CN105399114A - 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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- 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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- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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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, relate to inorganic chemical industry and organic chemical industry's technology, particularly relate to a kind of preparation method of salt of wormwood super-fine powder of not reuniting.
Background technology
Salt of wormwood is structure very clearly simple compound, is a kind of ancient and traditional chemical composition, is also a kind of along with entering a kind of product innovation constantly giving its New function, new feature and novelty teabag for the progress of science and technology.Salt of wormwood is as a kind of inorganic salt basic chemical industry raw material, and be the raw material producing Potassium ethanoate, Potassium monofluoride, potassium arsenite and potassium sorbate, be also usually used in glass, chemical industry, medicine, agricultural chemicals and chemical fertilizer, along with the development of science and technology, the purposes of salt of wormwood is more and more wider.
Along with the raising of living standards of the people, more and more pay attention to health, the consciousness of environment protection is also more and more stronger, therefore also proposes new requirement to agricultural chemicals; Not only require effective, also require low residue, hypotoxicity and low cost, many organophosphoruss and organosulfur class agricultural chemicals are eliminated gradually, many novel agrochemicals, owing to having the advantages such as hypotoxicity, low residue and efficient specificity, are therefore paid attention to, develop also rapid.
Wherein dicamba 98 is exactly a good example.As the new herbicides that the sixties in last century is developed by Novartis, the features such as it has stronger selectivity, consumption lacks, annual or perennial broadleaf weeds is prevented and kill off in the field being mainly used in the effect of wheat Deng He benzene section.For a long time, because dicamba 98 price is high, use cost is high, therefore its market focuses mostly in European and American developed countries.Although demand is stablized, development is always relatively slower, but from 2009, dicamba 98 demand increased fast, and mainly have benefited from novel process and reduce production cost, add that glyphosate is drug-fast and strengthen year by year, dicamba 98 is brought to the teeth of the storm again.
In process of production, salt of wormwood is its main raw material(s) to dicamba 98, often produces 1 ton of dicamba 98, about needs the salt of wormwood that consumption about 1 ton is measured.In reaction process, salt of wormwood is not homogeneous reaction (solid-liquid) with its material, the particle of conventional salt of wormwood is large, good fluidity, but can not suspend, settling velocity is fast, be unfavorable for the reaction between solid-liquid, catalytic performance is low, long reaction time, side reaction is many, causes the problem that major product yield is low, impurity is many.Dicamba 98 novel process and automatic production, require that salt of wormwood particle diameter needs to control below 100 microns, and do not allow caking of reuniting.
Due to reasons such as thermodynamics, electrostatic and liquid bridges, salt of wormwood super-fine powder self is always reunited together, adds that salt of wormwood itself very easily absorbs water to make moist, and conventional production process cannot accomplish its caking of not reuniting at all.Due to above-mentioned salt of wormwood nature, super-fine powder cannot be produced by synthesis technique, at present can only by pulverizing this approach.Salt of wormwood is water-soluble inorganic salt, cannot pass through wet pulverization, but in dry ground process, heating is serious, salt of wormwood micro mist temperatures as high 70-80 DEG C after pulverizing, will to reunite after pulverizing caking at once, mobility and suspension property poor, be not suitable for the production requirement of the organic syntheses such as dicamba 98.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of salt of wormwood super-fine powder (particle diameter≤100 micron) of not reuniting.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of salt of wormwood super-fine powder of not reuniting, comprising the following steps:
1), toward rear being with in the salt of wormwood of temperature (temperature is about 60-80 DEG C) of having a surplus of calcining add liquid anti-caking additive, Homogeneous phase mixing, the weight ratio of liquid anti-caking additive and salt of wormwood is 0.1 ~ 0.3%;
2), by step 1) potassium carbonate mixtures of gained pulverizes, and collection cut size≤100 micron, as salt of wormwood super-fine powder I after pulverizing;
3), by step 2) the salt of wormwood super-fine powder I of gained moves in transfer container, naturally cools to room temperature, obtain cooled salt of wormwood super-fine powder II;
4), to step 3) add the solid anti-hard caking agent accounting for cooled salt of wormwood super-fine powder II weight 0.2 ~ 1% in the cooled salt of wormwood super-fine powder II of gained, and carry out secondary stirring mixing (thus guaranteeing that anti-hard caking agent is all evenly adhered in all salt of wormwood super-fine powder surfaces), obtain the mixed salt of wormwood super-fine powder III of secondary;
5), by step 4) the mixed salt of wormwood super-fine powder III of the secondary of gained is by classification, and collection cut size≤100 micron is salt of wormwood super-fine powder of not reuniting.
Remarks illustrate: aperture can be adopted to be that the screen cloth of 100 microns carries out classification; Object removes in transfer or storage process the salt of wormwood of reuniting and luming that makes moist.
Improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 5) in, the salt of wormwood that particle diameter > is 100 microns is back to step 2) proceed to pulverize.
Improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 2) in, potassium carbonate mixtures after pulverizing is passed through classification, particle diameter≤100 micron are judged to reach Particle size requirements, the carrying out reaching Particle size requirements is collected, must pulverize rear salt of wormwood super-fine powder I, the carrying out not reaching Particle size requirements is pulverized again.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 1) in liquid anti-caking additive be that the primary octadecylamine acetate of 1:1 and dimethyl silicone oil form by weight ratio.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 4) in solid anti-hard caking agent be at least one in tricalcium phosphate, talcum powder or white carbon black (vapor phase process).Preferred white carbon black (vapor phase process).The effect of this solid anti-hard caking agent is the mobility improving super-fine powder salt of wormwood.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 5) in adopt aperture to be that the screen cloth of 100 microns carries out classification.Remarks illustrate: object removes in transfer or storage process the salt of wormwood of reuniting and luming that makes moist.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 1) be: liquid anti-caking additive is first scattered in solvent, then sprays band after firing equably by atomizer (high-pressure sprayer) and have a surplus in the salt of wormwood of temperature;
The mass ratio of described liquid anti-caking additive and solvent is: 1:1.5 ~ 2.5 (being preferably 1:2), and described solvent is dehydrated alcohol or anhydrous methanol.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 2) in, pulverize and adopt air-flow vortex pulverizing mill, classification adopts grading machine, collects and adopts cyclonic separation unit;
Described air-flow vortex pulverizing mill, grading machine, cyclonic separation unit and bag-type dust collector are arranged in order, the air outlet of described bag-type dust collector aims at the blast inlet of air-flow vortex pulverizing mill, thus realize using recirculating air (that is, tail gas realizes in Returning flow vortex pulverizing mill recycling after bag-type dust);
When supplementing new wind, described new wind is the clean dry air met the following conditions: relative humidity is less than 30%, and residua content is less than 0.1ppm, and filters through the accurate filter of 0.45 micron pore size.
Remarks illustrate: above-mentioned technique can guarantee that pulverizing rear salt of wormwood super-fine powder moisture content does not exceed standard, and without tramp material.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described cyclonic separation unit is secondary cyclone.Remarks illustrate: can guarantee qualified material primary recovery large 98% like this, and reduce the particulate dust entered in sack cleaner.
Further improvement as the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention: described step 4) secondary stirring mix stirring mixer used for side cone or bipyramid, mixing time is 0.5 ~ 2 hour; Thus guarantee that anti-hard caking agent is all evenly adhered in all salt of wormwood super-fine powder surfaces.
The salt of wormwood super-fine powder of not reuniting of gained of the present invention, can be used for the synthesis of herbicide dicamba and quizalofopPethyl, antipsychotic drug Aripiprazole key intermediate 2,3-dichloro phenmetrazine, but is also not limited only to this.
The salt of wormwood super-fine powder of not reuniting that employing the inventive method is prepared and obtained, there is following physical property: particle diameter≤100 micron, tap density is less than 0.55g/ml, weight loss on drying is less than 0.5%, gained salt of wormwood super-fine powder has the advantages such as the excellent and settling velocity of good fluidity, suspension is slow, and can preserve caking of not reuniting for a long time.Therefore, can be used as the catalyzer of organic synthesis, tie up acidity and potassium element supplying agent, catalytic performance can be significantly improved, accelerate speed of reaction and improve major product yield.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the process flow sheet of the preparation method of salt of wormwood super-fine powder of not reuniting of the present invention;
Fig. 2 is the size distribution collection of illustrative plates of the salt of wormwood super-fine powder of not reuniting of embodiment 1 gained;
The size distribution collection of illustrative plates of the salt of wormwood super-fine powder of Fig. 3 comparative example 6 gained;
The size distribution collection of illustrative plates of the salt of wormwood super-fine powder of Fig. 4 comparative example 7 gained;
The size distribution collection of illustrative plates of the salt of wormwood super-fine powder of Fig. 5 comparative example 8 gained.
Embodiment
Embodiment 1, a kind of salt of wormwood superfine preparation method of not reuniting, carry out following steps successively:
1) mixture be made up of primary octadecylamine acetate and dimethyl silicone oil (weight ratio is 1:1) of 1 kilogram, is taken as liquid anti-caking additive, add the anhydrous methanol of 2 kilograms, be placed in container, heat up heating (being about 50-60 DEG C), until all dissolve, obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8MPa), do not cool (namely completely after above-mentioned ready additive methanol solution being sprayed into equably just calcining, band have an appointment more than 60-80 DEG C temperature) 1000 kilograms of salt of wormwood in, start mixing tank (bipyramid or side's cone), mix 30 minutes, thus make additive and salt of wormwood mixing evenly.
2), step 1) gained potassium carbonate mixtures, pulverized by air-flow vortex pulverizing mill, then classification is carried out by grading machine, reach Particle size requirements (namely, meet the condition of particle diameter≤100 micron) salt of wormwood super-fine powder enter cyclonic separation unit (cyclonic separator) by grading machine and collect, obtain 992 kilograms and pulverize rear salt of wormwood super-fine powder I, the Returning flow vortex pulverizing mill not reaching Particle size requirements is pulverized again, and tail gas is Returning flow crushing system after bag-type dust.
Namely, air-flow vortex pulverizing mill, grading machine, cyclonic separation unit and bag-type dust collector are arranged in order, the air outlet of bag-type dust collector aims at the blast inlet of air-flow vortex pulverizing mill, thus realize using recirculating air (that is, tail gas Returning flow vortex pulverizing mill after bag-type dust recycles).
The ACM-60 model that air-flow vortex pulverizing mill such as can select Zhejiang Li Pu disintegrating apparatus company limited to produce, processing parameter during crushing operation: main frame frequency is 45Hz, loading frequency 32.5Hz, grade frequency 22.5Hz, induced draft fan frequency is 45Hz.
Each unit such as pulverizing, cyclonic separation and bag-type dust all use recirculating air, system does not enter fresh air substantially, (namely the new wind that crushing system need supplement be clean dry air, relative humidity is less than 30%, residua content is less than 0.1ppm, and filter through the accurate filter of 0.45 micron pore size), thus guarantee that pulverizing rear salt of wormwood super-fine powder moisture content does not exceed standard, and without tramp material.
3), step 2) gained salt of wormwood super-fine powder I moves in transfer container, naturally cooling, until room temperature, cooling time about needs 3-5 days, obtains cooled salt of wormwood super-fine powder II;
4) toward step 3) in the cooled 992 kilograms of salt of wormwood super-fine powder II of gained, add 2 kilograms of solid anti-hard caking agent (thermal silicas, HP200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carry out secondary mix and blend, the stirring mixer side of being used cone, mixing time is 2 hours, obtains 994 kilograms of mixed salt of wormwood super-fine powder III of secondary;
5) step 4) gained secondary mixing after salt of wormwood super-fine powder III, be that 100 microns of screen clothes carry out classification by aperture, obtain 990 kilograms of salt of wormwood super-fine powder of not reuniting, packaging detection put in storage.
Gained is not reunited salt of wormwood super-fine powder, detects size distribution, flowing property, suspension property and settling time as requested.
Size distribution detects and adopts Malvern size distribution instrument, and be dispersion solvent with dehydrated alcohol during detection, sample does not carry out ultrasonic disperse, and size distribution detected result is as described in table 1 and Fig. 2:
Table 1, embodiment 1 gained are not reunited salt of wormwood super-fine powder size distribution
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.What salt of wormwood super-fine powder do not reunited by embodiment 1 gained sample is 90 seconds by the time, good fluidity.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood super-fine powder and whether can all suspend, whether have layering.Embodiment 1 gained sample is not reunited can all suspending of salt of wormwood super-fine powder, without demixing phenomenon, having no the salt of wormwood of caking shape of reuniting bottom graduated cylinder.
Settling time: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, with the stopwatch meter salt of wormwood settling time, till no longer reducing with sedimentation face.Do not reunite settling time of salt of wormwood super-fine powder of embodiment 1 gained sample is 413 seconds, and settling velocity is slow.
Embodiment 2, a kind of salt of wormwood superfine preparation method of not reuniting, carry out following steps successively:
1) mixture be made up of primary octadecylamine acetate and dimethyl silicone oil (weight ratio is 1:1) of 3 kilograms, is weighed as liquid anti-caking additive, add the anhydrous methanol of 6 kilograms, be placed in container, heat up heating (being about 50-60 DEG C), until all dissolve; Obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8MPa), do not cool (namely completely after above-mentioned ready additive methanol solution being sprayed into equably just calcining, band have an appointment more than 60-80 DEG C temperature) 1000 kilograms of salt of wormwood in, start mixing tank (bipyramid or side's cone), mix 30 minutes, make additive and salt of wormwood mixing evenly.
2), step 1) potassium carbonate mixtures of gained, pulverized by air-flow vortex pulverizing mill, then by grading machine classification, reach Particle size requirements (namely, meet the condition of particle diameter≤100 micron) salt of wormwood micro mist enter cyclonic separator by grading machine and collect, obtain 996 kilograms and pulverize rear salt of wormwood super-fine powder I, the air-flow vortex pulverizing mill that is back to not reaching Particle size requirements is pulverized again, and tail gas is Returning flow crushing system after bag-type dust.
All the other contents are equal to embodiment 1.
3), step 2) gained salt of wormwood super-fine powder I moves in transfer container, naturally cooling, until room temperature, cooling time about needs 3-5 days, obtains cooled salt of wormwood super-fine powder II;
4), toward step 3) in the cooled 996 kilograms of salt of wormwood super-fine powder II of gained, add 10 kilograms of solid anti-hard caking agent (thermal silicas, HP200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carry out secondary mix and blend, the stirring mixer side of being used cone, mixing time is 0.5 hour, obtains 1006 kilograms of mixed salt of wormwood super-fine powder III of secondary;
5), step 4) gained secondary mixing after salt of wormwood super-fine powder III, be that 100 microns of screen clothes carry out classification by aperture, obtain 1004 kilograms of salt of wormwood super-fine powder of not reuniting, packaging detection put in storage.
Gained is not reunited salt of wormwood super-fine powder, detects size distribution, flowing property, suspension property and settling time as requested.
Table 2, embodiment 2 gained are not reunited salt of wormwood super-fine powder size distribution
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.What salt of wormwood super-fine powder do not reunited by embodiment 2 gained sample is 76 seconds by the time, good fluidity.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood micro mist and whether can all suspend, whether have layering.Embodiment 2 gained sample is not reunited can all suspending of salt of wormwood super-fine powder, without demixing phenomenon, having no the salt of wormwood of caking shape of reuniting bottom graduated cylinder.
Settling time: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, with the stopwatch meter salt of wormwood settling time, till no longer reducing with sedimentation face.Do not reunite settling time of salt of wormwood super-fine powder of embodiment 2 gained sample is 446 seconds, and settling velocity is slow.
Embodiment 3, a kind of salt of wormwood superfine preparation method of not reuniting, comprise the following steps successively:
1) mixture be made up of primary octadecylamine acetate and dimethyl silicone oil (weight ratio is 1:1) of 2 kilograms, is weighed as liquid anti-caking additive, add the anhydrous methanol of 4 kilograms, be placed in container, heat up heating (being about 50-60 DEG C), until all dissolve, obtain additive methanol solution.
With high-pressure sprayer (pressure is about 0.5-0.8MPa), do not cool (namely completely after above-mentioned ready additive methanol solution being sprayed into equably just calcining, band have an appointment more than 60-80 DEG C temperature) 1000 kilograms of salt of wormwood in, start mixing tank (bipyramid or side's cone), mix 30 minutes, make additive and salt of wormwood mixing evenly.
2), step 1) gained potassium carbonate mixtures, pulverized by air-flow vortex pulverizing mill, then by grading machine classification, reach Particle size requirements (namely, meet the condition of particle diameter≤100 micron) salt of wormwood micro mist enter cyclonic separator by grading machine and collect, obtain 995 kilograms and pulverize rear salt of wormwood super-fine powder I, the Returning flow vortex pulverizing mill not reaching Particle size requirements is pulverized again, and tail gas is Returning flow crushing system after bag-type dust.
All the other contents are with embodiment 1.
3), step 2) gained salt of wormwood super-fine powder I moves in transfer container, naturally cooling, until room temperature, cooling time about needs 3-5 days, obtains cooled salt of wormwood super-fine powder II;
4), toward step 3) in the cooled 995 kilograms of salt of wormwood super-fine powder II of gained, add 6 kilograms of solid anti-hard caking agent (thermal silicas, HP200, Jiangxi Bai Hong chemistry Science and Technology Ltd.), carry out secondary mix and blend, the stirring mixer side of being used cone, mixing time is 1 hour, obtains 1001 kilograms of mixed salt of wormwood super-fine powder III of secondary;
5) step 4) the rear salt of wormwood super-fine powder III of gained secondary mixing, be that 100 microns of screen clothes carry out classification by aperture, obtain 998 kilograms of salt of wormwood super-fine powder of not reuniting, packaging detection is put in storage.
The salt of wormwood super-fine powder of not reuniting of gained, detects size distribution, flowing property, suspension property and settling time as requested.
Table 3, embodiment 3 gained are not reunited salt of wormwood super-fine powder size distribution
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.What salt of wormwood super-fine powder do not reunited by embodiment 3 gained sample is 84 seconds by the time, good fluidity.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood micro mist and whether can all suspend, whether have layering.Embodiment 3 gained sample is not reunited can all suspending of salt of wormwood super-fine powder, without demixing phenomenon, having no the salt of wormwood of caking shape of reuniting bottom graduated cylinder.
Settling time: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, with the stopwatch meter salt of wormwood settling time, till no longer reducing with sedimentation face.Do not reunite settling time of salt of wormwood super-fine powder of embodiment 3 gained sample is 427 seconds, and settling velocity is slow.
Contrast experiment 1:
The method of the embodiment 6 in the synthesis technique of a kind of herbicide dicamba provided according to Yangnong Chemical Co., Ltd., Jiangsu's relative jewel (201210486647.0) etc.:
1), add 2, the 5-chlorophenesic acid of 300g dry toluene and 65g in 500ml reaction flask, under stirring at room temperature condition, add potassium hydroxide 21.2g, then the continuous reaction 2 hours that continues.After reaction terminates, underpressure distillation, with toluene band water, by the water removing in reaction system.After water has been removed, cooling, has almost quantitatively obtained 2,5-chlorophenesic acid potassium.
2), in 500ml high-pressure reactor, 379g step 1 is added) gained 2,5-chlorophenesic acid potassium toluene solution, add 96g common flour powder Anhydrous potassium carbonate, 6g butanols and 3g triethylamine.After passing into the addition of C O2, start heated and stirred, controlling temperature of reaction is 145 DEG C, more slowly passes into CO2 to pressure 6.0MPa.Along with the carrying out in reaction times, slowly supplement CO2 to guarantee reactor temperature, pressure maintains 145 DEG C and 6.0MPa.And maintain 10 hours in this case.After reaction terminates, close CO2 airing system, temperature of reactor starts to drop to less than 70 DEG C.After treating that in high-pressure reactor, gas drains, add system water and be stirred to reactant and all dissolve.Saponification through layering, acid adjustment, dehydration, press filtration and liquid feeding, obtain 3, the 6-dichlorosalicylic acid sodium solution 528g of 15%, yield 86.7%.
Contrast experiment 2:
Change common flour powder Anhydrous potassium carbonate into salt of wormwood super-fine powder of not reuniting of the present invention, and, by step 2) " maintaining 10 hours " make into " maintaining 5 hours ", and all the other are equal to above-mentioned contrast experiment 1.
Finally obtain 3, the 6-dichlorosalicylic acid sodium solution 554g of 15%, yield 91.0%.
Compare with contrast experiment 1, adopt salt of wormwood super-fine powder of not reuniting of the present invention, the reaction times can shorten 5 hours, and product yield can improve about 5%.
Comparative example 1, for embodiment 1, do to change as follows: by step 2) described in tail gas direct outer row after bag-type dust, airflow comminution system is bled by induced draft fan, and fresh air enters system from opening for feed, and all the other are equal to embodiment 1.
Comparative example 1 (without recirculating air), the average moisture content of gained salt of wormwood super-fine powder is 2.62%, considerably beyond salt of wormwood national standard.
And embodiment 1 (use recirculating air), the average moisture content of gained salt of wormwood super-fine powder is 0.23%.
That is, the defect of above-mentioned comparative example 1 to cause the salt of wormwood super-fine powder moisture content after pulverizing to exceed standard.
Comparative example 2, make into as described in Table 4 by the solid anti-hard caking agent in embodiment 1 respectively by thermal silica, consumption constant (or, cancel the use of solid anti-hard caking agent), all the other are equal to embodiment 1.
The concrete correlation data of the clarity of the mobility of salt of wormwood super-fine powder, solvability and solution is as described in Table 4:
Table 4, the mobility of adding different solid anti-hard caking agent, solvability and clarity contrast
As can be seen from above-mentioned correlation data, adopt fumed silica as the best performance of the salt of wormwood of (the present invention) gained during solid anti-hard caking agent.
Comparative example 3:
Cancel step 1 in embodiment 1) the use of liquid anti-caking additive, that is, do not add primary octadecylamine acetate and dimethyl silicone oil; All the other are equal to embodiment 1.
Products therefrom and suspension property of the present invention, dispersing property and hygroscopic contrast are described in table 5 below.
The suspension of table 5, salt of wormwood micro mist, dispersiveness and hygroscopic contrast
Comparative example 4:
Cancel embodiment 1 step 3), that is, by step 2) 992 kilograms of salt of wormwood super-fine powder I of gained directly carry out steps 4), all the other are equal to embodiment 1.
Final 967 kilograms of salt of wormwood super-fine powder of not reuniting, its size distribution is as described in Fig. 3 and table 6.
Table 6, comparative example 4 gained salt of wormwood super-fine powder size distribution
As can be seen from table 6 and Fig. 3, do not carry out cooling process owing to pulverizing rear salt of wormwood, temperature of charge is too high, even if directly by secondary mix and blend, also cannot avoid the problem of salt of wormwood super-fine powder reunion caking, false caking is serious.Therefore, the salt of wormwood after pulverizing needs to cool, and then by secondary mix and blend, just can produce the salt of wormwood super-fine powder of caking of not reuniting.
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.The mobility of comparative example 4 gained sample salt of wormwood super-fine powder is 129 seconds.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood micro mist and whether can all suspend, whether have layering.Can suspending of gained sample salt of wormwood super-fine powder, but there is obvious demixing phenomenon, the salt of wormwood of visible a small amount of caking shape of reuniting bottom graduated cylinder.
Comparative example 5: cancellation step 4) the middle use cancelling 2 kilograms of solid anti-hard caking agents; And, above-mentioned 2 kilograms of solid anti-hard caking agents are changed into step 2) in use, that is, in step 1) after gained potassium carbonate mixtures adds 2 kilograms of solid anti-hard caking agents, pulverized by air-flow vortex pulverizing mill; All the other contents are equal to embodiment 1.
Final 920 kilograms of salt of wormwood super-fine powder of not reuniting.
Its size distribution is as described in table 7 and Fig. 4.
Table 7, comparative example 5 gained salt of wormwood super-fine powder size distribution
As can be seen from table 7 and Fig. 4, pulverize again after octadecylamine acetate salt, dimethyl silicone oil and solid anti-hard caking agent first add particle salt of wormwood, small part salt of wormwood micro mist can produce false caking, affects preventing blocking effect, illustrates that liquid anti-agglomeration agent and solid anti-hard caking agent should separately add.Because fumed silica particle diameter is little, may be that crushing process is pulled away by wind, reduce actual consumption.
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.The mobility of comparative example 6 gained sample salt of wormwood super-fine powder is 104 seconds.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood micro mist and whether can all suspend, whether have layering.Can suspending of gained sample salt of wormwood super-fine powder, but there is obvious demixing phenomenon, the salt of wormwood of visible a small amount of caking shape of reuniting bottom graduated cylinder.
Comparative example 6, cancel whole step 1), that is, particle salt of wormwood directly carry out step 2); And cancellation step 4) in the use of 2 kilograms of solid anti-hard caking agents; All the other are equal to embodiment 1.
The salt of wormwood super-fine powder of final gained detects size distribution, flowing property, suspension property and settling time as requested.
Table 8, comparative example 6 gained salt of wormwood super-fine powder size distribution
As can be seen from table 8 and Fig. 5, do not add octadecylamine acetate salt, dimethyl silicone oil and solid anti-hard caking agent fumed silica, pulverize gained salt of wormwood ultra micro powder ball and get caking seriously, particle diameter does not obviously reach requirement.
The detection of mobility: take 100 grams of test samples, evaluate mobility with the funnel required time being 12mm full by nozzle diameter, the time is longer, and to represent mobility poorer.The mobility of comparative example 8 gained sample salt of wormwood super-fine powder is 187 seconds.
Suspension property: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, observing salt of wormwood micro mist and whether can all suspend, whether have layering.Comparative example 8 gained salt of wormwood super-fine powder suspension property is very poor, obvious layering, has the salt of wormwood of many caking shapes of reuniting bottom graduated cylinder.
Settling time: 150 milliliters of tool plug glass cylinders, pour the dehydrated alcohol of 100 milliliters into, then 10 grams of super-fine powder salt of wormwood samples are added, fluctuate after jumping a queue, until super-fine powder salt of wormwood is not deposited in bottom graduated cylinder, under being positioned over horizontal stand, with the stopwatch meter salt of wormwood settling time, till no longer reducing with sedimentation face.The settling time of comparative example 8 gained salt of wormwood super-fine powder is 247 seconds, and settling velocity is very fast.
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (9)
1. the preparation method of the salt of wormwood super-fine powder of not reuniting, is characterized in that comprising the following steps:
1) add liquid anti-caking additive, Homogeneous phase mixing in the salt of wormwood of temperature of, toward the rear band of calcining having a surplus, the weight ratio of described liquid anti-caking additive and salt of wormwood is 0.1 ~ 0.3%;
2), by step 1) potassium carbonate mixtures of gained pulverizes, and collection cut size≤100 micron, as salt of wormwood super-fine powder I after pulverizing;
3), by step 2) the salt of wormwood super-fine powder I of gained moves in transfer container, naturally cools to room temperature, obtain cooled salt of wormwood super-fine powder II;
4), to step 3) add the solid anti-hard caking agent accounting for cooled salt of wormwood super-fine powder II weight 0.2 ~ 1% in the cooled salt of wormwood super-fine powder II of gained, and carry out secondary stirring mixing, obtain the mixed salt of wormwood super-fine powder III of secondary;
5), by step 4) the mixed salt of wormwood super-fine powder III of the secondary of gained is by classification, and collection cut size≤100 micron is salt of wormwood super-fine powder of not reuniting.
2. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 1, is characterized in that: described step 5) in, the salt of wormwood that particle diameter > is 100 microns is back to step 2) proceed to pulverize.
3. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 1 and 2, it is characterized in that: described step 2) in, potassium carbonate mixtures after pulverizing is passed through classification, particle diameter≤100 micron are judged to reach Particle size requirements, the carrying out reaching Particle size requirements is collected, must pulverize rear salt of wormwood super-fine powder I, the carrying out not reaching Particle size requirements is pulverized again.
4. the preparation method of the salt of wormwood super-fine powder of not reuniting according to claim 1,2 or 3, is characterized in that: described step 1) in liquid anti-caking additive be that the primary octadecylamine acetate of 1:1 and dimethyl silicone oil form by weight ratio.
5. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 4, is characterized in that: described step 4) in solid anti-hard caking agent be at least one in tricalcium phosphate, talcum powder or white carbon black.
6. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 5, it is characterized in that: described step 1) be: liquid anti-caking additive is first scattered in solvent, then sprays band after firing equably by atomizer and have a surplus in the salt of wormwood of temperature;
The mass ratio of described liquid anti-caking additive and solvent is 1:1.5 ~ 2.5, and described solvent is dehydrated alcohol or anhydrous methanol.
7. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 6, is characterized in that: described step 2) in, pulverize and adopt air-flow vortex pulverizing mill, classification adopts grading machine, collects and adopts cyclonic separation unit;
Described air-flow vortex pulverizing mill, grading machine, cyclonic separation unit and bag-type dust collector are arranged in order, and the air outlet of described bag-type dust collector aims at the blast inlet of air-flow vortex pulverizing mill, thus realize using recirculating air;
When supplementing new wind, described new wind is the clean dry air met the following conditions: relative humidity is less than 30%, and residua content is less than 0.1ppm, and filters through the accurate filter of 0.45 micron pore size.
8. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 7, is characterized in that: described cyclonic separation unit is secondary cyclone.
9. the preparation method of salt of wormwood super-fine powder of not reuniting according to claim 4, is characterized in that: described step 4) secondary stirring mix stirring mixer used for side cone or bipyramid, mixing time is 0.5 ~ 2 hour.
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| CN110790235A (en) * | 2019-11-15 | 2020-02-14 | 浙江大洋生物科技集团股份有限公司 | Comprehensive utilization method of fluorine-containing potassium chloride as organic synthesis byproduct |
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| US5441669A (en) * | 1994-07-05 | 1995-08-15 | Seper; Karl W. | Preventing potassium bicarbonate from caking |
| CN1219506A (en) * | 1997-12-09 | 1999-06-16 | 韩思文 | Anticaking agent for ammonium nitrate |
| 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 |
| CN102259839A (en) * | 2011-06-17 | 2011-11-30 | 德化县新隆泰化工实业有限公司 | Anticaking agent special for potassium chlorate |
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| US5441669A (en) * | 1994-07-05 | 1995-08-15 | Seper; Karl W. | Preventing potassium bicarbonate from caking |
| CN1219506A (en) * | 1997-12-09 | 1999-06-16 | 韩思文 | Anticaking agent for ammonium nitrate |
| 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 |
| CN102259839A (en) * | 2011-06-17 | 2011-11-30 | 德化县新隆泰化工实业有限公司 | Anticaking agent special for potassium chlorate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110790235A (en) * | 2019-11-15 | 2020-02-14 | 浙江大洋生物科技集团股份有限公司 | Comprehensive utilization method of fluorine-containing potassium chloride as organic synthesis byproduct |
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