CN105399114B - Preparation method of non-agglomerated potassium carbonate ultra-fine powder - Google Patents
Preparation method of non-agglomerated potassium carbonate ultra-fine powder Download PDFInfo
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- CN105399114B CN105399114B CN201510787036.3A CN201510787036A CN105399114B CN 105399114 B CN105399114 B CN 105399114B CN 201510787036 A CN201510787036 A CN 201510787036A CN 105399114 B CN105399114 B CN 105399114B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/42—Preventing the absorption of moisture or caking
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a preparation method of non-agglomerated potassium carbonate ultra-fine powder, which comprises the following steps: adding a liquid anti-caking additive into calcined potassium carbonate with residual heat, and uniformly mixing; crushing the obtained potassium carbonate mixture, collecting particles of which the particle sizes are less than or equal to 100 micrometers, transferring the obtained potassium carbonate ultra-fine powder I into a transfer container, naturally cooling to room temperature, adding a solid anti-caking additive into the cooled potassium carbonate ultra-fine powder II, and stirring and mixing for the second time; and grading the obtained potassium carbonate ultra-fine powder III mixed for the second time, and collecting particles of which the particle sizes are less than or equal to 100 micrometers, thereby obtaining the non-agglomerated potassium carbonate ultra-fine powder. The obtained non-agglomerated potassium carbonate ultra-fine powder can be used for synthesizing herbicides including dicamba and quizalofop-p-ethyl as well as an antipsychotic drug, namely an aripiprazole key intermediate 2,3-dichloro-benzyl piperazine.
Description
Technical field
The invention belongs to chemical field, it is related to inorganic chemical industry and organic chemical industry's technology, more particularly to a kind of do not reunite
The preparation method of potassium carbonate superfine powder.
Background technology
Potassium carbonate is structure very clear and definite simple compound, is a kind of ancient and traditional chemical composition, is also
A kind of with enter generation science and technology progress and constantly give a kind of new product of its New function, new feature and new application.
Potassium carbonate, as a kind of inorganic salt basic chemical industry raw material, is the former of production potassium acetate, potassium fluoride, potassium arsenite and potassium sorbate
Material, is also commonly used for glass, chemical industry, medicine, pesticide and chemical fertilizer, with scientific and technological development, the purposes of potassium carbonate is more and more wider.
With the raising of living standards of the people, health is increasingly paid attention to, the consciousness of environmental conservation is also increasingly stronger, therefore
To pesticide it is also proposed that new requirement；Not only require effect good, also require low-residual, hypotoxicity and low cost, many organophosphors and
Organic sulfur class pesticide is gradually eliminated, many novel agrochemicals, due to having the advantages that hypotoxicity, low-residual and efficient specificity,
Therefore paid attention to, development is also rapid.
Wherein Mediben is exactly a good example.The novel herbicidal developed by Novartis as the sixties in last century
Agent, it have stronger selectivity, consumption few the features such as, be mainly used in the effect of Semen Tritici aestivi Deng He benzene section field prevent and kill off annual or
Perennial broad leaved weed.For a long time, because Mediben price is high, use cost is high, therefore its market focuses mostly in America and Europe
Developed country.Although demand is stable, development is relatively slower always, but from the beginning of 2009, Mediben demand rapid growth,
Mainly have benefited from new technology and reduce production cost, add that glyphosate is drug-fast and strengthen year by year, Mediben is brought to air port wave again
Point.
In process of production, potassium carbonate is its main raw material(s) to Mediben, often produces 1 ton of Mediben, about needs to consume 1 ton of left side
The potassium carbonate of right amount.In course of reaction, potassium carbonate is not homogeneous reaction (solid-liquid) with its material, and the granule of conventional potassium carbonate is big,
Good fluidity, but can not suspend, sedimentation velocity is fast, is unfavorable for the reaction between solid-liquid, catalytic performance is low, and the response time is long, secondary anti-
Ying Duo, causes that major product yield is low, the problem more than impurity.Mediben new technology and automated production are it is desirable to potassium carbonate particle diameter needs
Control below 100 microns, and do not allow caking of reuniting.
Due to reasons such as thermodynamics, electrostatic and liquid bridges, potassium carbonate superfine powder itself is always reunited together, adds potassium carbonate
Easily water suction itself is made moist, and conventional production process cannot accomplish its caking of not reuniting at all.Due to above-mentioned potassium carbonate nature
The reason it is impossible to produce superfine powder by synthesis technique, at present can only by pulverize this approach.Potassium carbonate be water solublity no
Machine salt is it is impossible to pass through waterproof pulverization, but it is serious to generate heat during dry pulverization process, and the potassium carbonate micropowder temperature after pulverizing is up to
70-80 DEG C, caking of at once will reuniting after pulverizing, mobility and suspendability are poor, are not suitable for the life of the organic synthesiss such as Mediben
Produce and require.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of potassium carbonate superfine powder (particle diameter≤100 micron) do not reunited
Preparation method.
In order to solve above-mentioned technical problem, the present invention provides a kind of preparation method of the potassium carbonate superfine powder do not reunited, bag
Include following steps:
1), toward after calcining, band is had a surplus in the potassium carbonate of warm (about 60-80 DEG C of temperature) and is added liquid anti-caking additive, uniformly
Mixing, the weight of liquid anti-caking additive and potassium carbonate ratio is for 0.1～0.3%；
2), by step 1) potassium carbonate mixtures of gained are pulverized, and collection cut size≤100 micron, after pulverizing
Potassium carbonate superfine powder；
3), by step 2) the potassium carbonate superfine powder of gained moves in transfer container, naturally cools to room temperature, after obtaining cooling
Potassium carbonate superfine powder；
4), to step 3) add the potassium carbonate superfine powder after accounting for cooling in potassium carbonate superfine powder after the cooling of gained
The solid anticaking agent of weight 0.2～1%, and carry out secondary stirring mixing (so that it is guaranteed that all potassium carbonate superfine powder surfaces are all
Uniformly attachment anticaking agent), obtain secondary mixed potassium carbonate superfine powder；
5), by step 4) the secondary mixed potassium carbonate superfine powder of gained passes through classification, collection cut size≤100 micron
, for potassium carbonate superfine powder of not reuniting.
Remarks illustrate: can be classified using the screen cloth that aperture is 100 microns；Purpose is to remove in transfer or storage process
Make moist the potassium carbonate luming of reuniting.
Improvement as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 5) in, particle diameter ＞
100 microns of potassium carbonate is back to step 2) proceed to pulverize.
Improvement as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 2) in, will pulverize
Potassium carbonate mixtures afterwards pass through classification, and particle diameter≤100 micron are judged to reach Particle size requirements, are up to the carrying out of Particle size requirements
Collect, obtain potassium carbonate superfine powder after pulverizing, not up to the carrying out of Particle size requirements is pulverized again.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 1) in
Liquid anti-caking additive is made up of than the primary octadecylamine acetate for 1:1 and dimethicone weight.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 4) in
Solid anticaking agent is at least one in tricalcium phosphate, Pulvis Talci or white carbon (vapor phase method).Preferably white carbon (vapor phase method).
The effect of this solid anticaking agent is the mobility improving superfine powder potassium carbonate.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 5) middle employing
Aperture is that 100 microns of screen cloth is classified.Remarks illustrate: purpose is to remove the reunion caking that makes moist in transfer or storage process
Potassium carbonate.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 1) be:
Liquid anti-caking additive is first scattered in solvent, is then equably sprayed after firing by aerosol apparatus (high-pressure sprayer)
Band is had a surplus in the potassium carbonate of temperature；
Described liquid anti-caking additive with the mass ratio of solvent is: 1:1.5～2.5 (preferably 1:2), described solvent is
Dehydrated alcohol or absolute methanol.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 2) in,
Pulverize and adopt air-flow vortex pulverizing mill, classification adopts grader, collects and adopts cyclonic separation unit；
Described air-flow vortex pulverizing mill, grader, cyclonic separation unit and bag-type dust collector are arranged in order, described cloth bag
The air outlet of dust arrester is directed at the air inlet of air-flow vortex pulverizing mill, thus realizing that (that is, tail gas removes through cloth bag using circulated air
Realize in Returning flow vortex pulverizing mill after dirt recycling)；
When need supplement fresh air, described fresh air is the clean dry air meeting following condition: relative humidity is less than 30%,
Residua content is less than 0.1ppm, and the accurate filter through 0.45 micron pore size filters.
Remarks illustrate: after above-mentioned technique can ensure that pulverizing, potassium carbonate superfine powder moisture content is not exceeded, and no exogenous impurity.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described cyclonic separation list
Unit is secondary cyclone.Remarks illustrate: so can ensure that qualified material primary recovery big 98%, and reduce entrance cloth bag
Particulate dust in cleaner unit.
Improvement further as the preparation method of the potassium carbonate superfine powder do not reunited of the present invention: described step 4) two
Mixer used by secondary stirring mixing is side's cone or bipyramid, and incorporation time is 0.5～2 hour；So that it is guaranteed that all potassium carbonate
Anticaking agent is all uniformly adhered on superfine powder surface.
The potassium carbonate superfine powder of not reuniting of gained of the present invention, can be used for herbicide dicamba and Quizalotop-ethyl, psychosiss
Medicine Aripiprazole key intermediate 2, the synthesis of 3- dichloro phenmetrazine, but it is also not limited to this.
The potassium carbonate superfine powder do not reunited being prepared using the inventive method, has following physical characteristics: particle diameter≤
100 microns, bulk density be less than 0.55g/ml, loss on drying be less than 0.5%, gained potassium carbonate superfine powder have good fluidity,
The advantages of suspension is excellent slow with sedimentation velocity, and caking of not reuniting can be preserved for a long time.Therefore, can be used as the catalysis of organic synthesiss
Agent, tie up acidity and potassium element supplying agent, catalytic performance can be significantly improved, accelerate reaction rate and improve major product yield.
Brief description
Below in conjunction with the accompanying drawings the specific embodiment of the present invention is described in further detail.
Fig. 1 is the process chart of the preparation method of potassium carbonate superfine powder do not reunited of the present invention；
Fig. 2 is the particle diameter distribution collection of illustrative plates of the potassium carbonate superfine powder of not reuniting of embodiment 1 gained；
The particle diameter distribution collection of illustrative plates of the potassium carbonate superfine powder of Fig. 3 comparative example 6 gained；
The particle diameter distribution collection of illustrative plates of the potassium carbonate superfine powder of Fig. 4 comparative example 7 gained；
The particle diameter distribution collection of illustrative plates of the potassium carbonate superfine powder of Fig. 5 comparative example 8 gained.
Specific embodiment
Embodiment 1, a kind of potassium carbonate superfine preparation method do not reunited, follow the steps below successively:
1), weigh 1 kilogram made by the mixture that primary octadecylamine acetate and dimethicone (weight than for 1:1) form
For liquid anti-caking additive, add 2 kilograms of absolute methanol, be placed in container, heat up heating (about 50-60 DEG C), until
All dissolve, obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8mpa), above-mentioned ready additive methanol solution is equably sprayed
Do not cool down completely after entering firm calcining in 1000 kilograms of potassium carbonate of (that is, with about more than 60-80 DEG C temperature), start blender (bipyramid
Or side bores), mix 30 minutes, so that additive and potassium carbonate mix evenly.
2), step 1) gained potassium carbonate mixtures, pulverized by air-flow vortex pulverizing mill, then entered by grader
Row classification, the potassium carbonate superfine powder reaching Particle size requirements (that is, meeting the condition of particle diameter≤100 micron) enters rotation by grader
Wind separative element (cyclone separator) is collected, obtain 992 kilograms pulverize after potassium carbonate superfine powder, not up to Particle size requirements
Returning flow vortex pulverizing mill is pulverized again, tail gas Returning flow crushing system after bag-type dust.
That is, air-flow vortex pulverizing mill, grader, cyclonic separation unit and bag-type dust collector are arranged in order, bag-type dust
The air outlet of device is directed at the air inlet of air-flow vortex pulverizing mill, thus realizing that (that is, tail gas is after bag-type dust using circulated air
Returning flow vortex pulverizing mill recycles).
Air-flow vortex pulverizing mill for example can be selected for the acm-60 model of Zhejiang Li Pu disintegrating apparatus company limited production, pulverizes
Technological parameter during operation: main frame frequency is 45hz, loading frequency 32.5hz, grade frequency 22.5hz, air inducing unit frequency is
45hz.
All using circulated air, system does not enter fresh air to each unit such as pulverizing, cyclonic separation and bag-type dust substantially, pulverizes
The fresh air that system need to be supplemented is clean dry air, and (that is, relative humidity is less than 30%, and residua content is less than 0.1ppm, and warp
The accurate filter crossing 0.45 micron pore size filters), so that it is guaranteed that potassium carbonate superfine powder moisture content is not exceeded after pulverizing and no outer
Carry out impurity.
3), step 2) gained potassium carbonate superfine powder move into transfer container in, natural cooling, until room temperature, cool time is about
Need 3-5 days, obtain the potassium carbonate superfine powder after cooling；
4) toward step 3) gained cooling after 992 kilograms of potassium carbonate superfine powder in, add 2 kilograms of solid anticaking agents
(fume colloidal silica, hp200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carries out secondary mix and blend, mixer used
For square cone, incorporation time is 2 hours, obtains 994 kilograms of secondary mixed potassium carbonate superfine powder；
5) step 4) gained secondary mixing after potassium carbonate superfine powder, be classified for 100 microns of screen clothes by aperture,
Obtain 990 kilograms of potassium carbonate superfine powder of not reuniting, packaging detection is put in storage.
Gained is not reunited potassium carbonate superfine powder, as requested when detection particle diameter distribution, mobile performance, suspendability and sedimentation
Between.
Particle diameter distribution detection adopts Malvern particle diameter distribution instrument, and with dehydrated alcohol as dispersion solvent during detection, sample does not enter
Row ultrasonic disperse, particle diameter distribution testing result is as described in table 1 and Fig. 2:
Table 1, embodiment 1 gained are not reunited potassium carbonate superfine powder particle diameter distribution
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.Embodiment 1 gained sample do not reunite potassium carbonate superfine powder by the time
For 90 seconds, good fluidity.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate superfine powder can all suspend, if having layering.Embodiment 1 gained sample is not reunited potassium carbonate ultra micro
Can all the suspending of powder, no lamination, graduated cylinder bottom has no the potassium carbonate of caking shape of reuniting.
Sedimentation time: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, uses
The stopwatch meter potassium carbonate sedimentation time, to settle face no longer reduces.Embodiment 1 gained sample is not reunited potassium carbonate superfine powder
Sedimentation time is 413 seconds, and sedimentation velocity is slow.
Embodiment 2, a kind of potassium carbonate superfine preparation method do not reunited, follow the steps below successively:
1), weigh 3 kilograms made by the mixture that primary octadecylamine acetate and dimethicone (weight than for 1:1) form
For liquid anti-caking additive, add 6 kilograms of absolute methanol, be placed in container, heat up heating (about 50-60 DEG C), until
All dissolve；Obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8mpa), above-mentioned ready additive methanol solution is equably sprayed
Do not cool down completely after entering firm calcining in 1000 kilograms of potassium carbonate of (that is, with about more than 60-80 DEG C temperature), start blender (bipyramid
Or side bores), mix 30 minutes, so that additive and potassium carbonate is mixed evenly.
2), step 1) gained potassium carbonate mixtures, pulverized by air-flow vortex pulverizing mill, then pass through grader
Classification, the potassium carbonate micropowder reaching Particle size requirements (that is, meeting the condition of particle diameter≤100 micron) is divided by grader entrance whirlwind
Be collected from device, obtain 996 kilograms pulverize after potassium carbonate superfine powder, not up to Particle size requirements be back to air-flow vortex micropowder
Machine is pulverized again, tail gas Returning flow crushing system after bag-type dust.
Remaining content is equal to embodiment 1.
3), step 2) gained potassium carbonate superfine powder move into transfer container in, natural cooling, until room temperature, cool time is about
Need 3-5 days, obtain the potassium carbonate superfine powder after cooling；
4), toward step 3) gained cooling after 996 kilograms of potassium carbonate superfine powder in, add 10 kilograms of solid anticaking agents
(fume colloidal silica, hp200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carries out secondary mix and blend, mixer used
For square cone, incorporation time is 0.5 hour, obtains 1006 kilograms of secondary mixed potassium carbonate superfine powder；
5), step 4) gained secondary mixing after potassium carbonate superfine powder, be classified for 100 microns of screen clothes by aperture,
Obtain 1004 kilograms of potassium carbonate superfine powder of not reuniting, packaging detection is put in storage.
Gained is not reunited potassium carbonate superfine powder, as requested when detection particle diameter distribution, mobile performance, suspendability and sedimentation
Between.
Table 2, embodiment 2 gained are not reunited potassium carbonate superfine powder particle diameter distribution
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.Embodiment 2 gained sample do not reunite potassium carbonate superfine powder by the time
For 76 seconds, good fluidity.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate micropowder can all suspend, if having layering.Embodiment 2 gained sample is not reunited potassium carbonate superfine powder
Can all suspend, no lamination, graduated cylinder bottom have no reunite caking shape potassium carbonate.
Sedimentation time: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, uses
The stopwatch meter potassium carbonate sedimentation time, to settle face no longer reduces.Embodiment 2 gained sample is not reunited potassium carbonate superfine powder
Sedimentation time is 446 seconds, and sedimentation velocity is slow.
Embodiment 3, a kind of potassium carbonate superfine preparation method do not reunited, comprise the following steps successively:
1), weigh 2 kilograms made by the mixture that primary octadecylamine acetate and dimethicone (weight than for 1:1) form
For liquid anti-caking additive, add 4 kilograms of absolute methanol, be placed in container, heat up heating (about 50-60 DEG C), until
All dissolve, obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8mpa), above-mentioned ready additive methanol solution is equably sprayed
Do not cool down completely after entering firm calcining in 1000 kilograms of potassium carbonate of (that is, with about more than 60-80 DEG C temperature), start blender (bipyramid
Or side bores), mix 30 minutes, so that additive and potassium carbonate is mixed evenly.
2), step 1) gained potassium carbonate mixtures, pulverized by air-flow vortex pulverizing mill, then divided by grader
Level, the potassium carbonate micropowder reaching Particle size requirements (that is, meeting the condition of particle diameter≤100 micron) enters cyclonic separation by grader
Device is collected, and obtains potassium carbonate superfine powder after 995 kilograms of pulverizing, and the Returning flow vortex pulverizing mill of not up to Particle size requirements enters
Row is pulverized again, tail gas Returning flow crushing system after bag-type dust.
Remaining content is with embodiment 1.
3), step 2) gained potassium carbonate superfine powder move into transfer container in, natural cooling, until room temperature, cool time is about
Need 3-5 days, obtain the potassium carbonate superfine powder after cooling；
4), toward step 3) gained cooling after 995 kilograms of potassium carbonate superfine powder in, add 6 kilograms of solid anticaking agents
(fume colloidal silica, hp200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carries out secondary mix and blend, mixer used
For square cone, incorporation time is 1 hour, obtains 1001 kilograms of secondary mixed potassium carbonate superfine powder；
5) step 4) gained secondary mixing after potassium carbonate superfine powder, be classified for 100 microns of screen clothes by aperture, obtained
998 kilograms of potassium carbonate superfine powder of not reuniting, packaging detection is put in storage.
The potassium carbonate superfine powder of not reuniting of gained, detection particle diameter distribution, mobile performance, suspendability and sedimentation as requested
Time.
Table 3, embodiment 3 gained are not reunited potassium carbonate superfine powder particle diameter distribution
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.Embodiment 3 gained sample do not reunite potassium carbonate superfine powder by the time
For 84 seconds, good fluidity.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate micropowder can all suspend, if having layering.Embodiment 3 gained sample is not reunited potassium carbonate superfine powder
Can all suspend, no lamination, graduated cylinder bottom have no reunite caking shape potassium carbonate.
Sedimentation time: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, uses
The stopwatch meter potassium carbonate sedimentation time, to settle face no longer reduces.Embodiment 3 gained sample is not reunited potassium carbonate superfine powder
Sedimentation time is 427 seconds, and sedimentation velocity is slow.
Contrast experiment 1:
A kind of herbicide according to offers such as Yangnong Chemical Co., Ltd., Jiangsu's relative jewel (201210486647.0)
The method of the embodiment 6 in the synthesis technique of Mediben:
1), add 2, the 5- chlorophenesic acid of 300g dry toluene and 65g in 500ml reaction bulb, under the conditions of being stirred at room temperature
Add potassium hydroxide 21.2g, then continue the reaction 2 hours that continues.After reaction terminates, vacuum distillation, with toluene band water, by reaction system
In water remove.After water has removed, cooling, almost quantitative obtain 2,5- chlorophenesic acid potassium.
2), in 500ml high-pressure reactor, add 379g step 1) gained 2,5- chlorophenesic acid potassium toluene solution, add
96g ordinary powder shape Anhydrous potassium carbonate, 6g butanol and 3g triethylamine.After being passed through appropriate co2, begin to warm up stirring, control reaction
Temperature is 145 DEG C, is more slowly passed through co2 to pressure 6.0mpa.With the carrying out in response time, slowly supplement co2 anti-to guarantee
Temperature in device, pressure is answered to maintain 145 DEG C and 6.0mpa.And maintain 10 hours in this case.After reaction terminates, close
Co2 air supply system, temperature of reactor begins to decline less than 70 DEG C.After gas drains in high-pressure reactor, add system
Water stirs and all dissolves to reactant.Saponification through layering, acid adjustment, dehydration, filter pressing and liquid feeding, obtain 15% 3,6- dichloro
Sodium salicylate solution 528g, yield 86.7%.
Contrast experiment 2:
Ordinary powder shape Anhydrous potassium carbonate is changed to potassium carbonate superfine powder of not reuniting of the present invention, and, by step 2)
" maintaining 10 hours " makes " maintaining 5 hours " into, and remaining is equal to above-mentioned contrast experiment 1.
Finally give 15% 3,6- dichlorosalicylic acid sodium solution 554g, yield 91.0%.
Compare with contrast experiment 1, using the potassium carbonate superfine powder do not reunited of the present invention, the response time can shorten 5
Individual hour, and product yield can improve 5% about.
Comparative example 1, for embodiment 1, make following change: by step 2) described in tail gas straight after bag-type dust
Meet outer row, airflow comminution system is evacuated by air-introduced machine, fresh air enters system from charging aperture, and remaining is equal to embodiment 1.
Comparative example 1 (without circulated air), the average moisture content of gained potassium carbonate superfine powder is 2.62%, considerably beyond potassium carbonate state
Family's standard.
And, embodiment 1 (using circulated air), the average moisture content of gained potassium carbonate superfine powder is 0.23%.
That is, the defect of above-mentioned comparative example 1 be can lead to pulverize after potassium carbonate superfine powder moisture content exceeded.
Comparative example 2, the solid anticaking agent in embodiment 1 is made into as described in Table 4 by fume colloidal silica respectively, consumption
Constant (or, cancel the use of solid anticaking agent), remaining is equal to embodiment 1.
The concrete correction data of the clarity of the mobility of potassium carbonate superfine powder, dissolubility and solution is as described in Table 4:
Table 4, the mobility adding different solid anticaking agents, dissolubility and clarity contrast
(present invention) institute when above-mentioned correction data can be seen that using fumed silica as solid anticaking agent
The best performance of the potassium carbonate obtaining.
Comparative example 3:
Cancel step 1 in embodiment 1) liquid anti-caking additive use, i.e. without primary octadecylamine acetate and
Dimethicone；Remaining is equal to embodiment 1.
The suspendability of products therefrom and the present invention, dispersive property and hygroscopic contrast are described in table 5 below.
Table 5, the suspension of potassium carbonate micropowder, dispersibility and hygroscopic contrast
Comparative example 4:
Cancel embodiment 1 step 3), i.e. by step 2) 992 kilograms of potassium carbonate superfine powder of gained directly carry out step
4), remaining is equal to embodiment 1.
Final 967 kilograms of potassium carbonate superfine powder of not reuniting, its particle diameter distribution is as described in Fig. 3 and Biao 6.
Table 6, comparative example 4 gained potassium carbonate superfine powder particle diameter distribution
Can be seen that because after pulverizing, potassium carbonate does not carry out cooling treatment from table 6 and Fig. 3, temperature of charge is too high, even if
Directly pass through secondary mix and blend, also cannot avoid the problem of potassium carbonate superfine powder reunion caking, false caking is serious.Therefore,
Potassium carbonate after pulverizing needs to be cooled down, and then passes through secondary mix and blend again, just can produce the carbonic acid of caking of not reuniting
Potassium superfine powder.
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.The mobility of comparative example 4 gained sample potassium carbonate superfine powder is 129 seconds.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate micropowder can all suspend, if having layering.Can having suspended of gained sample potassium carbonate superfine powder
Come, but have obvious lamination, the potassium carbonate of the visible a small amount of caking shape of reuniting in graduated cylinder bottom.
Comparative example 5: cancellation step 4) the middle use cancelling 2 kilograms of solid anticaking agents；And, above-mentioned 2 kilograms of solids are prevented
Agglomeration agent changes into step 2) in use, i.e. in step 1) gained potassium carbonate mixtures add 2 kilograms of solid anticaking agents after, lead to
Cross air-flow vortex pulverizing mill to be pulverized；Remaining content is equal to embodiment 1.
Final 920 kilograms of potassium carbonate superfine powder of not reuniting.
Its particle diameter distribution is as described in table 7 and Fig. 4.
Table 7, comparative example 5 gained potassium carbonate superfine powder particle diameter distribution
Can be seen that from table 7 and Fig. 4 and be initially charged granule when octadecylamine acetate salt, dimethicone and solid anticaking agent
Pulverize again after potassium carbonate, small part potassium carbonate micropowder can produce false caking, affect preventing blocking effect, liquid anti-agglomeration agent is described
Should be added separately with solid anticaking agent.Due to fumed silica particle diameter little it may be possible to crushing process is pulled away by wind, reduce
Actual consumption.
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.The mobility of comparative example 6 gained sample potassium carbonate superfine powder is 104 seconds.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate micropowder can all suspend, if having layering.Can having suspended of gained sample potassium carbonate superfine powder
Come, but have obvious lamination, the potassium carbonate of the visible a small amount of caking shape of reuniting in graduated cylinder bottom.
Comparative example 6, the whole step 1 of cancellation), i.e. granule potassium carbonate is directly carried out step 2)；And cancellation step 4) in
The use of 2 kilograms of solid anticaking agents；Remaining is equal to embodiment 1.
When the potassium carbonate superfine powder of final gained detects particle diameter distribution, mobile performance, suspendability and sedimentation as requested
Between.
Table 8, comparative example 6 gained potassium carbonate superfine powder particle diameter distribution
Can be seen that from table 8 and Fig. 5 and be not added with octadecylamine acetate salt, dimethicone and solid anticaking agent vapor phase method two
Silicon oxide, pulverizes gained potassium carbonate ultra micro powder ball and takes caking serious, particle diameter does not substantially reach requirement.
The detection of mobility: weigh 100 grams of test samples, come with the funnel required time as 12mm full by nozzle diameter
Evaluate mobility, the time is longer, and to represent mobility poorer.The mobility of comparative example 8 gained sample potassium carbonate superfine powder is 187 seconds.
Suspendability: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, sees
Examine whether potassium carbonate micropowder can all suspend, if having layering.Comparative example 8 gained potassium carbonate superfine powder suspendability is very
Hence it is evident that layering, the potassium carbonate of many caking shapes of reuniting is arranged difference at graduated cylinder bottom.
Sedimentation time: 150 milliliters of tool plug glass cylinders, pour 100 milliliters of dehydrated alcohol into, be subsequently adding 10 grams of superfine powder
Potassium carbonate sample, fluctuates after jumping a queue, and until superfine powder potassium carbonate is not deposited in graduated cylinder bottom, is positioned under horizontal stand, uses
The stopwatch meter potassium carbonate sedimentation time, to settle face no longer reduces.The sedimentation time of comparative example 8 gained potassium carbonate superfine powder is
247 seconds, sedimentation velocity was quickly.
Last in addition it is also necessary to it is noted that listed above be only the present invention several specific embodiments.Obviously, this
Bright be not limited to above example, can also have many deformation.Those of ordinary skill in the art can be from present disclosure
The all deformation directly derived or associate, are all considered as protection scope of the present invention.
Claims (9)
1. the preparation method of the potassium carbonate superfine powder do not reunited, is characterized in that comprising the following steps:
1), toward after calcining, band is had a surplus in the potassium carbonate of temperature and is added liquid anti-caking additive, uniformly mixes, described liquid anti-caking
The weight of additive and potassium carbonate is than for 0.1～0.3%；
2), by step 1) potassium carbonate mixtures of gained are pulverized, and collection cut size≤100 micron, as carbonic acid after pulverizing
Potassium superfine powder；
3), by step 2) the potassium carbonate superfine powder of gained moves in transfer container, naturally cools to room temperature, obtain the carbon after cooling
Sour potassium superfine powder；
4), to step 3) add the potassium carbonate superfine powder weight after accounting for cooling in potassium carbonate superfine powder after the cooling of gained
0.2～1% solid anticaking agent, and carry out secondary stirring mixing, obtain secondary mixed potassium carbonate superfine powder；
5), by step 4) the secondary mixed potassium carbonate superfine powder of gained passes through classification, collection cut size≤100 micron,
For potassium carbonate superfine powder of not reuniting.
2. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 1, is characterized in that: described step 5)
In, the potassium carbonate that 100 microns of particle diameter ＞ is back to step 2) proceed to pulverize.
3. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 1 and 2, is characterized in that: described step
2), in, the potassium carbonate mixtures after pulverizing are passed through classification, particle diameter≤100 micron are judged to reach Particle size requirements, are up to grain
What footpath required is collected, and obtains potassium carbonate superfine powder after pulverizing, not up to the carrying out of Particle size requirements is pulverized again.
4. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 3, is characterized in that: described step 1) in
Liquid anti-caking additive be made up of than the primary octadecylamine acetate for 1:1 and dimethicone weight.
5. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 4, is characterized in that: described step 4) in
Solid anticaking agent be tricalcium phosphate, at least one in Pulvis Talci or white carbon.
6. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 5, is characterized in that: described step 1)
For: liquid anti-caking additive is first scattered in solvent, then equably sprays band after firing by aerosol apparatus and have a surplus temperature
Potassium carbonate in；
The mass ratio of described liquid anti-caking additive and solvent is 1:1.5～2.5, and described solvent is dehydrated alcohol or no water beetle
Alcohol.
7. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 6, is characterized in that: described step 2)
In, pulverize and adopt air-flow vortex pulverizing mill, classification adopts grader, collects and adopts cyclonic separation unit；
Described air-flow vortex pulverizing mill, grader, cyclonic separation unit and bag-type dust collector are arranged in order, described bag-type dust
The air outlet of device is directed at the air inlet of air-flow vortex pulverizing mill, thus realizing using circulated air；
When need supplement fresh air, described fresh air is the clean dry air meeting following condition: relative humidity is less than 30%, Residual oil
Content is less than 0.1ppm, and the accurate filter through 0.45 micron pore size filters.
8. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 7, is characterized in that: described cyclonic separation
Unit is secondary cyclone.
9. the preparation method of the potassium carbonate superfine powder do not reunited according to claim 4, is characterized in that: described step 4)
Mixer used by secondary stirring mixing is side's cone or bipyramid, and incorporation time is 0.5～2 hour.
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| CN101659421A (en) * | 2009-09-09 | 2010-03-03 | 张家港市华昌药业有限公司 | Method for preventing ammonium chloride from caking |
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