CN106883874B - A method of producing novel rubber protective wax - Google Patents
A method of producing novel rubber protective wax Download PDFInfo
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- CN106883874B CN106883874B CN201510928606.6A CN201510928606A CN106883874B CN 106883874 B CN106883874 B CN 106883874B CN 201510928606 A CN201510928606 A CN 201510928606A CN 106883874 B CN106883874 B CN 106883874B
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1081—Alkanes
- C10G2300/1085—Solid paraffins
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- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of methods producing novel rubber protective wax.This method is on the basis of common sweating de-oiling technique, the oil of liquid is carried out to force separation wax and oil by wax layer using air-flow in sweating effort, generation gas is decomposed using inorganic salts simultaneously and form short space in wax layer, to fast and effeciently eliminate the non-suitable component in paraffin grade wax to Wax-for preventing rubber；Sweating obtained component allocates production preventing rubber wax product with alhpa olefin again.The advantages that method production process of the present invention is simple, operating cost is low, product can play permanently effective protective action to rubber and its product.
Description
Technical field
The invention belongs to Wax special production technical fields, more particularly to a kind of method producing novel rubber protective wax.
Background technology
The rubber product chemical substances such as aerial ozone and other factors during processing, storage and use are made
Phenomena such as being declined with the cracking of lower generation rubber article, whiting, mechanical performance, these phenomenons are referred to as " aging ", with old
The performance of the progress of change process, rubber and its product can continuously decrease so that losing use value completely.Ozone is to cause rubber
The principal element of aging.Rubber product, such as tire, can accelerated ageing process during dynamic use.
In order to extend storage period and the service life of rubber and its product, aging can be inhibited by needing some are added in rubber
The substance of process, these substances are known as anti-aging agent.Rubber antioxidant is divided into chemical antiager and physical antioxidant.Wax-for preventing rubber
It is physical antioxidant, is usually made at present by main component allotment of pertroleum waxes such as paraffin, microwaxes.
The general name of the pertroleum wax all kinds of wax products obtained 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 dewaxing, de-oiling, refined and molding
Production, typically contain C18~C50The components such as n-alkane, isoparaffin and minimal amount of cycloalkane, usual fusing point is 50
DEG C~74 DEG C, it is in coarse flaky crystal structure under solid-state.Microwax is that decompression residuum passes through again after propane equal solvent depitching
Dewaxing, de-oiling, refined and molding and etc. production, generally by C30~C60Isoparaffin, cycloalkane and a small amount of N-alkanes
Hydrocarbon, aromatic hydrocarbon composition, usual dropping point is 65 DEG C~92 DEG C, has the needle-like crystal structure more tiny than paraffin under solid-state.It is de-
Wax is the process that the slack wax that oil content is 10~30% or so is prepared by raw material of lube cut, and dewaxing technique mainly has squeezing
Dewaxing and solvent dewaxing.De-oiling is that the process of 2% base oil wax below of oil content, de-oiling technique master are prepared using slack wax as raw material
There are solvent deoiling and sweating de-oiling.
Wax-for preventing rubber has certain solubility, the size of solubility and the type of alkane and temperature to have in rubber
It closes.Wax-for preventing rubber is added during rubber processing with together with other auxiliary agents, in higher temperature（Such as curing temperature）Lower rubber
Various alkane in protection wax are dissolved completely in sizing material；And in lower temperature（Such as room temperature）Content of the lower alkane in rubber is big
In its solubility limit at such a temperature be in hypersaturated state, at this time since the concentration of rubber surface wax is relatively low, preventing rubber
N-alkane and isoparaffin in wax can be migrated to rubber surface at leisure, gradually form protective filmy layer（Bloom）, to
Play the role of age inhibiting.
Wax-for preventing rubber is related with the kind of rubber and the formation speed and quality of protecting film to the protective action of ozone.It is anti-
The formation speed and quality of cuticula are influenced by many factors, such as filler and softening agent, temperature in use, the rubber of rubber product
The chemical composition of protection wax（Main carbon number distribution and the n-alkane of specific carbon number and containing for isoparaffin including pertroleum wax
Amount）Deng.Rubber product manufacturer can be according to the kind of rubber raw materials, the kind of filler and softening agent and ratio, production in product
The factors such as the environment temperature that product use propose the technology requirement to Wax-for preventing rubber chemical composition.
Some patents propose specific requirement to the chemical composition of Wax-for preventing rubber, as U.S.P.4877456 propositions are used for
C in the protection wax of rubber product21~C26、C36~C51The content of n-alkane in range should all reach 20%~45%, while just
The total content of structure alkane should at least reach 75%；U.S.P.5296129 emphasizes C22~C44N-alkane content, suggest simultaneously
C30~C60Isoparaffin content should account for the 16%~30% of alkane total amount.
The pertroleum wax of the single trade mark cannot meet technology requirement of the Wax-for preventing rubber to chemical composition, so production rubber is anti-
It usually requires to be allocated using the pertroleum wax of different manufacturers, the different trades mark when protecting wax, such as CN01106005.0（Preventing rubber
Wax）、CN200410080803.9（Wax-for preventing rubber）、CN200910056973.6（A kind of novel rubber protective wax）、
CN201310205094.1（A kind of Wax-for preventing rubber and preparation method thereof）Etc. patents, be all using the oil such as paraffin and microwax
Wax is as the main component, and adds a small amount of property-modifying additive（Polyethylene wax, ethylene-vinyl acetate copolymer and antioxidant etc.）.By
It is a variety of by the technical parameters of production processes such as the property of crude oil, fraction range, dewaxing and de-oiling etc. in the chemical composition of pertroleum wax
The chemical composition of the influence of factor, pertroleum wax often will appear larger fluctuation, so needing basis when production Wax-for preventing rubber
The variation of raw material pertroleum wax property constantly adjusts formula, this brings many troubles to the determination of the purchasing of raw materials and formula.It is general simultaneously
Non- Suitable ingredients containing partial rubber protection wax in logical pertroleum wax, this shortens Wax-for preventing rubber and prevents rubber and its product
Protect the time.
In terms of pertroleum wax production technology, common manufacturing process mainly has distillation, solvent deoiling, sweating de-oiling etc..
Distillation is to achieve the purpose that separating-purifying using the boiling point difference of different hydrocarbons, and the boiling range for reducing distillation can be effective
The width of product carbon distribution is reduced, but little to the scale effect of n-alkane and isoparaffin, simultaneously because distillation process needs
Pertroleum wax is heated to boiling point or more, consumes a large amount of energy.
Solvent deoiling method is with oil according to wax in selective solvent（Acetone, benzene and toluene mixture；Or acetone, toluene；
Or methyl ethyl ketone, toluene）The property of middle different solubility achievees the purpose that separating-purifying, can effectively improve the N-alkanes in product
Hydrocarbon content, but the width of carbon distribution is influenced less, while solvent deoiling investment of production equipment is big；It is needed in production process a large amount of
Using solvent, recycling design needs to consume a large amount of energy；Contain benzene homologues in solvent, environment can be impacted；Solvent is easy
Combustion, be easy to cause production accident.
Sweating de-oiling method carries out separating-purifying using different hydrocarbons component property with different melting point.It is each in pertroleum wax
The molecular weight of kind component Bu Tong can all make its fusing point different with structure.When being all n-alkane, the larger N-alkanes of molecular weight
The fusing point of hydrocarbon is higher, and the fusing point of the smaller n-alkane of molecular weight is relatively low；When molecular weight is identical, isoparaffin and cycloalkane
Fusing point will be less than n-alkane, and isomery degree more high-melting-point is lower.So sweating de-oiling can reduce the distribution of product carbon
Width can change normal paraffin content again.
Compared with distillating method, since the melting temperature of various hydro carbons is far below boiling temperature, so sweating degreasing process
Energy consumption far below distillation detach；Compared with solvent deoiling method, sweating degreasing process does not use solvent, so sweating de-oiling
Cheng Anquan, it is energy saving and on environment without influence.And two aspect of width and normal paraffin content that diaphoresis can be distributed in product carbon
Change chemical composition, so ratio two side of the sweating de-oiling separation process in production process and adjusting n-alkane and isoparaffin
Face is all advantageous.
Common sweating de-oiling technique mainly includes the following steps that：（1）Preparation：Pad water（It is full of sweatbox with water
Ware plate lower space）After feed（Raw material is heated to being packed into sweatbox when fusing point or more is in a liquid state）；（2）Crystallization：By raw material with
Rate of temperature fall no more than 4 DEG C/h progressively cools to 10~20 DEG C of its fusing point or less.In cooling procedure, various components press fusing point
Sequence from high to low crystallizes and forms solid successively；（3）Sweating：After wax layer temperature reaches preset cooling final temperature,
Bleed off pad water；Raw material is slowly heated to preset sweating final temperature again.In sweating effort, various components by fusing point by
Low to high sequence is successively fused into liquid and flows out（Under wax）, the wax layer residue that finally obtains（On wax）Be exactly high-melting-point,
The wax of low oil-containing；Continue to increase temperature, be taken out on wax with fusing, as crude product；（4）It is refined：Generally use is clay-filtered（It will
It is warming up to predetermined temperature after crude product fusing, carclazyte is added and is simultaneously filtered after constant temperature was stirred to the predetermined time）；Again through being molded, packing
It is purpose product.
To common sweating de-oiling technique, in sweating effort although wax and oily two class components are respectively at solid and liquid
State, but also be difficult to be kept completely separate.To make the oil content of final products meet the requirements, generally use extends sweating sessions and improves
The method of sweating final temperature.Extending sweating sessions can cause the production cycle to extend；Product can be led to by improving sweating final temperature
Yield declines.
Compared with solvent deoiling, sweating de-oiling technique is intermittently operated, and product yield is relatively low, the production cycle is longer, but
Be sweating de-oiling technique have small investment, production process is simple, operating cost is low, production process is safe, it is energy saving and to environment without
The advantages that pollution, still has part of the manufacturer producing soap manufacturing paraffin product using this method at present.
For many years, sweating de-oiling method has obtained some development, such as CN89214332 in production equipment and process aspect（It is vertical
Formula 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 de-oiling production equipment；CN91206202
（A kind of high-efficient sweat pot for paraffin wax）It is improved in sweating de-oiling technique.But that there are still product yields is relatively low for these methods,
The shortcomings of production cycle is longer.
Alpha-olefin（α-olefin, Alpha Olefins）Refer to monoolefine of the double bond in strand end, industrially refers exclusively to
Alpha-olefins more than five carbon atom numbers, the usually mixture of carbon number range wider distribution.Alpha-olefin generally use paraffin is split
Solution or ethylene are made by oligomerization in the presence of a catalyst.Alpha-olefin obtains the mixture of acid with ozone reaction.
Sweating de-oiling technique is the unique solvent-free de-oiling method being currently known for commercial scale petroleum paraffin product,
Advocating environmentally protective, low-carbon energy-saving the concern for being increasingly subject to people today.Meanwhile improve Wax-for preventing rubber in it is effective at
Part, it is also problem in the urgent need to address to the guard time of rubber and its product effectively to extend it.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of method producing novel rubber protective wax, specifically
Using paraffin as raw material, the non-Suitable ingredients in paraffin to Wax-for preventing rubber are removed through sweating, then production rubber is allocated with alpha-olefin
Protect wax product.The sweating is to use sweatbox, excellent after raw material heating fusing on the basis of common sweating process
Choosing mixes the inorganic salt powder that decomposable asymmetric choice net generates gas under stress；And it is taken by wax layer using air-flow in sweating effort
The oil of liquid is taken out of to force separation wax and oil, separating effect is enhanced and accelerates separating rate.The thermostatic process of crystallization and
Inorganic salts are absorbed in sweating effort decomposes the pernicious gas generated.It removes unreacted inorganic salts using water-washing method and decomposes and produce
Object.The method production process of the present invention is simple, operating cost is low, product can play rubber and its product permanently effective protection
The advantages that effect.
A kind of method producing novel rubber protective wax of the present invention, including the following contents：
A sweatings：Include the following steps：
（A1）Charging：It is less than 2.0%, paraffin that fusing point is 52 DEG C~72 DEG C in mass using oil content as raw material, heating is molten
Sweatbox is packed into after change；
（A2）Crystallization：The pre- constant temperature of 8 DEG C~20 DEG C of raw material fusing point or less is cooled to the rate of 1.0 DEG C/h~4.0 DEG C/h
Degree, and constant temperature is for a period of time；
（A3）Sweating：It is heated up with the rate of 0.5 DEG C/h~3.0 DEG C/h；Wax layer reaches first predetermined temperature and constant temperature one
It the section time, is continuously heating to second predetermined temperature and constant temperature stops sweating afterwards for a period of time；Air-flow is forced in sweating effort
Pass through wax layer；Continue heating to melt and take out on wax；
（A4）It is refined：It is spare after purpose group lease making is refined；
B is allocated：
By alpha-olefin and above-mentioned sweating and after refining, products therefrom is 10~40 by weight：60~90 ratio heating is molten
Melt and be uniformly mixed, is preventing rubber wax product after molding.
In the method for the present invention, the starting paraffin is common commercial goods, oil content（In mass）Less than 2.0%,
Fusing point is 52 DEG C~72 DEG C, preferably 62 DEG C~70 DEG C.
Process of the present invention it is preferred mixing the nothing that decomposable asymmetric choice net generates gas under stress after raw material heating fusing
Machine salt powder, the pressure（Gauge pressure）Generally 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.It is described
Inorganic salt powder can slowly be decomposed in sweating effort and release gas and itself and decomposition product is soluble easily in water, can be with
It is one or more of ammonium salt, carbonate, bicarbonate.The granularity of the inorganic salt powder is 50~500 mesh, addition
Account for the 0.1%~10.0% of sweating raw material（Weight）, preferred ratio is 0.2%~3.0%.Thermostatic process in crystallization and sweating
Inorganic salts are absorbed in journey decomposes the pernicious gas generated.In subtractive process using water-washing method remove unreacted inorganic salts and
Decomposition product.
In the method for the present invention, the sweatbox is generally sweating ware, and added above dismountable close in wax layer
Envelope system and pressue device, in step（A1）Charging and step（A2）Inorganic salts are inhibited to decompose production in the temperature-fall period of crystallization
Raw gas escapes wax layer.The pressure（Gauge pressure）For 0.5~15.0 atmospheric pressure, preferably 1.0~8.0 atmospheric pressure.
In the method for the present invention, the sweating ware increases in wax layer pressue device added above and/or below wax layer
Vacuum plant.The wax layer that forces air flow through uses the increase air pressure above wax layer and/or reduces air pressure below wax layer,
Make wax layer upper and lower form pressure difference to realize.The pressure difference is generally 0.1~5.0 atmospheric pressure, and preferably 0.2~2.0
A atmospheric pressure, to force air flow through wax layer.
In the method for the present invention, rate of temperature fall preferably 1.5 DEG C/h~3.0 DEG C/h of the raw material wax layer crystallization process.Institute
State 10 DEG C~15 DEG C of cooling final temperature preferred raw material paraffin melting point or less.
In the method for the present invention, the time in the constant temperature stage of the raw material wax layer crystallization process is 0.1~3.0 h, preferably
1.0~3.0 h, while pressure is continuously decreased to normal pressure.Pressure is continuously decreased while crystallization process constant temperature to normal pressure, decompression speed
Rate is 0.1~150.0 atmospheric pressure/hour, preferably 0.3~8.0 atmospheric pressure/hour.
In the method for the present invention, heating rate preferably 1.0 DEG C/h~2.0 DEG C/h of the raw material wax layer sweating effort.Institute
First predetermined temperature for stating heating is -10 DEG C of raw material fusing point~-3 DEG C of raw material fusing point, preferably -8 DEG C of raw material fusing point~raw material
- 3 DEG C of fusing point；Two pre- constant temperatures of heating are -5 DEG C of raw material fusing point~+8 DEG C of raw material fusing point, preferably -3 DEG C of raw material fusing point~original
Expect+5 DEG C of fusing point.
In the method for the present invention, the constant temperature time of the sweating effort is 0~5.0 hour, preferably 0.1~5.0 hour,
More preferably 1.0~5.0 hours.
In the method for the present invention, the heating rate and cooling rate of said wax layer can pass through air bath, water-bath, oil bath
Or other feasible modes are controlled, it is preferred to use water-bath or oil bath.Wax layer heating is controlled using water-bath or oil bath mode
When rate and rate of temperature fall, chuck can be increased outside sweating ware, chuck is connected with removable coil pipe and the circulatory system, chuck, disk
Pipe etc. can make wax layer lifting/lowering temperature process faster, wax layer more uniform temperature；The circulatory system has program cooling/heating function, cycle
The substances such as water or conduction oil are added as circulatory mediator in system.
It is described to force air flow through wax layer and implement in sweating effort any stage in the method for the present invention, preferably
Implement at sweating initial stage.
In the method for the present invention, the wax layer that forces air flow through is utilized in what increase air pressure above wax layer was realized,
0.2~2.0 atmospheric pressure can such as be applied above wax layer（Gauge pressure）Pressure, and wax layer below remain normal pressure.
In the method for the present invention, the wax layer that forces air flow through is utilized in what reduction air pressure below wax layer was realized,
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.
Step of the present invention（A4）Described in purpose component refer in sweating effort first time constant temperature terminate it is permanent to second
Temperature terminates product under the wax collected in the process, usually under two waxes.
In the method for the present invention, the sweatbox can also connect absorption system, in the thermostatic process of crystallization and
Inorganic salts are absorbed in sweating effort decomposes generation（It is harmful）Gas.Absorption system uses liquid absorption mode.
In the method for the present invention, the alpha-olefin is the alpha-olefin that carbon number is more than or equal to 23, preferably C23~C30Content is
60% or more alpha-olefin.
In the method for the present invention, the allotment be by alpha-olefin and sweating and it is refined after products therefrom by weight being 10
~40：60~90 ratio, preferably 15~30：70~85 ratio, heating are melted and are uniformly mixed, and are rubber after molding
Protect wax product.
The effect of Wax-for preventing rubber is to form protecting film in rubber surface to play the role of completely cutting off ozone.Research shows that smelly
Oxygen is mainly to occur between 0~50 DEG C to the aging action of rubber.When temperature is less than 0 DEG C, due to the activation point of ozone
Son is few, cannot chemically react, i.e., rubber will not generate aging phenomenon because of the effect of ozone；Temperature in use is at 50 DEG C or more
When, ozone can resolve into oxygen, thus rubber will not generate aging phenomenon because of ozone.
Part of the various components only at a certain temperature more than solubility limit in rubber can just move in Wax-for preventing rubber
Rubber article is moved on to form cere to play protective action.Wax-for preventing rubber prevents rubber between 0~50 DEG C
Shield effect it is related with the formation speed and quality of protecting film, can quickly be formed suitable depth, it is fine and close, can be attached to very well
The protecting film of rubber surface can just effectively play the protective action to rubber.The formation speed and quality of protecting film are by many factors
Influence, most important one factor is the chemical composition of Wax-for preventing rubber.Meanwhile additive amount of the Wax-for preventing rubber in rubber
It is restricted, this is because Wax-for preventing rubber and rubber mutual compatibility are poor, local stress can be generated when excessive in rubber product, from
And the dynamic flexural property of rubber is reduced, so protecting film cannot be formed between 0~50 DEG C when containing in Wax-for preventing rubber
When non-Suitable ingredients, the time that Wax-for preventing rubber plays the role of effective protection will be influenced.
The speed that Wax-for preventing rubber forms protecting film in rubber surface is related with the speed that alkane is migrated to rubber surface, and
Migration velocity is influenced by many factors such as the structure of alkane, molecular weight and temperature.Research shows that positive structure when molecular weight is identical
Migration velocity of the alkane in rubber is relatively fast, and isoparaffin migration velocity is slower, and the higher alkane of degree of branching（That is institute
" oil " of meaning）, the migration velocity of cycloalkane and aromatic hydrocarbon in rubber it is very slow, to film forming do not work substantially；Temperature pair
Solubility and migration velocity of the alkane in rubber all have an impact, it is however generally that, temperature raising can make alkane molten in rubber
Xie Du increases, and migration velocity of the alkane in rubber is made to improve, and the migration velocity of the alkane of different carbon atom numbers is specific
At a temperature of can reach maximum value.Research shows that C at 0 DEG C23~C24Migration velocity it is maximum, C at 30 DEG C29~C30Migration velocity
Maximum, and the C at 50 DEG C38~C39Migration velocity it is maximum.Therefore temperature forms alkane in rubber surface the speed of protecting film
Influence be the synthesis result influenced on solubility and migration velocity：In low temperature, each component of Wax-for preventing rubber is moved
Shifting rate is relatively low, forms protecting film at this time and relies primarily on the alkane compared with low carbon atom number；In higher temperature, since solubility increases
Add the low carbon atom number alkane for making rubber surface to be redissolved in rubber, forms protecting film at this time and rely primarily on higher carbon atom
Several alkane.Due to being necessarily present in the surface of rubber to the alkane molecule that rubber shields rather than in rubber
Portion, that is to say, that at a certain temperature, the alkane of specific carbon number plays good protective action to rubber, and at another temperature
Protective action is not played then.The solubility of alkane can since temperature raises increased, to form effective protecting film, needs addition more
At a high temperature of play the alkane of protective action, i.e., the content of higher carbon number alkane is higher than compared with low carbon number alkane in Wax-for preventing rubber
Content.
The protecting film that Wax-for preventing rubber is formed in rubber surface must be fine and close and can be attached to rubber surface very well
Cere could play protective action to rubber long-term effectively in this way.N-alkane migration velocity in rubber is very fast, Ke Yi
Rubber surface quickly forms protecting film, but the adhesive force for protecting membrane crystallization coarse and with rubber that n-alkane is formed is smaller,
This coarse crystallization makes have hole between crystal, not can effectively prevent the transmission of ozone, simultaneously because the attachment with rubber
Power is smaller, is easy to fall off from rubber surface in the form of sheets, therefore poor to the protective action of rubber.And in isoparaffin molecular structure
Containing branch, solubility is smaller in rubber, and migration velocity is slow with respect to n-alkane, but rubber surface crystallize or with just
The crystallization formed when structure alkane cocrystallization is tiny, can make protecting film densification and adhesion is good, can effectively stop ozone infiltration,
Achieve the purpose that well to protect.Therefore it requires to contain a certain amount of isoparaffin in the chemical composition of Wax-for preventing rubber.
As the above analysis, to enable Wax-for preventing rubber to play protective action to rubber long-term effectively, just should
Suitable depth, protecting film fine and close, that rubber surface can be attached to very well can be quickly formed between 0~50 DEG C, this is just
It is required that carbon number distribution concentrates on C in its chemical composition23~C39Between, and contain a certain number of isoparaffins, and " oil ", ring
The content of alkane and aromatic hydrocarbon is very low.
Studies have shown that presently commercially available paraffin grade wax and microwax usually contain the alkane of 20 carbon numbers or more, i.e., centainly contain
There is C23Below and/or C39The non-suitable component of above Wax-for preventing rubber, while also containing a certain number of " oil ".Especially
Contain a large amount of C in microwax39The non-Suitable ingredients of the Wax-for preventing rubbers such as above alkane, cycloalkane and aromatic hydrocarbon, are not suitable for
It is directly used as the raw material of production Wax-for preventing rubber, even if it is also unfavorable to be used as sweating raw material to produce Wax-for preventing rubber.And
Paraffin is based on n-alkane and isoparaffin, it is only necessary to reduce " oil " content and carbon number distribution is made to concentrate on C23~C39Between,
It just can be used for producing Wax-for preventing rubber.In general, fusing point in 62 DEG C~70 DEG C of paraffin isomerization Determination of Alkane Content than fusing point 52
DEG C~62 DEG C of paraffin wants high, the allotment component preferably as Wax-for preventing rubber.But fusing point is in the carbon of 62 DEG C~70 DEG C paraffin
Number distribution concentrates on C30More than, i.e., protective action is played to rubber and its product between 30 DEG C~50 DEG C, so also needing to be added
The component of protective action can be played between 0 DEG C~30 DEG C.
Ozone can promote the ozone that is primarily due to of rubber and its product ager process to be reacted with the double bond in rubber, make double
Key is broken or generates crosslinking, and alpha-olefin is small molecule, participates in forming protecting film after moving to rubber surface, while its double bond can
It reacts with ozone prior to the double bond in rubber, therefore dual protective effect can be played to rubber.Alpha-olefin is anti-with ozone
Should after generate organic acid, carboxyl can influence the stereoregular of molecular structure, so that crystallization is become tiny, this is also beneficial to rubber
Protective action.C23~C30Migration velocity and C of the alpha-olefin in rubber23~C30Alkane it is suitable, can 0 DEG C~30 DEG C it
Between protective action is played to rubber and its product.
Sweating de-oiling method is to be detached using wax and oil property with different melting point to produce pertroleum wax, this method
The width of carbon number distribution can be reduced can adjust the ratio of n-alkane and isoparaffin again, therefore be to adjust paraffin chemical composition
Effective ways, but in common sweating effort, in wax layer solid wax and the oil of liquid be difficult be kept completely separate, this is because
Wax and oily two kinds of components are all nonpolar hydrocarbon molecules, and intermolecular force is larger；Solid wax crystallization forms capillary simultaneously
Pipe structure has stronger suction-operated to oil, and it is difficult that this results in wax and oil only in the common sweating effort of gravity natural separation
To be kept completely separate.Generally use, which extends the methods of sweating sessions, raising sweating final temperature, makes the oil content of final products meet
It is required that but this can cause production cycle length, wax product yield low again.
The present invention is by the further investigation to Wax-for preventing rubber to the protective action principle of rubber and its product, for cycloalkanes
The case where non-Suitable ingredients of the Wax-for preventing rubbers such as hydrocarbon and aromatic hydrocarbon are primarily present in microwax, using fusing point at 62 DEG C~70 DEG C
Paraffin be raw material effectively to reduce the content of cycloalkane and aromatic hydrocarbon, and the content of isoparaffin can be increased；And use sweating
Method removes " oil " and C of the fusing point in 62 DEG C~70 DEG C of paraffin23Below and C39The Wax-for preventing rubbers such as above alkane it is non-
Suitable ingredients improve the content of the Suitable ingredients in Wax-for preventing rubber in this way, therefore effectively extend the anti-of Wax-for preventing rubber
The time is protected, and good protective action is played to rubber and its product between 30 DEG C~50 DEG C；C is added simultaneously23~C30α-
Alkene plays protective action between 0 DEG C~30 DEG C to rubber and its product, simultaneously as alpha-olefin contains double bond, it can be to rubber
And its product plays additional protective action.
The present invention is in order to improve the efficiency of this solvent-free production paraffin method of sweating de-oiling, by common sweating effort
Further investigation, be difficult to be kept completely separate reason for wax and oil, liquid carried out by wax layer using air-flow in sweating effort
The method of oil forces the separation of wax and oil, enhances separating effect and accelerates separating rate, and the constant temperature by increasing sweating
Stage is so that wax and oil can be detached more completely.Decomposable asymmetric choice net is further preferably mixed under stress after raw material heating fusing simultaneously
The inorganic salt powder of gas is generated, these substances slowly settle due to granularity is smaller in the wax layer of liquid.Keep pressure condition
It is lower that raw material is cooled to 10 DEG C~15 DEG C of fusing point or less, and constant temperature 0.1h~3.0h is so that wax layer crystallization is more abundant；Simultaneously in perseverance
Pressure is continuously decreased to normal pressure during temperature.Raw material is cooled to wax layer in the time terminated to sweating effort after fusing point or less and is in
Softer solid state, inorganic salts slowly decompose the gas released during this, micro-bubble can be formed in wax layer, these
The space that micro-bubble is formed is easy to form several tiny channels in wax layer in sweating effort, to be conducive to sweating
Oily discharge in journey.The oily to force separation wax and oil of liquid is carried out by wax layer using air-flow in sweating effort simultaneously,
It enhances separating effect and accelerates separating rate.
It is an advantage of the invention that：By using air-flow to be forced by the method that wax layer carries out fluid oil in sweating effort
The separation of wax and oil, enhances separating effect and accelerates separating rate；The gas generated is decomposed in wax using inorganic salts simultaneously
Short space is formed in layer, is also beneficial to the quick discharge of oil, to effectively remove the non-suitable of Wax-for preventing rubber in paraffin
Component；Again with the preventing rubber wax product of alpha-olefin allotment production, there is suitable chemical composition, while effectively increasing rubber
The content of glue protection wax Suitable ingredients, that is, extend the service life of rubber.The method of the present invention is low with plant investment, produces
Process is simple and operating cost is low, safe, energy saving and solvent-free pollution environment, product can play rubber and its product has for a long time
The advantages that protective action of effect.
Specific implementation mode
Sweating ware top connects dismountable sealing device and is connect with pressurized buffer tank and compressor, and/or in sweating
Ware lower part connects pressure-reducing cushioning tank and vacuum pump；Raw material heating is melted and is filled after preferably mixing inorganic salt powder under stress
Enter sweating ware；Wax layer heating-cooling speed is controlled with water-bath；In sweating effort, start compressor with formed above just in wax layer
Pressure, and/or start vacuum pump in wax layer negative pressure formed below, to force air flow through wax layer；Wax layer heating reaches first
Simultaneously constant temperature for a period of time, continues to be warming up to second preset temperature and constant temperature stops sweating afterwards for a period of time a preset temperature
Journey；Purpose component is refined；Sweating product is allocated with alpha-olefin, is molded, being purpose product after packaging again.Pass through these
Means can be improved the effective content of preventing rubber wax product and product made to have suitable chemical composition.
By the following examples 1 and embodiment 2 illustrate the present invention production novel rubber protective wax method.
Embodiment 1
The present embodiment includes：A sweatings and B allocate two parts.
A：Sweating
This part includes：（A1）Preparation,（A2）Crystallization,（A3）Sweating,（A4）The processes such as refined.
（A1）Preparation
Sweating ware chuck and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；The heating function for starting the circulatory system, makes recirculated water be warming up to 70 DEG C.
Water is padded below sweating ware ware plate.The sealing system on installation sweating ware top is simultaneously connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump；Start compressor and keeps pressurized buffer pressure inside the tank steady
It is scheduled on 3.2~3.4 atmospheric pressure（Gauge pressure）.
With 66#Scale wax（Gaoqiao Petrochemical Company company, 66.60 DEG C of fusing point, oil content 1.64%, isoparaffin content 53.12%,
C23Following content 1.20%, C39The above content 28.05%）For raw material, it is heated to after 70 DEG C of fusings in 3.2~3.4 atmospheric pressure
（Gauge pressure）Lower addition sweating ware.
（A2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 56.0 DEG C with
Wax layer is set to crystallize to form solid, and constant temperature 1.0h is so that wax layer crystallization is more abundant.The constant temperature stage is controlled by emptying system and is pressurizeed
Buffering pressure inside the tank is gradually decrease to normal pressure with the rate of 5.0 atmospheric pressure/h.Close the refrigerating function of the circulatory system.
（A3）Sweating
Sweating ware is discharged and pads water；Sweating ware outlet connection intermediate storage tank（Ⅰ）To receive under a wax；Start compressor and keeps
Pressurized buffer pressure inside the tank is stablized in 1.2~1.4 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Start cycle
The heating function of system makes wax layer temperature be increased to 60.0 DEG C and constant temperature 3.0h with the heating rate of 1.5 DEG C/h；Stop compressor.
Sweating ware exports the thick intermediate products storage tank of changing-over（Ⅰ）To receive under two waxes, i.e., thick intermediate products（Ⅰ）；Start vacuum
It pumps and pressure-reducing cushioning pressure inside the tank is kept to stablize in -50~-70 KPa（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue with
The heating rate of 1.5 DEG C/h makes wax layer temperature be increased to 69.0 DEG C and constant temperature 3.0h；Stop vacuum pump, terminates sweating effort.Sweating
Ware outlet is changed to connection intermediate storage tank（Ⅱ）；Continue heat cycles water and is warming up to 80 DEG C on fusing taking-up wax.
（A4）It is refined
Thick intermediate products storage tank（Ⅰ）In two wax the following group lease makings washing, it is clay-filtered after be intermediate products（Ⅰ）.
Intermediate products（Ⅰ）Property：66.35 DEG C of fusing point, oil content 0.42%, isoparaffin content 61.35%, C23Following content
0、C39The above content 1.03%.
B is allocated：
By alpha-olefin C2428（Chevron Phillips Products, C24~C28 Alpha-olefin content ＞ 72%, fusing point 61.7
DEG C, needle penetration 95（0.1mm））With intermediate products（Ⅰ）It is 15 by weight：85 ratio heating is melted and is uniformly mixed, and is molded
It is preventing rubber wax product afterwards（Ⅰ）.
Embodiment 2
The present embodiment includes：A sweatings and B allocate two parts.
A：Sweating
This part includes：（A1）Preparation,（A2）Crystallization,（A3）Sweating,（A4）The processes such as refined.
（A1）Preparation
Sweating ware chuck and removable coil pipe are connect with the circulatory system, coil pipe is fixed on sweating ware；It is to be situated between with water
Matter；The heating function for starting the circulatory system, makes recirculated water be warming up to 70 DEG C.
Water is padded below sweating ware ware plate.The sealing system on installation sweating ware top is simultaneously connect with pressurized buffer tank and compressor
It is good；Pressure-reducing cushioning tank is installed in sweating ware lower part and connects vacuum pump；Pressurized buffer tank emptying system and sweating ware lower part are arranged
Gas port is connected with absorption system respectively, using 5% NaOH solution as absorbing medium.
Start compressor and pressurized buffer pressure inside the tank is kept to stablize in 3.2~3.4 atmospheric pressure（Gauge pressure）.It grinds and sieves
Separate the sodium bicarbonate of the mesh of 100 mesh~200.
With 66#Scale wax（With embodiment 1）For raw material, it is heated to after 70 DEG C of fusings in 3.2~3.4 atmospheric pressure（Gauge pressure）
The aforementioned sodium bicarbonate powder of lower incorporation 1.0%, is added sweating ware after mixing；Pressurized buffer pressure inside the tank is kept to stablize
3.2~3.4 atmospheric pressure.
（A2）Crystallization
Start the circulatory system refrigerating function, control wax layer temperature with the rate of temperature fall of 2.0 DEG C/h drop to 56.0 DEG C with
Wax layer is set to crystallize to form solid, and constant temperature 1.0h is so that wax layer crystallization is more abundant.The constant temperature stage is controlled by emptying system and is pressurizeed
Buffering pressure inside the tank is gradually decrease to normal pressure with the rate of 5.0 atmospheric pressure/h.The constant temperature stage gas of discharge passes through 5%
NaOH solution decomposes the carbon dioxide generated to absorb sodium bicarbonate.Close the refrigerating function of the circulatory system.
（A3）Sweating
Sweating ware is discharged and pads water；Sweating ware outlet connection intermediate storage tank（Ⅲ）To receive under a wax；Start compressor and protects
Pressurized buffer pressure inside the tank is held to stablize in 1.2~1.4 atmospheric pressure（Gauge pressure）, sweating ware ware plate lower section keeps normal pressure；Startup follows
The heating function of loop system makes wax layer temperature be increased to 60.0 DEG C and constant temperature 3.0h with the heating rate of 1.5 DEG C/h；Stop compressing
Machine.
Sweating ware exports the thick intermediate products storage tank of changing-over（Ⅱ）To receive under two waxes, i.e., thick intermediate products（Ⅱ）；Start true
Sky pumps and pressure-reducing cushioning pressure inside the tank is kept to stablize in -50~-70 KPa（Gauge pressure）, wax layer top air pressure holding normal pressure；Continue
Wax layer temperature is set to be increased to 69.0 DEG C and constant temperature 3.0h with the heating rate of 1.5 DEG C/h；The gas being discharged in sweating effort passes through
5% NaOH solution decomposes the carbon dioxide generated to absorb sodium bicarbonate.
Stop vacuum pump, terminates sweating effort.The outlet of sweating ware is changed to connection intermediate storage tank（Ⅳ）；Continue heat cycles water liter
Temperature is taken out with fusing on wax to 80 DEG C.
（A4）It is refined
Thick intermediate products storage tank（Ⅱ）In two wax the following group lease makings washing, it is clay-filtered after be intermediate products（Ⅱ）.
Intermediate products（Ⅱ）Property：66.46 DEG C of fusing point, oil content 0.19%, isoparaffin content 66.28%, C23Contain below
Amount 0, C39The above content 0.33%.
B is allocated：
By alpha-olefin C2428（With embodiment 1）With intermediate products（Ⅱ）It is 30 by weight：70 ratio heating melting is simultaneously
It is uniformly mixed, is preventing rubber wax product after molding（Ⅱ）.
Comparative example 1
Patent CN01106005.0 discloses a kind of Wax-for preventing rubber, it is by low melt point paraffin, high melting point paraffin, crystallite
Wax and polyethylene wax are made, and the proportioning of embodiment 2 is low melt point paraffin（No. 60）：25%；High melting point paraffin（No. 62）：52%；
Microwax（No. 85）：21%；Polyethylene wax（Molecular weight 5000-10000）：2%.
By 2 product of embodiment and common 58 in product of the embodiment of the present invention, comparative example CN01106005.0#Paraffin is mixed respectively
Mix progress barrier propterty comparison in rubber.
Experimental rubber dispensing（Parts by weight）As shown in the table：
| Raw material | Parts by weight | Raw material | Parts by weight |
| Natural rubber | 50 | Butyl rubber BR | 50 |
| Zinc oxide | 5 | Aliphatic acid | 1 |
| Carbon black（HAF） | 60 | Talcum powder | 40 |
| Pulverized sulfur | 1.5 | Vulcanization accelerator（TMTD） | 1 |
| Operation oil | 15 | Wax | 2 |
Physical properties are measured after above-mentioned sample is vulcanized 65 min at 150 DEG C, it is as a result as follows：
| Wax type | Pull apart strength, MPa | Elongation at break, % | 300% stress at definite elongation, MPa | 500% stress at definite elongation, MPa | Hardness（Shao Er A）Degree |
| No. 58 paraffin | 24.2 | 735 | 13.6 | 4.8 | 54 |
| Comparative example | 24.7 | 780 | 11.2 | 4.4 | 52 |
| Embodiment 1 | 24.6 | 778 | 12.9 | 4.5 | 56 |
| Embodiment 2 | 24.8 | 772 | 12.5 | 4.7 | 54 |
As can be seen from the above table, using the rubber system prepared by the Wax-for preventing rubber of this patent embodiment 1 and embodiment 2
Product, every physical index are all suitable with comparative example.
Weather experiment is carried out to the rubber sample after above-mentioned vulcanization, it is as a result as follows：
As can be seen from the above table, the protection using the Wax-for preventing rubber of Example 1 and Example 2 of the present invention to rubber product
Performance is significantly improved.
By embodiment 1-2 can be seen that the present invention production novel rubber protective wax method, by increase pressurization and/
Or the improvement to sweatbox such as vacuum facility；Short space is formed in wax layer using inorganic salts decomposition, and in sweating effort
In force air flow through wax layer and increase the improvement to sweating process such as constant temperature stage；It enhances the separating effect of wax and oil and adds
Fast separating rate, has effectively removed the non-suitable component of Wax-for preventing rubber in paraffin grade wax, then allocate and produce with alpha-olefin
Preventing rubber wax product, effectively increase the effective content of Wax-for preventing rubber and make product have suitable chemical composition, it is right
Rubber and its product have permanently effective protective action.
Claims (23)
1. a kind of method producing novel rubber protective wax, including the following contents：
A sweatings：Include the following steps：
（A1）Charging：It is less than 2.0%, paraffin that fusing point is 52 DEG C~72 DEG C in mass using oil content as raw material, after heating fusing
It is packed into sweatbox；
（A2）Crystallization：The predetermined temperature of 8 DEG C~20 DEG C of raw material fusing point or less is cooled to the rate of 1.0 DEG C/h~4.0 DEG C/h, and
Constant temperature is for a period of time；
（A3）Sweating：It is heated up with the rate of 0.5 DEG C/h~3.0 DEG C/h；When wax layer reaches one section of first predetermined temperature and constant temperature
Between, it is continuously heating to second predetermined temperature and constant temperature stops sweating afterwards for a period of time, forced air flow through in sweating effort
Wax layer；Continue heating to melt and take out on wax；First predetermined temperature is -10 DEG C of raw material fusing point~raw material fusing point -3
DEG C, second pre- constant temperature is -5 DEG C of raw material fusing point~+8 DEG C of raw material fusing point；
（A4）It is refined：It is spare after purpose group lease making is refined；
B is allocated：
By alpha-olefin that carbon number is 23 or more and above-mentioned sweating and it is refined after products therefrom be 10~40 by weight：60~90
Ratio heating is melted and is uniformly mixed, and is preventing rubber wax product after molding.
2. according to the method for claim 1, which is characterized in that step（A1）After middle raw material heating fusing under stress
Mix the inorganic salt powder that decomposable asymmetric choice net generates gas.
3. according to the method for claim 2, which is characterized in that the inorganic salt powder decomposes release in sweating effort
Go out gas, and itself and decomposition product are soluble easily in water.
4. according to the method for claim 2, which is characterized in that the inorganic salts are selected from ammonium salt, carbonate, bicarbonate
One or more of.
5. according to the method for claim 2, which is characterized in that the granularity of the inorganic salt powder is 50~500 mesh.
6. according to the method for claim 2, which is characterized in that the addition of the inorganic salt powder accounts for sweating raw material weight
The 0.1%~10.0% of amount.
7. according to the method for claim 2, which is characterized in that in step（A1）Charging and step（A2）The cooling of crystallization
Apply air pressure above wax layer in the process, the gas generated to inhibit inorganic salts to decompose escapes wax layer.
8. according to the method for claim 7, which is characterized in that the air pressure is 0.5~15.0 air of gauge
Pressure.
9. according to the method for claim 1, which is characterized in that step（A3）Described in force air flow through wax layer use
Increase air pressure above wax layer and/or reduce air pressure below wax layer, so that wax layer upper and lower is formed pressure difference and realize, the pressure
Force difference is 0.1~5.0 atmospheric pressure.
10. according to the method for claim 1, which is characterized in that step（A2）Described in the rate that cools down be 1.5 DEG C/h~
3.0℃/h。
11. according to the method for claim 1, which is characterized in that step（A2）Described in predetermined temperature be starting paraffin
10 DEG C~15 DEG C below fusing point.
12. according to the method for claim 1, which is characterized in that step（A2）Described in constant temperature time be 0.1~
3.0h。
13. according to the method for claim 1, which is characterized in that step（A2）In continuously decrease pressure while constant temperature
To normal pressure, the rate of the decompression is 0.1~150.0 atmospheric pressure/hour.
14. according to the method for claim 1, which is characterized in that step（A3）Described in the rate that heats up be 1.0 DEG C/h~
2.0℃/h。
15. according to the method for claim 1, which is characterized in that step（A3）Described in the constant temperature stage time be 0.1~
5.0 hour.
16. according to the method for claim 1, which is characterized in that step（A3）Described in the wax layer that forces air flow through exist
Sweating initial stage implements.
17. according to the method for claim 9, which is characterized in that step（A3）Described in the wax layer that forces air flow through adopt
Increase air pressure above wax layer to realize, applies the gauge of 0.2~2.0 atmospheric pressure above wax layer, and below wax layer
Remain normal pressure.
18. according to the method for claim 9, which is characterized in that step（A3）Described in the wax layer that forces air flow through adopt
It reduces air pressure below wax layer to realize, air pressure keeps normal pressure above wax layer, and maintains -0.2~-1.0 below wax layer
The gauge of atmospheric pressure.
19. according to the method for claim 2, which is characterized in that in step（A2）The thermostatic process and step of crystallization（A3）
Inorganic salts are absorbed using liquid absorption mode in sweating effort and decompose the gas generated, in step（A4）Water is used in subtractive process
The mode of washing removes unreacted inorganic salts and decomposition product.
20. according to the method for claim 1, which is characterized in that alpha-olefin and sweating and refined rear products therefrom in step B
Allotment weight ratio be 15~30：70~85.
21. according to the method for claim 1, which is characterized in that the sweatbox is sweating ware.
22. according to the method for claim 1, which is characterized in that C in the alpha-olefin23~C30Content is 60% or more.
23. according to the method for claim 6, which is characterized in that the addition of the inorganic salt powder accounts for sweating raw material
The 0.2%~3.0% of weight.
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