CN103820253A - Process and device for continuously preparing powdery MES (fatty acid methyl ester sulfonate) particles - Google Patents
Process and device for continuously preparing powdery MES (fatty acid methyl ester sulfonate) particles Download PDFInfo
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- CN103820253A CN103820253A CN201410048579.9A CN201410048579A CN103820253A CN 103820253 A CN103820253 A CN 103820253A CN 201410048579 A CN201410048579 A CN 201410048579A CN 103820253 A CN103820253 A CN 103820253A
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- 239000002245 particle Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 21
- 235000019387 fatty acid methyl ester Nutrition 0.000 title claims abstract description 20
- 230000008569 process Effects 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 23
- 150000002148 esters Chemical class 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000428 dust Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 238000007701 flash-distillation Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 20
- 238000006386 neutralization reaction Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000005469 granulation Methods 0.000 claims description 13
- 230000003179 granulation Effects 0.000 claims description 13
- 230000003472 neutralizing effect Effects 0.000 claims description 13
- 230000007246 mechanism Effects 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910021536 Zeolite Inorganic materials 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 150000001447 alkali salts Chemical class 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 238000006277 sulfonation reaction Methods 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 19
- 238000004090 dissolution Methods 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000005453 pelletization Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005550 wet granulation Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000004702 methyl esters Chemical class 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010410 dusting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 229940023462 paste product Drugs 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 229960003010 sodium sulfate Drugs 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 229940038773 trisodium citrate Drugs 0.000 description 2
- 206010009866 Cold sweat Diseases 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 229920003109 sodium starch glycolate Polymers 0.000 description 1
- 229940079832 sodium starch glycolate Drugs 0.000 description 1
- 239000008109 sodium starch glycolate Substances 0.000 description 1
- 229940056729 sodium sulfate anhydrous Drugs 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- -1 supercarbonate Chemical compound 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 235000019263 trisodium citrate Nutrition 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a process and a device for continuously preparing powdery MES (fatty acid methyl ester sulfonate) particles. A process flow is simple, and the provided preparation device is simple in structure. According to the technical scheme, the process for continuously preparing the powdery MES particles comprises the following steps of (1) causing a powdery mixture of a neutralizer, a wrapper and a stabilizer and fatty acid methyl ester acid ester to enter a high-shear reactor according to a certain proportion; (2) forming MES particles, and causing the MES particles to enter a flash dryer; (3) keeping the obtained MES particles at certain granularity; (4) causing mixed airflow discharged from an outlet of the flash dryer to enter a cyclone separator for separation; (5) obtaining a finished product. The device for continuously preparing the powdery MES particles comprises the high-shear reactor, the flash dryer, the cyclone separator, a bag-type dust collector and an induced draft fan, which are sequentially communicated, wherein the high-shear reactor is provided with an acid ester inlet, a powder inlet, an air inlet and a material outlet communicated with the flash dryer respectively.
Description
Technical field
The present invention relates to a kind of manufacturing process of surfactant particles, especially the manufacturing process of methyl sodiosul foaliphatate particle.
Background technology
Methyl sodiosul foaliphatate (MES) is a kind of novel anion surfactant, excellent property, has a extensive future, and can replace petroleum base tensio-active agent as LAS, AOS etc., meets the overall development trend of resource and environment.Research shows, methyl sodiosul foaliphatate has good soil removability, little to skin irritation, performance gentleness, without irritated, and toxicity is low, safe, can be in a large number for various liquid, powdered detergent.
The production main processes of MES is the lipid acid being obtained through techniques such as hydrolysis or saponification acidolysis by natural animal-plant oil, obtain fatty acid methyl ester with methanol esterification again, methyl esters and gas phase sulfur trioxide sulfonation, resterification, decolouring, neutralization obtain paste product, or continue the dry powder-like product that obtains.Wherein paste product content is in 30% left and right, and its product can because of the reduction of the envrionment temperatures such as storage, isolate water-yielding stratum and similar bean dregs sample solidification layer cause material inhomogeneous, affect outward appearance and use; 80% powdery or chip solid MES are producing in drying process, and material can experience by lotion, high viscosity fluid, and the phase change of the three phases of Zhongdao chip solid or powder, exists energy consumption large, the problem that continuous production is poor.
The application of current MES in washing powder remains in certain restriction, this is mainly because the production of current laundry powder mainly adopts high tower spraying (high-temperature hot-air in 250～350 ℃ is produced), because the temperature of dusting is higher, and powder spraying slurry is generally alkalescence, easily causes the decomposition of MES in the process of dusting.
For addressing this problem, generally tend to now rear allotment of labor's skill, first MES is processed into MES particle and is fitted on afterwards again in washing powder.The production of granular MES product, currently mainly be divided into wet granulation and non-slurry pelletizing, wherein wet granulation is take the disclosed CN103320235A of Na Aisi " particle of a kind of fatty acids methyl esters sodium sulfonate and preparation method thereof " as representative, it adopts paste MES(is 30%MES) carry out wet granulation with zeolite, silicate, modified starch and wilkinite, then drying, sub-sieve obtain; Wherein non-slurry pelletizing is take the biological disclosed CN102277238A of enlightening health as representative; it adopts 80% sheet MES is raw material; after mixing with Sodium sulfate anhydrous.min(99), 4A zeolite, sodium starch glycolate and wilkinite; extruding pelletization in the situation that there is outer protection wind, is cooled to sclerosis completely through-5～30 ℃ of dry airs and obtains particle.These preparation technologies all have its weak point:
1) adopt wet granulation, moisture higher in particle, need to further be dried, energy consumption is larger, and in drying process, temperature control is too high also there will be the phenomenons such as particle is clamminess; Adopt non-slurry pelletizing, need to select the MES of high-content, high-content MES has on the make passed through the drying process of highly energy-consuming.
2), because the Krafft's point of MES self is higher, caused the dissolution in low temperature of these two kinds of MES particles poor.
3) technique process complexity, production efficiency is lower, and production capacity is subject to larger restriction.
Therefore, how developing that a kind of technique is simple, the preparation method of energy-conserving and environment-protective, powdery MES product that production efficiency high and low temperature solvability is good, MES is applied in washing powder, is a difficult problem urgently to be resolved hurrily.
Summary of the invention
The object of the invention is to overcome the deficiency in above-mentioned background technology, provide a kind of serialization to prepare technique and the preparation facilities thereof of powdery MES particle.The technique providing has that technical process is simple, energy-conserving and environment-protective, feature that production efficiency is high, and the powdery MES particle flow that obtains is good, be difficult for bonding, and dissolution in low temperature is good, can be directly used in allotment of labor's skill after washing powder; The preparation facilities providing is simple in structure, easy to manufacture, and cost is lower.
Technical scheme of the present invention is:
A technique for powdery MES particle is prepared in serialization, comprises the following steps
1) pulverulent mixture of neutralizing agent, coating agent, stablizer enters a high-shear reactor by a certain percentage, and the fatty acid methyl ester acid esters that fatty acid methyl ester forms after sulfonation simultaneously also enters high-shear reactor by a certain percentage;
2) material stops 10～60s in high-shear reactor reactor, neutralization reaction occurs and be wrapped to form MES particle; Then open induced draft fan, the dual function that MES particle send by centrifugal force and wind enters flash distillation dryer from high-shear reactor output;
3) from the output of flash distillation dryer top, enter cyclonic separator by upstream effect through the MES particle of flash distillation dryer processing, utilize during this time air-flow to remove a small amount of water of neutralization heat and neutralization generation, make MES particle cooling (be cooled to and be less than 40 ℃) dry (be dried to water content and be less than 5%); Control blast simultaneously and make the thicker MES particle of part get back to further pulverizing of continuation in high-shear reactor, make the MES particle obtaining maintain certain granules degree;
4) mixed airflow that exports out from flash distillation dryer enters cyclonic separator and separates, and isolated pulverulent material directly enters finished powder storehouse, and isolated mixed airflow enters after sack cleaner dedusting, emptying by induced draft fan;
5) in finished powder storehouse, MES particle packing obtains finished product; Bag-type dust separates the part dust obtaining and gets back to high-shear reactor entrance continuation reaction granulation;
The part by weight that feeds intake in described step 1) is: 20～40 parts of fatty acid methyl ester acid esters, 2～10 parts of neutralizing agents, 50～75 parts of coating agents, 0～1 part of stablizer.
Described neutralizing agent is the mixing of one or two or more kinds arbitrary proportion in basic salt, basic oxide, alkaline hydrated oxide; Its metal ion is at least one in sodium, potassium, magnesium, calcium.Described basic salt is the mixture of one or two or more kinds arbitrary proportion in carbonate, supercarbonate, silicate, described basic oxide are mixing of one or two or more kinds arbitrary proportion in sodium oxide, potassium oxide, magnesium oxide, calcium oxide, and described alkaline hydrated oxide is mixing a kind of in sodium hydroxide, potassium hydroxide or two kinds of arbitrary proportions.
Described coating agent is the mixing of one or two or more kinds arbitrary proportion in 4A zeolite, wilkinite, diatomite, sodium sulfate.
Described stablizer is the mixing of one or two or more kinds arbitrary proportion in citric acid, Citrate trianion, phosphoric acid, phosphoric acid salt, hydrophosphate, metal ion be wherein receive, at least one in potassium, magnesium calcium.
In the pulverulent mixture of described neutralizing agent, coating agent, stablizer, can also add part discoloring agent, tinting material; Described discoloring agent can be hypochlorite, percarbonate etc., metal ion be wherein receive, at least one in potassium, magnesium calcium.
A kind of powdery MES particle serialization preparation facilities, is characterized in that this device comprises high-shear reactor, flash distillation dryer, cyclone separator, sack cleaner and the induced draft fan being communicated with successively by pipeline; The horizontal layout of described high-shear reactor and be shaped with respectively acid esters entrance, powder entrance, gas inlet and connect the material outlet of flash distillation dryer.
Described high-shear reactor comprises: a horizontal layout and the cylindrical reactor vessel, that is shaped with respectively acid esters entrance, powder entrance, material outlet and gas inlet are positioned carry out the stirring cutting mechanism of high speed shear and drive the transmission rig that stirs cutting mechanism in reaction vessel and to material in reaction vessel; Described acid esters entrance, powder entrance are positioned at one end of reactor; Gas inlet, material outlet are positioned at the other end of reactor.
Described stirring cutting mechanism comprise pass through reaction vessel two ends and with the coaxially arranged stir shaft of reaction vessel, be positioned at reaction vessel and be distributed on multiple agitating vanes of stir shaft circumferential surface and be fixed on several baffle plates of reaction vessel inwall.
One end of described agitating vane is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane also, around the line inclination certain angle at its two ends, promotes to form the drive surface that material moves along reaction vessel axis.
Described baffle plate is the ring plate being arranged between adjacent two baffle plates, this dull and stereotyped circumferential periphery is along being fixed on reaction vessel inwall, and inner periphery edge stretches and keeps certain spacing passage as Flow of Goods and Materials with described stir shaft toward reaction vessel internal diameter direction.
The shell of described flash distillation dryer is a cylinder of vertically installing, and mixed gas outlet is positioned at cylinder top, and material inlet is positioned at cylinder bottom and directly communicates with the material outlet of high speed shear device.
Described cyclone separator comprises cyclonic separator and is positioned at the finished powder storehouse of cyclonic separator below; Described cyclonic separator opening for feed is by the mixed airflow outlet of pipeline communication flash distillation dryer; Described cyclonic separator is one or two and is connected in series and forms above.
The present invention compared with prior art, has following outstanding advantages:
1) use fatty acid methyl ester acid esters directly in and granulation, the MES particle moisture content less (<3%) obtaining, simply dryly just can obtain qualified product, has avoided in use high tower spray drying, energy consumption high material easily decomposes.
2) shortcomings such as neutralization parcel completes simultaneously, and the MES particle component obtaining is more even, and the coating agent of having avoided existing in conventional granulation process easily departs from, particle component is inhomogeneous; Due to fabulous being scattered in MES such as coating agents, while particularly using carbonate to make neutralizing agent, in finished product MES particle, more microbubble can be there is simultaneously, the dissolution in low temperature of MES particle can be greatly improved.
3) directly utilize neutralization heat, MES particle is dried, capacity usage ratio high (with CN103320235A, CN102277238A comparison, can save energy more than 70%);
4) in conjunction with high-shear reactor and flash distillation dryer, the material particles degree obtaining is evenly controlled, and particle diameter is at 30～50 orders, without further pulverizing.
5) serialization that realizes granulation is produced, and production efficiency improves (with CN102277238A comparison, production efficiency improves 500%) greatly.
6) apparatus structure is simple, easily manufactured easy, and cost is lower.
Accompanying drawing explanation
Fig. 1 is the structural representation of powdery MES particle serialization preparation facilities;
Fig. 2 is the structural representation of high-shear reactor in Fig. 1 device.
Wherein 1 is fatty acid methyl ester acid esters, 2 is the mixture of neutralizing agent, coating agent and stablizer, and 3 is air, and 4 is high-shear reactor, 5 is flash distillation dryer, 6 is cyclone separator, and 7 is product outlet, and 8 is sack cleaner, 9 is dust outlet, 10 is induced draft fan, and 11 is input funnel, 6-1 finished powder storehouse;
1-1 is powder entrance, and 1-2 is acid esters entrance, and 1-3 is gas inlet, and 1-4 is material outlet, and 1-5 is agitating vane, and 1-6 is baffle plate, and 1-7 is shear agitation mechanism, and 1-8 is cylindrical reactor vessel, and 1-9 is transmission rig, and 1-10 is stir shaft.
Embodiment
Below in conjunction with accompanying drawing, invention is described further.
Thinking of the present invention be utilize fatty acid methyl ester acid esters directly direct in high-shear reactor with neutralizing agent, coating agent and stablizer in and granulation, and utilize normal temperature wind remove neutralization heat and be dried a small amount of water that removes reaction generation, control wind pressure and wind speed simultaneously and optionally make large footpath particle continue to get back to the further pulverizing of high-shear reactor do.Here high-shear reactor is reaction granulating equipment, can further play again porphyrization.Avoided like this in conventional MES granulation, be dried the shortcomings such as the energy consumption of bringing is high, equipment is complicated, and equipment has been simple, utilization ratio is high, can realize continuous and stable production, has greatly improved production efficiency.The shortcomings such as simultaneously, because neutralization parcel completes simultaneously, the MES particle component obtaining is more even, and the coating agent of having avoided existing in conventional granulation process easily departs from, particle component is inhomogeneous, coating agent etc. is evenly distributed in MES particle simultaneously; Neutralizing agent adopts basic salt (preferably use carbonate, supercarbonate, or use silicate), basic oxide (mixing of one or two or more kinds arbitrary proportion in preferential oxidation sodium, potassium oxide, magnesium oxide, calcium oxide), alkaline hydrated oxide (the preferably mixing of a kind of or two kinds of arbitrary proportions in sodium hydroxide, potassium hydroxide); In the MES particle that production obtains, contain more small pore, these can greatly improve the dissolution in low temperature of MES particle.The effect of stablizer is to make the pH value of N-process more stable, prevents that peracid from crossing the decomposition that alkali factor causes product.
As seen from the figure, device of the present invention is mainly made up of high-shear reactor 4, flash distillation dryer 5, cyclone separator 6, sack cleaner 8 and induced draft fan 10.Wherein the Main Function of high-shear reactor is to make MES acid esters and neutralizing agent, the rapid contact reacts of coating agent shear granulation, large particle is realized further and being pulverized simultaneously; The Main Function of flash distillation dryer is to utilize normal temperature wind MES particle to be lowered the temperature and remove a small amount of water to be dried; The Main Function of cyclone separator is to collect MES particle.
In described high-shear reactor: the horizontal layout of cylindrical reactor vessel 1-8, left end is shaped with respectively the mixed powder of fatty acid methyl ester acid esters entrance 1-2 and powder entrance 1-1(neutralizing agent, coating agent and stablizer can directly transport to this powder entrance, or transport to this powder entrance by input funnel 11), right-hand member is shaped with material outlet 1-4, gas inlet 1-3; Be positioned at reaction vessel, the motor-driven band wheel mechanism of transmission rig 1-9(for the 1-7 of shear agitation mechanism that material in reaction vessel is carried out to shear agitation) shear agitation mechanism is driven.In shear agitation mechanism, stir shaft 1-10 axially passes through reaction vessel, and coaxially arranged with reaction vessel; The part stir shaft circumferential surface that is positioned at reaction vessel, is uniformly fixed wtih multiple agitating vane 1-5, and several baffle plates 1-6 is fixed on (baffle number is determined as required, shown 2 baffle plates in figure) on reaction vessel inwall.
One end of above-mentioned agitating vane (being generally plane) is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane is also around the line inclination certain angle at its two ends (be the plane that tilts of agitating vane with stir shaft cross section between the angle that forms), the drive surface moving along reaction vessel axis to form promotion material.The size of described angle determines the speed that material moves, and can be 0-30 degree conventionally; Specifically determine as required.
Described baffle plate is the ring plate being arranged between adjacent two baffle plates; This flat board is also coaxially arranged with reaction vessel, its circumferential periphery is along being fixed on reaction vessel inwall, inner periphery edge stretches and keeps certain spacing (spacing size is set as required) with described stir shaft toward reaction vessel internal diameter direction, forms the passage of Flow of Goods and Materials.
Above-mentioned high-shear reactor can simply be processed and obtain, and above-mentioned flash distillation dryer, cyclone separator, sack cleaner and induced draft fan all outsourcing obtain.
Further illustrate by specific embodiment below.
Embodiment 1
1,1t/h MES particle production line
Sodium carbonate, 4A zeolite, citric acid (weight ratio 7:9:1) are with the flow of 700kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 300kg/h, in carrying out therein and granulation; High-shear reactor is selected the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 55 ℃; Material output afterwards enters flash distillation dryer again, opens induced draft fan simultaneously and makes material in flash distillation dryer lower the temperature rapidly and remove neutralization generation moisture; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtaining is as follows:
| Index | Result |
| Actives, % | 30.6 |
| Disodium salt (folding hundred), % | 3.4 |
| Tap density, g/ml | 0.66 |
| Granularity D90, μ m | 380 |
| Dissolution in low temperature | Qualified |
2,1t/h MES particle production line
Sodium bicarbonate, sodium sulfate and Trisodium Citrate (weight ratio 2:5:1) are with the flow of 650kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 350kg/h, in carrying out therein and granulation; High-shear reactor is selected the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 57 ℃; Material output afterwards enters flash distillation dryer again, opens induced draft fan simultaneously and makes material in flash distillation dryer lower the temperature rapidly and remove neutralization generation moisture; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtaining is as follows:
| Index | Result |
| Actives, % | 35.1 |
| Disodium salt (folding hundred), % | 2.7 |
| Tap density, g/ml | 0.71 |
| Granularity D90, μ m | 371 |
| Dissolution in low temperature | Qualified |
3,1t/h MES particle production line
Sodium carbonate, wilkinite and sodium phosphate (weight ratio 7:9:1) are with the flow of 700kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 300kg/h, in carrying out therein and granulation; High-shear reactor is selected the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 55 ℃; Material output afterwards enters flash distillation dryer again, opens induced draft fan simultaneously and makes material in flash distillation dryer lower the temperature rapidly and remove neutralization generation moisture; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtaining is as follows:
| Index | Result |
| Actives, % | 30.6 |
| Disodium salt (folding hundred), % | 2.6 |
| Tap density, g/ml | 0.69 |
| Granularity D90, μ m | 371 |
| Dissolution in low temperature | Qualified |
4,1t/h MES particle production line
Sodium carbonate, 4A zeolite and Trisodium Citrate (weight ratio 1:20:0.05) are with the flow of 800kg/h, and fatty acid methyl ester acid esters enters high-shear reactor with the flow of 200kg/h, in carrying out therein and granulation; High-shear reactor is selected the reactor of volume 10L, material mean residence time 10s, and neutralization is warming up to 51 ℃; Material output afterwards enters flash distillation dryer again, opens induced draft fan simultaneously and makes material in flash distillation dryer lower the temperature rapidly and remove neutralization generation moisture; Regulate blast control discharging MES particle diameter;
The MES particle index finally obtaining is as follows:
| Index | Result |
| Actives, % | 21.6 |
| Disodium salt (folding hundred), % | 2.6 |
| Tap density, g/ml | 0.64 |
| Granularity D90, μ m | 367 |
| Dissolution in low temperature | Qualified |
Claims (10)
1. a technique for powdery MES particle is prepared in serialization, comprises the following steps
1) pulverulent mixture of neutralizing agent, coating agent, stablizer enters a high-shear reactor by a certain percentage, and the fatty acid methyl ester acid esters of fatty acid methyl ester after sulfonation also enters high-shear reactor by a certain percentage simultaneously;
2) material stops 10～60s in high-shear reactor reactor, neutralization reaction occurs and be wrapped to form MES particle; Then from high-shear reactor output, enter flash distillation dryer;
3) after the MES particle output of flash distillation dryer processing, enter cyclonic separator, lower the temperature and be dried; Make the thicker MES particle of part get back in high-shear reactor simultaneously and continue further to pulverize, make the MES particle obtaining maintain certain granules degree;
4) mixed airflow that exports out from flash distillation dryer enters cyclonic separator and separates, and isolated pulverulent material directly enters finished powder storehouse, and isolated mixed airflow enters after sack cleaner dedusting emptying;
5) in finished powder storehouse, MES particle packing obtains finished product; Bag-type dust separates the part dust obtaining and gets back to high-shear reactor entrance continuation reaction granulation;
The part by weight that feeds intake in described step 1) is: 20～40 parts of fatty acid methyl ester acid esters, 2～10 parts of neutralizing agents, 50～75 parts of coating agents, 0～1 part of stablizer.
2. the mixing that described neutralizing agent according to claim 1 is one or two or more kinds arbitrary proportion in basic salt, basic oxide, alkaline hydrated oxide; Metal ion is wherein at least one in sodium, potassium, magnesium, calcium.
3. the technique of powdery MES particle is prepared in serialization according to claim 2, it is characterized in that: described coating agent is the mixing of one or two or more kinds arbitrary proportion in 4A zeolite, wilkinite, diatomite, sodium sulfate.
4. the technique of powdery MES particle is prepared in serialization according to claim 3, it is characterized in that: described stablizer is the mixing of one or two or more kinds arbitrary proportion in citric acid, Citrate trianion, phosphoric acid, phosphoric acid salt, hydrophosphate; Metal ion is wherein at least one in sodium, potassium, magnesium, calcium.
5. a powdery MES particle serialization preparation facilities, is characterized in that this device comprises high-shear reactor (4), flash distillation dryer (5), cyclone separator (8), sack cleaner and the induced draft fan being communicated with successively by pipeline; The horizontal layout of described high-shear reactor and be shaped with respectively acid esters entrance (1-2), powder entrance (1-1), gas inlet (1-3) and connect the material outlet (1-4) of flash distillation dryer.
6. powdery MES particle serialization preparation facilities according to claim 5, is characterized in that: described high-shear reactor comprises: a horizontal layout and the cylindrical reactor vessel, that is shaped with respectively fatty acid methyl ester acid esters entrance, powder entrance, material outlet and gas inlet are positioned carry out the stirring cutting mechanism of high speed shear and drive the transmission rig that stirs cutting mechanism in reaction vessel and to material in reaction vessel; Described fatty acid methyl ester acid esters entrance, powder entrance are positioned at one end of reactor; Gas inlet, material outlet are positioned at the other end of reactor.
7. powdery MES particle serialization preparation facilities according to claim 6, is characterized in that: described stirring cutting mechanism comprises and passes through reaction vessel two ends and the stir shaft (1-10) coaxially arranged with reaction vessel, be positioned at reaction vessel and be distributed on multiple agitating vanes (1-5) of stir shaft circumferential surface and be fixed on several baffle plates (1-6) of reaction vessel inwall.
8. powdery MES particle serialization preparation facilities according to claim 7, is characterized in that: one end of described agitating vane is fixed on stir shaft, and the other end stretches to the outer diameter; Agitating vane also, around the line inclination certain angle at its two ends, promotes to form the drive surface that material moves along reaction vessel axis.
9. powdery MES particle serialization preparation facilities according to claim 8, it is characterized in that: described baffle plate is the ring plate being arranged between adjacent two baffle plates, this dull and stereotyped circumferential periphery is along being fixed on reaction vessel inwall, and inner periphery edge stretches and keeps certain spacing passage as Flow of Goods and Materials with described stir shaft toward reaction vessel internal diameter direction.
10. powdery MES particle serialization preparation facilities according to claim 9, is characterized in that: described cyclone separator comprises cyclonic separator and is positioned at the finished powder storehouse of cyclonic separator below; Described cyclonic separator opening for feed is by the mixed airflow outlet of pipeline communication flash distillation dryer; Described cyclonic separator is one or two and is connected in series and forms above.
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| CN108727233A (en) * | 2018-07-27 | 2018-11-02 | 赞宇科技集团股份有限公司 | A kind of drying technology and device improving alpha-sulfo methyl hexadecanoate sodium dissolution in low temperature |
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