CN1325821A - Process for preparing molecular sieve-base micropowder material - Google Patents
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Abstract
A process for preparing molecular sieve-base micropowder material uses heavy intermediate-base petroleum asphalt, intermediate-base coal asphalt or petroleum coke as raw material, and includes such steps as physical crushing the carbon-contained raw powder, grinding, adding activating agent and high-temp. charring in inertial atmosphere and activating. Its advantages include high specific surface area greater than 2000 sq.m/g, low density, and high weatherability, high-and low-frequency electromagnetic wave absorption and resistance to oxidazation and corrosion.
Description
The invention belongs to electromagenetic wave radiation protection, microwave absorbing, novel molecular sieve and micropore micropowder material field.
Along with the high speed development of modern science and technology, increasing Electrical and Electronic equipment has been penetrated into each corner of society.People enjoy to the full the modern life convenient, comfortable in, a kind of invisible environmental pollution one electromagnetic environment is polluted and is also just quietly attacked, and becomes increasingly conspicuous.Now, countries in the world have all been recognized this problem, have carried out the research to hazards of electromagnetic radiation and protection in succession, and make the electromagnetic radiation hygienic standard.China is no exception, is no more than 20V/m with strength of electric field for high frequency electromagnetic radiation in real work, and magneticstrength is no more than 5A/m as the reference standard.
Hertzian wave has following harm:
1, electromagnetism damage
Hazards of Electromagnetic Radiation is relevant with wave frequency.From a security point of view, the harm maximum of radio-frequency radiation.Radio-frequency radiation is often referred to frequency respectively at frequency electromagnetic waves and the microwave of 100kHz～300MHz and 300～300000MHz.Radio-frequency radiation is a kind of combined effect to health effects, and is relevant with multiple factors such as electromagnetic radiation intensity, duration of contact, equipment protection measures, presents complicacy.This complicacy shows as electromagnetic radiation " three property ": (1) electromagnetic radiation raises a certain portion temperature of whole body or health in human body, produces macroscopical thermal effect; (2) electromagnetic radiation makes intraorganic some part produce the microcosmic thermal effect in human body, though temperature does not obviously change, body can produce lasting variation; (3) the outer effect of the heat of electromagnetic radiation still has strong influence to body biophysics or biological process on microcosmic, this influence is complexity but also meticulous not only, and is to take place on the level of molecule and cell one-level.
Human body central neural system and the system function disorder of the refreshing footpath of plant can be caused in the higher frequency electromagnetic field,, poor appetite bad, alopecia, hidrosis as dizziness, malaise, hypomnesis, sleep, ECG change such as the visible arrhythmia of cardiovascular systems, bradyrhythmia.
Microwave mainly shows neuroendocrine system and cardiovascular systems to the influence of human body, and the people who is engaged in the microwave operation for a long time often has more neurasthenia symptom, ECG change such as the visible arrhythmia of cardiovascular systems, bradyrhythmia.In addition, microwave also can cause abnormal symptoms such as crystalline lens, surrounding hemogram and sexual function change.
2, electromagnetic interference
Electromagnetic radiation can directly have influence on the normal operation of electronics in the every field, instrument, causes the electromagnetic interference to working equipment.On the one hand, electromagenetic wave radiation causes interference to electronic electric equipment on every side, produces misoperation; On the other hand, itself to around electromagnetic interference very responsive again, thereby cause serious social concern such as computerized information leakage.In case the generation electromagnetic interference might cause catastrophic consequence.With regard to once taking place, a cause electromagnetic interference heart was opened fight device malfunctioning and make the lethal incident of patient as the U.S..In addition, in the last few years, because of electromagnetic interference makes the malfunctioning report of airplane crash incident that causes of Aircraft Vectoring System also of common occurrence.The electromagnetic interference source category is a lot, by sources can be divided into two classes: artificial interference source and natural interference source.The natural interference source comprises the sky noise that thunderstorm, lightning produce, sunspot blast and the movable noise that is produced and the cosmic noise of milky way system.The artificial interference source is by electromagnetic interference dynamo-electric or that other Prosthesis produces, comprises Industrial Scientific Medical radio-frequency apparatus, ac high-voltage transmission line, igniter for automobile, microwave oven, transfer lever, emitter etc.Because the artificial interference source category is in continuous increase, and strength ratio natural interference source is big, and is current, artificial electromagnetic interference has become main source.
3, mobile communication microwave radiation
Developing rapidly of current wireless communication industry makes the telex over radio broadcast mode increasing.Mobile phone enjoys people's favor because it is multiple functional, easy to carry.But its electromagnetic-wave leakage causes people's attention day by day.Studies have shown that the microwave electromagnetic radiation can cause the illness of aspects such as living organism, nervus centralis, cardiovascular systems, crystalline lens, blood.Regulation exposure in 8 hours on the continuous one continuous wave average power density is 50uwcm among China GB10436-89 " operation place microwave radiation hygienic standard ", and per daily dose is 400uwhcm.This investigation is learnt: the microwave of mobile phone and interphone belongs to the continuity electromagenetic wave radiation, and no matter is Motorola type mobile phone or siemens's interphone, and microwave leakage is all higher; And antenna position is the highest, and secondly receiver portion (being subjected to words portion) is figure disc and telephone transmitter secondly again.Especially emission state.The moment microwave of the antenna part of mobile phones such as interphone and some Motorola leaks and can limit the quantity of considerably beyond national per daily dose standard.And interphone antenna position microwave leak can be the highest, up to 10640uwcm (＞10mwcm).As seen most of duration of service cellular telephone day are slightly long, promptly surpass 400uwhcm per daily dose limit value.Electromagnetic radiation intensity and square distance are inversely proportional to.By this point is also verified in the test of 5 centimetres and 10 centimetres different distance of words in moving.So the suggestion user is not influencing under the obedient prerequisite, as far as possible quiet environment or remote the use.Especially under emission state.Interphone or mobile telephone, all near human body head, the microwave energy that mobile phone leaks is almost all absorbed by people's brain during use.Reported in literature, brain be human body to the sensitive part of microwave radiation, brain is subjected to the microwave radiation of hard intensity like this.Its harm is serious.As seen to the protection of the microwave radiation of mobile telephone, and user's health supervision is to reduce microwave to one of effective measure of human body harm.
Because popularizing of mobile telephone, the mobile communication base station spreads all over the place, and build the dwelling house or the commercial zone of urban district population comparatively dense in more, and the pollution of Electromagnetic Radiation on Environment causes the public's concern day by day.
4, microwave oven electromagnetic radiation
Microwave is electromagnetic a kind of, and frequency is 300MHz～300GHz, and wherein 2450MHz is the operating frequency of household microwave oven.Continued the beginning of the fifties first household microwave oven by since U.S. development and formally putting goods on the market, and the kind of household microwave oven, performance and sales volume develop rapidly.Household microwave oven has not only thoroughly been eliminated people, and extremely the high temperature fire is roasting, the kitchen hard work that oil smoke is choked, and also more Modern Family creates the life that high quality improves grade, and has showed tempting prospect.Especially in the later stage seventies, states such as Japan, Korea S catch up from behind, and also become big producing country, and the volume of production and marketing of this three state has reached more than 60% of international marketing total amount.China's microwave oven industry is started late, and the initial stage eighties just begins development, produces.But mainly also be in the stage that the assembling of import loose mail is produced, the enterprise that can really form scale production is but few for number.Enter the nineties, along with developing by leaps and bounds of national economy, improving constantly of living standards of the people, the particularly quickening of life of urban resident rhythm, people need a kind of conveniently household appliances to replace heavy kitchen work, just progressively accepted by China people so have the microwave oven of characteristics such as saving time, laborsaving, energy-conservation, clean, microwave oven market has begun real startup.The production that starts one after another of initial stage nineties domestic production producer is produced and is mainly concentrated on Guangdong, two places, Shanghai.Simultaneously, overseas some major companies also adopt mode such as holding, joint to seize Chinese market one after another.At present the enterprise that produces has at home reached family more than 30, shows according to statistical figure in 1997, surplus the annual production of China's microwave oven has reached 400 ten thousand, become the 4th big producing country after the U.S., Japan, Korea S, and majority is a joint venture using Chinese and foreign investment.At present, the tame microwave oven in Glanz, Shuande, Guangdong one manufacturing enterprise only, annual production promptly reaches 1,200 ten thousand, and it is visible that microwave oven market is big both at home and abroad.
The heating principle microwave heating of microwave oven is food when being subjected to microwave radiation, and its interior molecules is transformed into heat energy with microwave energy absorbed, and the temperature of food is raise.Microwave is a kind of hertzian wave, and real mainly is electric field energy to the food heat effect.We know that heated food product is made up of many polar molecules with positive and negative electric charge, and positive and negative electric charge is to be the arrangement of not planning when added electric field not.After adding electric field, polar molecule will rotate to along direction of an electric field and arrange.The change of direction of an electric field makes the also corresponding rotary oscillation of polar molecule, under the effect of high-frequency electric field, owing to the molecule in the food swings back and forth acutely, thereby causes frictional heating, and produces heat.The wave band majority of household microwave oven utilization is the ultrashort wave of 2450MHz, that is to say that water molecules in the food wants changed polarity 2,450 1,000,000 times in 1 second, just under these circumstances, phase mutual friction and collision between the water molecules, produced a large amount of heat, and these heat are absorbed by food molecule, and food is just " it is ripe to shake " also.
The safety problem microwave oven of microwave oven in use, the microwave in the stove might leak out, and a large amount of microwave radiations can damage human body.In order to ensure user's health, all corresponding leakage standard of having formulated microwave oven of a lot of in the world countries, these standards mostly are defined under the regular service condition, and from microwave oven 5cm place, every square centimeter yield of radiation must not surpass 5mw.Evidence is when human body is exposed to 700mw/cm
2In the microwave of above intensity, the pain sensation will appear in skin in ten minutes.Especially people's eyes, owing to there is not the covering of fat, moisture is more again, does not have the blood vessel heat radiation in the crystal, microwave will be more obvious to the damage that it causes.
The harm that electromagnetic radiation causes is increasing, therefore must take practical measures to be protected.At present, main safeguard procedures have: shielding, filtering, absorption etc.The mechanism of electromagnetic shielding is electromagnetic induction phenomenon.Under extraneous alternating electromagnetic field, by electromagnetic induction, produce induced current in the shield shell, and this electric current has produced the electromagnetic field opposite with the external electromagnetic field orientation at shielding space, thereby offset external electromagnetic field, reach shield effectiveness.The electromagnetic interference process must possess three elements: electromagnetic interference source, electromagnetic susceptibility equipment, route of transmission, the three is indispensable.Adopt shielding measure, can suppress the interior hertzian wave of shielded cell on the one hand and leak, suppress electromagnetic interference source, also can prevent in the external electromagnetic waves inlet chamber on the other hand.But, since the difference of shielding material surface action, the key that is selected to the shield effectiveness quality of material.The attenuation of Electromagnetic factor alpha is to weigh decay in the conductor material parameter of speed of hertzian wave, and α is big more, decays soon more, and shield effectiveness is good more.Therefore, good conductor such as iron (steel), aluminium, copper just are commonly used to as electromagnetic screen, and all coil outer masks the aluminum hull of a hollow in the receiving set, are wrapping oscillatron with iron sheet in the electron oscillograph, or the like, these all are electromagnetic shielding concrete application in practice.
High frequency earthing can further suppress electromagnetic radiation.High frequency earthing comprises the ground connection of high-frequency apparatus shell and the ground connection of shielding.Shielding unit can improve shield effectiveness after good ground connection has been arranged, and is comparatively obvious with medium wave band.Shield earthing generally adopts single-point grounding, and individual cases such as large-scale shielded cell are advisable with multipoint earthing.The grounding wire of high frequency earthing is unsuitable oversize, and its length preferably can be limited in the wavelength 1/4, even can't reach this requirement, also should avoid the odd-multiple of wavelength 1/4.
Filtering is to suppress one of effective means of electromagnetic interference.Aspect the conduction that tackles electromagnetic interference signal and some radiation interference, the power supply Electromagnetic interference filter is quite effective device.For example, the high-frequency apparatus supply lead can cause the conduction coupling, so that causes leakage and interference, and the active shielding chamber is not as taking measures to the device power supply (DPS) line, can influence shield effectiveness because lead disturbs, solving lead interferential effective way is to enter the shielded cell place at supply lead power filter is installed.The installation of wave filter is ground proximity as far as possible, and it is long and increase its impedance coupling to go into the path, ground with the vagabond current of non-filter, reduces filter effect.
For radio frequency, particularly microwave radiation also often utilizes absorbing material to carry out microwave absorbing.It is to develop according to the coupling resonance principle, and micro-wave energy is converted into heat energy.The scheme of microwave absorbing has two: (1) only is attached on cover body or the baffle with absorbing material the electromagnetic radiation wave energy is absorbed; (2) absorbing material is attached on shielding material cover body and the baffle, further slackens the transmission of radio frequency electromagnetic.
Except that above-mentioned safeguard procedures, strengthen individual protection, as wear special metallic plastron, wear special metal helmet and Metal Eyeglasses also is the effective measure that further suppress electromagnetic radiation.In addition, as technical measures, also can be by improving the design of high-frequency apparatus and feeder line thereof, to reduce its radiation power; Each high-frequency apparatus of reasonable Arrangement is to reduce the electromagnetic intensity of operating station.
Along with the development of technology such as microwave communication, radar, space flight, electronic countermeasure, electric wave absorbing materials more and more is subject to people's attention, and research is being goed deep into, and is widening in the field of application.Stealth technique has become the great technical progress of the balance of military power; and microwave absorbing material is the base mateiral of stealth technique; remove and be applied to stealth aircraft; outside on the cruise missile; also be used to be coated in artillery in a large number; tank; missile launcher and weapon depot outside; make these military equipments and facility become the blind area of the various radar microwave signals of enemy; play protection oneself; hit enemy's effect; it also is very important that civilian and technical skill aspect developing is used various electric wave absorbing materials; developing rapidly of world today's electronic industry; all like microwave ovens; beeper; mobile telephone; televisor; home electronicss such as computer increase day by day; electromagenetic wave radiation has become people and has been subjected to the hertzian wave that can't feel and pollutes, and becomes society's one big public hazards and new environmental pollution.Therefore, carry out microwave absorbing material militarily with civilian on research have great importance.
Electromagnetic wave absorbent material is that electromagnetic wave energy is absorbed the energy (mainly being the heat energy form) that is converted into other form the biglyyest, represent with loss tangent as loss: the former is dielectric loss for tg δ=tg δ e+tg δ m=ε " ε '+μ " μ ', and the latter is a magnetic loss.Bigger as absorbing material complex permittivity imaginary part ε " and complex permeability imaginary part μ ", its absorbing property is all right.
Through the exploration of two more than ten years, domesticly had suitable basis in the absorbing material field.At present, the absorbing material of domestic research mainly contains inorganic and organic two big classes:
Inorganic materials also can be subdivided into: ferrite wave-absorbing material, metal fine powder absorbing material, polycrystalline iron fiber absorbing material etc.Ferrite Material occupies critical role in the radio-radar absorber field always, particularly the VHF/UHF frequency range (＜1GHz), its wave-absorbing effect is superior.But the ferrite absorption agent is in the higher frequency range of frequency, and assimilation effect is undesirable.Also there are shortcomings such as density is big, weather resisteant difference in the ferrite absorption agent in addition.Characteristics such as temperature stability is good owing to having for the metal powder absorption agent, microwave magnetic permeability is big, specific inductivity is big, thereby research is more active, metal current powder absorption agent mainly contains two classes: a class is a metal carbonyl powder, as carbonyl Fe, and carbonyl Ni, carbonyl Co.Another kind of is nano-metal ultrafine powder, and its granularity is 20nm ~ 1.5 μ m.At present, domesticly also further investigate in this respect, but the problem that also exists some to be difficult to overcome,, problems such as proportion too big and anti-oxidant, acid-alkali-corrosive-resisting ability little as the low frequency magnetic permeability.
The organic absorbing material that grew up in recent years has conduction high polymer absorbing material, hand to levy medium absorbing material etc.Wherein, the conduction high polymer absorbing material presents good radar wave absorption characteristic in the microwave section, but extremely low in its magnetic loss of low frequency range.It is on the basis of traditional absorption agent that hand is levied the medium absorbing material, introduces to revolve ripple amount ξ, particularly adds in the absorbing material based on magnetic loss, can effectively improve specific absorption, and the broadening absorption band in recent years, has become the hot topic of research.Hand is levied the medium absorbing material owing to need bigger thickness, and simultaneously, heatproof, wet fastness are poor, from the coated material practicality big distance are arranged still at present.
In a word, the domestic in recent years research in the absorbing material field is very active, has obtained significant progress, but relatively lags behind with abroad comparing also, particularly in fundamental research fields such as wave-absorbing mechanisms.So domestic research in the absorbing material field does not all have big breakthrough, also has suitable distance from practicality always.Simultaneously, shielding, the filtering technique of eliminating electromagnetic radiation at present can only reduce radiation to a certain extent, can not fundamentally eliminate electromagnetic radiation, and the equipment complexity, the cost height.The most promising at present be the exploitation high-performance, low cost, broadband, concoct novel wave-absorbing material easily.
Purpose of the present invention is exactly the above-mentioned deficiency that overcomes prior art, provide a kind of good at height frequency range wave-absorbing effect, density is low, weather resisteant good, anti-oxidant, corrosion resistant Multifunction material and its manufacture method.
The present invention is a kind of manufacture method of molecular sieve-base micropowder material, and this method comprises the steps:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: with the NaOH, the KOH that pulverize by weight 1: 0.1-6: the composite mixing of ratio, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then.
The another kind of manufacture method that belongs to the molecular sieve-base micropowder material of same inventive concept with such scheme comprises the steps:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: NaOH or KOH are pulverized, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then.
Compare with prior art, the molecular sieve-base micropowder material of being made by method of the present invention is good at height frequency range wave-absorbing effect, density is low, weather resisteant good, anti-oxidant, corrosion-resistant
Describe the present invention in detail below with reference to embodiment.
The manufacture method of molecular sieve-base micropowder material of the present invention comprises the steps:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: with the NaOH, the KOH that pulverize by weight 1: 0.1-6: the composite mixing of ratio, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then.
The another kind of manufacture method of molecular sieve-base micropowder material of the present invention is that activator and aforesaid method are had any different, and all the other steps are identical, and activator is wherein made NaOH or KOH pulverizing.
The granularity of the former powder of carbon containing of described pulverizing is the 150-300 order.
Former powder of carbon containing and activator by weight 1: the mixed of 0.2-10 is even.
Described temperature is up to 1200 ℃.
Described temperature range is 300-1200 ℃.
Described elevated temperature is divided into two stages, and fs 300-600 ℃, stop then heating up, charing 5-200min, subordinate phase heats up 600 ℃-1200 ℃ from being not less than 500 ℃, activation 1-200min.
Can also sneak into the Co (NO that is not higher than 4 parts by weight in the described activator
3)
3Ni (the NO that is not higher than 4 parts by weight
3)
2
Described washing uses a small amount of method repeatedly of distilled water to carry out.
The mixing step of former powder of the carbon containing of described pulverizing and activator is: take by weighing respectively in proportion by the former powder/activator of carbon containing, then activator is dissolved in isopyknic distilled water, the more former powder of carbon containing is poured into and fully stirred, it is mixed.
Described drying is seasoning or heat drying.
Described inert atmosphere can be nitrogen, helium, argon gas, CO
2Or vacuum.
Embodiment 1:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: with the NaOH, the KOH that pulverize by weight 1: 0.1-6: the composite mixing of ratio, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then, makes molecular sieve-base micropowder material.
Embodiment 2:
Except that NaOH, KOH mixed in 1: 0.1 by weight, other step was with embodiment 1.
Embodiment 3:
Except that NaOH, KOH mixed in 1: 1 by weight, other step was with embodiment 1.
Embodiment 4:
Except that NaOH, KOH mixed in 1: 3 by weight, other step was with embodiment 1.
Embodiment 5:
Except that NaOH, KOH mixed in 1: 6 by weight, other step was with embodiment 1.
Embodiment 6:
Except that with former powder of carbon containing and 1: 0.1 by weight the mixed of activator, other with
Embodiment 1-5.
Embodiment 7:
Except that with former powder of carbon containing and 1: 1 by weight the mixed of activator, other is with embodiment 1-5.
Embodiment 8:
Except that with former powder of carbon containing and 1: 10 by weight the mixed of activator, other is with embodiment 1-5.
Embodiment 9:
Except that with former powder of carbon containing and 1: 20 by weight the mixed of activator, other is with embodiment 1-6.
Embodiment 10:
Except that with former powder of carbon containing and 1: 50 by weight the mixed of activator, other is with embodiment 1-6.
Embodiment 11:
Except that with the former powder of carbon containing and activator by weight 1: the mixed of 0.2-10, other is with embodiment 1-6.
Embodiment 12:
Except that with former powder of carbon containing and 1: 0.2 by weight the mixed of activator, other with
Embodiment 1-6.
Embodiment 13:
Except that with former powder of carbon containing and 1: 5 by weight the mixed of activator, other is with embodiment 1-6.
Embodiment 14:
Except that activator used NaOH or KOH, other conditioned disjunction step was with embodiment 1-13.
Embodiment 15:
Except that the granularity of the former powder of carbon containing was chosen 100 orders, other was with embodiment 1-14.
Embodiment 16:
Except that the granularity of the former powder of carbon containing was chosen 150 orders, other was with embodiment 1-14.
Embodiment 17:
Except that the granularity of the former powder of carbon containing was chosen 300 orders, other was with embodiment 1-14.
Embodiment 18:
Except that the granularity of the former powder of carbon containing distributed between the 100-300 order, other was with embodiment 1-14.
Embodiment 19:
Removing the charing temperature is 300-600 ℃, and activation temperature is outside 600-1200 ℃, and other is with embodiment 1-19.
Embodiment 20:
Removing the charing temperature is 300 ℃, and activation temperature is outside 600 ℃, and other is with embodiment 1-19.
Embodiment 21:
Removing the charing temperature is 300 ℃, and activation temperature is outside 900 ℃, and other is with embodiment 1-19.
Embodiment 22:
Removing the charing temperature is 300 ℃, and activation temperature is outside 1200 ℃, and other is with embodiment 1-19.
Embodiment 23:
Removing the charing temperature is 400 ℃, and activation temperature is outside 600 ℃, and other is with embodiment 1-19.
Embodiment 24:
Removing the charing temperature is 400 ℃, and activation temperature is outside 900 ℃, and other is with embodiment 1-19.
Embodiment 25:
Removing the charing temperature is 400 ℃, and activation temperature is outside 1200 ℃, and other is with embodiment 1-19.
Embodiment 26:
Removing the charing temperature is 600 ℃, and activation temperature is outside 600 ℃, and other is with embodiment 1-19.
Embodiment 27:
Removing the charing temperature is 600 ℃, and activation temperature is outside 900 ℃, and other is with embodiment 1-19.
Embodiment 28:
Removing the charing temperature is 600 ℃, and activation temperature is outside 1200 ℃, and other is with embodiment 1-19.
Embodiment 29:
In embodiment 1-19, described elevated temperature can be divided into two stages, at first temperature is risen to 300-600 ℃, charing 5-200min can not make temperature be reduced to below 500 ℃ at this, then from being not less than 500 ℃ of intensifications, reach 600 ℃-1200 ℃, activation 1-200min.Temperature is high more, and charing and activatory time are short more.
Embodiment 30:
Can also sneak into the Co (NO that is not higher than 4 parts by weight in the described activator
3)
3, preferably not being higher than 2.8 parts by weight, other is with embodiment 1-29.
Embodiment 31:
Can also sneak into the Ni (NO that is not higher than 4 parts by weight in the described activator
3)
2, preferably not being higher than 2.8 parts by weight, other is with embodiment 1-30.
Embodiment 32:
The former powder of the carbon containing of described pulverizing can be direct mixing with mixing of activator, also can mix as follows, promptly take by weighing respectively in proportion, activator is dissolved in isopyknic distilled water then by the former powder/activator of carbon containing, again the former powder of carbon containing is poured into and fully stirred, it is mixed.Other is with embodiment 1-31.
Method according to the foregoing description all can be made the molecular sieve-base micropowder material that meets the object of the invention.The present invention has following characteristics:
(1) prepared product belongs to novel carbonaceous molecular sieve (＞2000m
2/ g) type crystalline state carbon materials;
(2) technology is simple, and charing, activation and molecular sieve condition are approaching, can finish in a step;
(3) reaction conditions gentleness, the time is very short, and very high production efficiency is arranged;
(4) the product endoporus prosperity of manufacturing, wave-sucking performance is strong, can be used as military and civilian Microwave Absorption Coating material;
(5) the charged ability of product is strong, is fine electrical condenser and electrode materials;
(6) the manufacturing product is easy to and the coating compatibility, and is easy to use.
Use the made molecular sieve-base micropowder material of the inventive method can make the molecular sieve-base micropowder antiradar coatings.This coating is made up of two portions, and wherein most critical is the microwave absorbing base mateiral, and an other class is cakingagent or solidifying agent.This class solidifying agent can be liquid epoxy type or resin type coating, also can be solids epoxy type or resin type coating.During use, generally be that base mateiral is composite by different technology with the solidifying agent of definite composition, brush or spray to designated surface then.
The molecular sieve-base micropowder material outward appearance black that the inventive method makes, internal void prosperity, specific surface are big, absorption, a class microcrystalline molecular sieve type carbon element micropowder material that receptivity is strong.This class micropowder material has micropore very flourishing and that distribute and concentrate, generally is distributed between the 5-10A.This class carbon element micropowder material has regular crystalline structure and a large amount of delocalization unbound electrons, thereby has very high electroconductibility.Very flourishing micropore makes directed down the moving of the electromagnetic outside effect of delocalized electron in this class novel molecular sieve base micro mist suction ripple base mateiral simultaneously, also can produce transient magnetic field around it, has certain magnetic diffusivity.Therefore, if novel molecular sieve base micro mist is inhaled ripple base mateiral reasonable in design, can satisfy wave-absorbing effect fully, thoroughly to stop the electromagnetic radiation of microwave.In addition, this class carbon also has characteristics such as antioxygen, high temperature resistant and chemical stability be good, has a wide range of applications.
The method that the molecular sieve-base micropowder material that uses the inventive method to make is made absorbing material is as follows:
A) composite with solid curing agent
Epoxy type or resin type solid coating are inhaled the ripple base mateiral with this molecular sieve analog base micro mist under certain condition and can be merged well, are good solidifying agent.Select epoxy type or resin type solid coating, in inhaling ripple base mateiral/solidifying agent=2-80: 100 ratio is mixed, be ground to the 200-300 order then, carry out Electrostatic Treatment, and be pressed into solid piece, and pulverize again, be ground to the 200-300 order, electrostatic spraying gets final product in 200 ℃ of oven dry to all kinds of implements surface again then.
B) composite with liquid curing-agent
Select epoxy type or resin type solid coating, in inhaling ripple base mateiral/solidifying agent=20-50: 100 ratio is mixed, and is ground to the 200-300 order, adds solvent then, and wiring solution-forming is brushed to all kinds of implements surface, dry getting final product.
As the ratio according to the former powder of carbon containing/composite activator powder=1: 3, the novel molecular sieve base wave-absorbing material fundamental property of handling the back gained according to above-mentioned charing, activation etc. is as follows:
(1) basic physicals
Specific surface area: 3734.90m
2/ g; Middle aperture surface area: 2697.63m
2/ g;
Micropore pore volume: 0.92cm
3/ g; Average micropore size: 0.60nm;
Mesopore volume: 1.84cm
3/ g; Mean pore size: 2.36nm;
Total pore volume: 2.21cm
3/ g; Tap density: 0.23g/ml.
(2) electromagnetic parameter
Novel molecular sieve base wave-absorbing material basic electromagnetic parameter
| ????f(GHz) | ????ε’ | ????ε” | ????μ’ | ????μ” |
| ????3.0 ????4.0 ????5.0 ????6.0 ????7.0 ????8.0 ????9.0 ????10.0 ????11.0 ????12.0 ????13.0 ????14.0 ????15.0 ????16.0 ????17.0 ????18.0 | ????55.02 ????41.00 ????36.98 ????47.17 ????33.89 ????28.31 ????31.54 ????32.02 ????27.76 ????26.42 ????28.31 ????26.25 ????24.81 ????23.43 ????22.01 ????20.97 | ????47.92 ????48.33 ????38.29 ????67.50 ????55.39 ????45.19 ????30.40 ????29.84 ????30.32 ????30.95 ????29.79 ????28.89 ????27.78 ????27.26 ????26.20 ????25.16 | ????0.84 ????0.84 ????0.87 ????0.60 ????0.71 ????0.81 ????0.90 ????0.85 ????0.89 ????0.86 ????0.83 ????0.85 ????0.86 ????0.87 ????0.90 ????0.92 | ????0.12 ????0.19 ????0.22 ????0.02 ????0.02 ????0.03 ????0.09 ????0.07 ????0.05 ????0.06 ????0.07 ????0.06 ????0.07 ????0.06 ????0.07 ????0.08 |
(3) microwave oven microwave leak detection
Door of microwave oven is the antetheca of furnace chamber, is the first road barrier that prevents microwave leakage.Fire door is made up of metal frame and glass window.The layer of metal net is arranged in viewing window, three kinds of devices that prevent microwave leakage are arranged on the fire door: the one, the wire netting in the viewing window, it plays shielding effect to hertzian wave; The 2nd, the sealed leak-proof device around the door; The 3rd, the microwave absorbing bar is inlayed on a limit, and two-door hook is housed in the fire door, and it is the linked switch of control power supply, and door opened moment cuts off the power supply automatically, to eliminate the leakage of microwave in the stove.The microwave oven microwave leak detection result of Haier
The molecular sieve-base micropowder material that the inventive method makes be except can doing to inhale the ripple base mateiral, can also be as other materials such as molecular sieves, thus have broad application prospects.
Above-mentioned just illustrative to the description of invention with reference to embodiment, and do not constitute qualification to it.For the person of ordinary skill of the art, on basis of the present invention, can carry out many modification or improvement, but not break away from essence of the present invention.
Claims (10)
1, a kind of manufacture method of molecular sieve-base micropowder material is characterized in that, this method comprises the steps:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: with the NaOH, the KOH that pulverize by weight 1: 0.1-6: the composite mixing of ratio, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then.
2, a kind of manufacture method of molecular sieve-base micropowder material is characterized in that, this method comprises the steps:
(1) pre-treatment of raw material: with heavy intermediate crude pitch, intermediate base ature of coal pitch or refinery coke is raw material, adopts the fragmentation of physical pulverization method, abrasive dust, makes it become 100-300 purpose fine powder;
(2) preparation activator: NaOH or KOH are pulverized, make the former powder of activator;
(3) with the former powder of above-mentioned carbon containing and activator by weight 1: the mixed of 0.1-50 is even, and it is fully contacted;
(4) charing and activation: with the above mixed raw material reactor of packing into, progressively elevated temperature at first makes the former burgyization of carbon containing in inert atmosphere, makes it activation then, stops heating at last, is cooled to room temperature under inert atmosphere protection;
(5) washing is with dry: reaction product is taken out from reactor, and the method that washes with water is washed it to the pH=7, and is dry then.
3, manufacture method according to claim 1 and 2 is characterized in that, the granularity of the former powder of carbon containing of described pulverizing is the 150-300 order.
4, manufacture method according to claim 1 and 2 is characterized in that, former powder of carbon containing and activator by weight 1: the mixed of 0.2-10 is even.
5, manufacture method according to claim 1 is characterized in that, the temperature range of described intensification is 300 ℃-1200 ℃.
6, manufacture method according to claim 5 is characterized in that, described elevated temperature is divided into two stages, fs 300-600 ℃, stop then heating up charing 5-200min, subordinate phase is warming up to 600 ℃-1200 ℃ from being not less than 500 ℃, activation 1-200min.
7, manufacture method according to claim 1 and 2 is characterized in that, can also sneak into the Co (NO that is not higher than 4 parts by weight in the described activator
3)
3Ni (the NO that is not higher than 4 parts by weight
3)
2
8, manufacture method according to claim 1 and 2 is characterized in that, described washing uses a small amount of method repeatedly of distilled water to carry out.
9, manufacture method according to claim 1 and 2, it is characterized in that, the mixing step of former powder of the carbon containing of described pulverizing and activator is: take by weighing respectively in proportion by the former powder/activator of carbon containing, activator is dissolved in isopyknic distilled water then, again the former powder of carbon containing is poured into and fully stirred, it is mixed.
10, manufacture method according to claim 1 and 2 is characterized in that, described drying is seasoning or heat drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00107740 CN1325821A (en) | 2000-05-25 | 2000-05-25 | Process for preparing molecular sieve-base micropowder material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00107740 CN1325821A (en) | 2000-05-25 | 2000-05-25 | Process for preparing molecular sieve-base micropowder material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348486C (en) * | 2004-12-01 | 2007-11-14 | 中国石油天然气股份有限公司 | Method for preparing nano-pore carbon molecular sieve with high specific surface area from petroleum coke |
| CN106190021A (en) * | 2016-07-10 | 2016-12-07 | 上海大学 | A kind of preparation method of zeolite absorbing material |
| CN115140736A (en) * | 2022-05-16 | 2022-10-04 | 中南大学 | Multi-component composite ferrite modified activated carbon, preparation method thereof and application thereof in desulfurization and denitrification |
-
2000
- 2000-05-25 CN CN 00107740 patent/CN1325821A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348486C (en) * | 2004-12-01 | 2007-11-14 | 中国石油天然气股份有限公司 | Method for preparing nano-pore carbon molecular sieve with high specific surface area from petroleum coke |
| CN106190021A (en) * | 2016-07-10 | 2016-12-07 | 上海大学 | A kind of preparation method of zeolite absorbing material |
| CN115140736A (en) * | 2022-05-16 | 2022-10-04 | 中南大学 | Multi-component composite ferrite modified activated carbon, preparation method thereof and application thereof in desulfurization and denitrification |
| CN115140736B (en) * | 2022-05-16 | 2023-09-19 | 中南大学 | Multicomponent composite ferrite modified activated carbon, preparation method thereof and application thereof in desulfurization and denitrification |
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