1.5Kg, sorbitan monopalmitate 1.2Kg, oleamide yl carboxylic acid sodium 0.3Kg are added after being heated to 90 DEG C of fusings, is stirred.
（A2）It is prepared by water-phase material
2.0Kg NaCl is dissolved in 15.0 Kg water, and is heated to 95 DEG C.
（A3）It is prepared by emulsion
Stirred with 300r/min speed（A1）The oil phase material of middle preparation, and will（A2）The water-phase material of middle preparation is slowly added into oil phase material, is continued to stir 20min, is formed water-in-oil type emulsion.
（Four）Sweating
With embodiment 1.
The ink wax product of the present embodiment production（Ⅳ）Property：75.0 DEG C of fusing point, 4.91 DEG C of melting range.Ink wax product（Ⅳ）Yield be 11.3%（Relative to 470 DEG C~500 DEG C cuts of raw material）.
Embodiment
4
The present embodiment includes：（One）Hydrogenation,（Two）Distillation,（Three）Emulsification,（Four）The part of sweating four.
（One）Hydrogenation
With embodiment 1.
（Two）Distillation
With embodiment 1.
（Three）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（Two）470 DEG C~500 DEG C cut 80.0Kg prepared by part distillation, sorbitan monostearate 1.5Kg, diethylene glycol fatty acid ester 0.2Kg, OA-12 0.3Kg are added after being heated to 90 DEG C of fusings, is stirred.
（A2）It is prepared by water-phase material
By 2.0Kg KNO316.0 Kg water is dissolved in, and is heated to 95 DEG C.
（A3）It is prepared by emulsion
Stirred with 800r/min speed（A1）The oil phase material of middle preparation, and will（A2）The water-phase material of middle preparation is slowly added into oil phase material, is continued to stir 15min, is formed water-in-oil type emulsion.
B：Sweating
With embodiment 1.
The ink wax product of the present embodiment production（Ⅴ）Property：75.1 DEG C of fusing point, 4.83 DEG C of melting range.Ink wax product（Ⅴ）Yield be 11.1%（Relative to 470 DEG C~500 DEG C cuts of raw material）.
The production method of ink wax of the present invention is can be seen that by embodiment 1-4, by selecting appropriate catalyst and reaction condition, the alkene in raw material and oxygenatedchemicals are converted into the Suitable ingredients of ink wax；Sweating raw material is enriched with by distilling；By increasing the improvement to sweatbox such as pressurization and/or vacuum facility；Dispersed short space is formed in wax layer using the water or salting liquid of emulsification, the improvement to sweating process such as wax layer, the constant temperature stage for increasing crystallization and sweating effort is forced air flow through in sweating effort；Enhance the separating effect of solids fraction and liquid composition and accelerate separating rate, so that sweating separating technology produces ink wax of the fusing point more than 70 DEG C.
Claims (26)
1. a kind of production method of ink wax, including herein below：
（One）Hydrogenation：F-T synthetic products are hydrogenated with hydrogenation catalyst effect, and alkene therein and oxygenatedchemicals are converted into n-alkane；
（Two）Distillation：Above-mentioned hydrogenated products therefrom is produced into the cut that initial boiling point is 450~480 DEG C, the end point of distillation is 490~520 DEG C in distilling apparatus, as sweating raw material；
（Three）Emulsification：Comprise the following steps：
（A1）It is prepared by oil phase material：With process（Two）It is raw material to distill the cut produced, heating fusing；Oil soluble emulsifying agent is added, is stirred, forms oil phase material；
（A2）It is prepared by water-phase material：Water or salting liquid are heated, form water-phase material；
（A3）It is prepared by emulsion：Water-phase material is added in oil phase material under agitation, continues stirring after all adding 5~60 minutes；
（Four）Sweating：Comprise the following steps：
（B1）Preparation：Will（A3）Emulsion prepared by process loads sweatbox；
（B2）Crystallization：Emulsion is first cooled to by+10 DEG C of+4 DEG C~fusing point of sweating raw material fusing point with 5.0 DEG C/h~30.0 DEG C/h speed, then wax layer is cooled to by proper temperature with 0.5 DEG C/h~3.5 DEG C/h speed, high temperature constant temperature is for a period of time；5 DEG C~20 DEG C below sweating raw material fusing point of cooling final temperature is cooled to 0.5 DEG C/h~3.0 DEG C/h speed again, and cryogenic thermostat is for a period of time；
（B3）Sweating：Predetermined temperature is warming up to 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；
（B4）It is refined：It is ink wax after being refined on wax.
2. in accordance with the method for claim 1, characterized in that, described oil soluble emulsifying agent is selected from one group of material that nonionic surface active agent, anionic surfactant, cationic surface active agent, amphoteric surfactant, response type surfactant active are formed；The HLB value of oil soluble emulsifying agent is 1~10；The freezing point or fusing point of the surfactant are less than sweating heating maximum temperature.
3. in accordance with the method for claim 2, characterized in that, described nonionic surface active agent is selected from one group of material that sorbitan monooleate, sorbitan monostearate, diethylene glycol fatty acid ester, diethylene glycol monolaurate, sorbitan monopalmitate, tetraethylene glycol monostearate, polyoxypropylene stearate, sorbitan mono-laurate, polyoxyethylene fatty acid ester are formed；Described anionic 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, the one group of material formed along succinate monoester sodium sulfonate；Described cationic surface active agent is selected from one group of material that benzyl quaternary ammonium salt, dodecyl benzyl dimethyl ammonium chloride, DTAC, cetyl trimethylammonium bromide, OTAC, triacetamide oleate are formed；Described amphoteric surfactant is selected from one group of material that empgen BB, OA-12, aliphatic group imidazolidine derivatives, alkyl imidazoline derivatives, 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 the compound emulsifying agent that two or more surfactants are formed.
5. in accordance with the method for claim 1, it is characterised in that described salting liquid is selected from one group of solution that sodium chloride solution, Klorvess Liquid, sodium carbonate liquor, solution of potassium carbonate, metabisulfite solution and potassium sulfate solution are formed；The mass concentration of salting liquid is 1%~30%.
6. in accordance with the method for claim 1, it is characterised in that step（A3）Described in mixing speed be 50~1500 revs/min, prepare emulsion temperature be 80 DEG C~98 DEG C.
7. in accordance with the method for claim 1, it is characterised in that step（A3）The proportioning for obtaining emulsion is：Sweating paraffin mass percent is 60.0%~90.0%, and water or salting liquid mass percent are 9.9%~30.0%, and emulsifying agent mass percent is 0.1%~10.0%.
8. in accordance with the method for claim 7, it is characterised in that the proportioning of the emulsion is：Sweating paraffin mass percent is 65.0%~84.0%, and water or salting liquid mass percent are 15.0%~30.0%, and emulsifying agent mass percent is 1.0%~5.0%.
9. in accordance with the method for claim 1, it is characterised in that the weight content of the n-alkane in the F-T synthetic products is more than 85%.
10. in accordance with the method for claim 1, it is characterised in that process（One）The operating condition of middle hydrogenation is：The h of volume space velocity 0.2~2.0 when 3~10MPa of reaction pressure, 150~300 DEG C of reaction temperature, liquid-1With hydrogen liquid volume ratio 100~1000：1.
11. in accordance with the method for claim 1, it is characterised in that process（One）Described in hydrogenation catalyst be Ni/Al2O3、W-Ni/Al2O3、Mo-Ni/Al2O3Or W-Mo-Ni/Al2O3Catalyst, active metal component is using the weight content that oxide is counted as 20%~70% in catalyst.
12. in accordance with the method for claim 1, it is characterised in that step（B2）Described in the proper temperature of high-temperature constant temperature section be+4.0 DEG C of -1.0 DEG C~fusing point of sweating raw material fusing point, preferably sweating raw material fusing point~+2.0 DEG C of fusing point；The time of high-temperature constant temperature section is 0.1~4.0 hour, preferably 1.0~4.0 hours.
13. in accordance with the method for claim 1, it is characterised in that step（B2）Described in cooling final temperature for 8 DEG C~15 DEG C below sweating raw material fusing point.
14. in accordance with the method for claim 1, it is characterised in that step（B2）Described in the cryogenic thermostat stage time be 0.1~3.0 hour.
15. in accordance with the method for claim 1, it is characterised in that step（B3）Described in predetermined temperature be less than 1 DEG C~10 DEG C of purpose product fusing point.
16. in accordance with the method for claim 1, it is characterised in that step（B3）Described in constant temperature time be 0.1~5.0 hour.
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 implement at sweating initial stage.
18. in accordance with the method for claim 1, it is characterized in that, the described wax layer that forces air flow through uses the increase air pressure above wax layer and/or air pressure is reduced below wax layer, make wax layer upper and lower form pressure differential to realize, described pressure differential is 0.1~5.0 atmospheric pressure, preferably 0.2~2.0 atmospheric pressure.
19. in accordance with the method for claim 18, it is characterised in that step（B3）Described in force air flow through wax layer use above wax layer increase air pressure realize, above wax layer apply 0.2~2.0 atmospheric pressure gauge, and wax layer below remain normal pressure.
20. in accordance with the method for claim 18, it is characterised in that step（B3）Described in force air flow through wax layer use below wax layer reduce air pressure realize, above wax layer air pressure keep normal pressure, and below wax layer maintain -0.2~-1.0 atmospheric pressure gauge.
21. in accordance with the method for claim 2, it is characterised in that described response type surfactant active is reacted by organic acid and ammoniacal liquor, and is added Organic Alcohol and be made：Organic acid and the ammoniacal liquor stirring reaction under conditions of 10~30 DEG C generate organic acid ammonium salt after 5~60 minutes；Under conditions of 60~70 DEG C, Organic Alcohol is added into the organic acid ammonium salt prepared, stirring makes it well mixed for 5~30 minutes, that is, obtains response type surfactant active.
22. in accordance with the method for claim 21, it is characterised in that described organic acid is saturation and unsaturated acids of the carbon number 1~36.
23. in accordance with the method for claim 22, characterized in that, described organic acid, which is selected from caprylic acid, acid of the positive tenth of the twelve Earthly Branches, n-capric acid, undecanoic acid, laurate, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, stearic acid, linoleic acid, oleic acid, nonadecanoic acid, arachidic acid, oxalic acid, malic acid, citric acid, maleic acid, fumaric acid, forms one or more of one group of material.
24. in accordance with the method for claim 21, it is characterised in that the mass concentration of the ammoniacal liquor is 1%~25%.
25. in accordance with the method for claim 21, it is characterised in that described Organic Alcohol is saturated monohydroxy alcohol of the carbon number 1~12, preferably methanol and/or ethanol.
26. in accordance with the method for claim 1, it is characterised in that described sweatbox is sweating ware.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114686262A (en) * | 2020-12-31 | 2022-07-01 | 内蒙古伊泰煤基新材料研究院有限公司 | Method for preparing high-hardness wax for Fischer-Tropsch ink |
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| CA421565A (en) * | 1944-07-18 | Standard Oil Development Company | Wax sweating process | |
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