CN101670251B - A kind of manufacture method of spherical anionic surfactant - Google Patents
A kind of manufacture method of spherical anionic surfactant Download PDFInfo
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- CN101670251B CN101670251B CN2009100994815A CN200910099481A CN101670251B CN 101670251 B CN101670251 B CN 101670251B CN 2009100994815 A CN2009100994815 A CN 2009100994815A CN 200910099481 A CN200910099481 A CN 200910099481A CN 101670251 B CN101670251 B CN 101670251B
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- 239000003945 anionic surfactant Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000000463 material Substances 0.000 claims abstract description 109
- 238000005469 granulation Methods 0.000 claims abstract description 35
- 230000003179 granulation Effects 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 33
- 238000001125 extrusion Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- -1 paratoluenesulfonic acid sodium salt Chemical class 0.000 claims description 20
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 14
- 235000011152 sodium sulphate Nutrition 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 235000002639 sodium chloride Nutrition 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 5
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 5
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 235000010981 methylcellulose Nutrition 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 235000011008 sodium phosphates Nutrition 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- LNAZSHAWQACDHT-XIYTZBAFSA-N (2r,3r,4s,5r,6s)-4,5-dimethoxy-2-(methoxymethyl)-3-[(2s,3r,4s,5r,6r)-3,4,5-trimethoxy-6-(methoxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6r)-4,5,6-trimethoxy-2-(methoxymethyl)oxan-3-yl]oxyoxane Chemical compound CO[C@@H]1[C@@H](OC)[C@H](OC)[C@@H](COC)O[C@H]1O[C@H]1[C@H](OC)[C@@H](OC)[C@H](O[C@H]2[C@@H]([C@@H](OC)[C@H](OC)O[C@@H]2COC)OC)O[C@@H]1COC LNAZSHAWQACDHT-XIYTZBAFSA-N 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 239000002202 Polyethylene glycol Substances 0.000 claims 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 1
- 125000001931 aliphatic group Chemical group 0.000 claims 1
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 claims 1
- 229910021653 sulphate ion Inorganic materials 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000012798 spherical particle Substances 0.000 abstract description 5
- 238000005563 spheronization Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 22
- 239000008187 granular material Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 230000033228 biological regulation Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000007873 sieving Methods 0.000 description 7
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 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 description 4
- 230000001788 irregular Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 150000008051 alkyl sulfates Chemical class 0.000 description 3
- 239000004566 building material Substances 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 239000004088 foaming agent Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920000084 Gum arabic Polymers 0.000 description 2
- 241000978776 Senegalia senegal Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000205 acacia gum Substances 0.000 description 2
- 235000010489 acacia gum Nutrition 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000021050 feed intake Nutrition 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- 238000013268 sustained release Methods 0.000 description 2
- 239000012730 sustained-release form Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- RZXLPPRPEOUENN-UHFFFAOYSA-N Chlorfenson Chemical compound C1=CC(Cl)=CC=C1OS(=O)(=O)C1=CC=C(Cl)C=C1 RZXLPPRPEOUENN-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 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
- 238000005187 foaming Methods 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229960003943 hypromellose Drugs 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229940069328 povidone Drugs 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D10/00—Compositions of detergents, not provided for by one single preceding group
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/20—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by expressing the material, e.g. through sieves and fragmenting the extruded length
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Detergent Compositions (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
技术领域 technical field
本发明涉及一种圆球形阴离子表面活性剂产品的制造方法。该产品可用于民用、工业用清洗剂,建材发泡剂等产品中。The invention relates to a manufacturing method of a spherical anionic surfactant product. The product can be used in civil and industrial cleaning agents, foaming agents for building materials and other products.
背景技术 Background technique
阴离子表面活性剂除了以一定浓度(含~35%或~70%活性物)的液体形态供货外,还有采用粉末(细小不规则颗粒)状、颗粒(稍大不规则颗粒)状、片状或针(圆条)状等固体形态供货。以前,固体形态阴离子表面活性剂制造方法有:In addition to being supplied in liquid form with a certain concentration (containing ~35% or ~70% active matter), anionic surfactants are also available in the form of powder (fine irregular particles), granules (slightly larger irregular particles), tablets, etc. It is supplied in solid form such as shape or needle (round bar) shape. Previously, solid form anionic surfactants were manufactured by:
采用含水量60~70%(重量)的低浓度浆料为原料,通过高塔喷雾干燥的方法制取。如,日本专利:特开昭55-69698、特开昭53-39037,中国专利:ZL00131365.7所公开的制造方法;或采用含固体量60~80%(重量)的高浓度浆料,以喷雾干燥的方式制取。如日本专利:特开昭54-106428公开的方式。上述方法制得的为粉末(细小不规则颗粒)状产品,粒径小且不规则,视密度低,生产和使用过程中物料容易结团,造成溶解困难,同时还会产生大量的粉尘飞扬,危害健康和污染环境。The low-concentration slurry with a water content of 60-70% (weight) is used as a raw material, and is prepared by a high-tower spray-drying method. Such as, Japanese patent: JP 55-69698, JP 53-39037, Chinese patent: the disclosed manufacturing method of ZL00131365.7; Prepared by spray drying. Such as Japanese patent: the mode disclosed in JP-A-54-106428. The product obtained by the above method is a powder (fine irregular particle) product with small and irregular particle size and low apparent density. During production and use, the material is easy to agglomerate, resulting in difficulty in dissolution, and simultaneously a large amount of dust is generated. Hazardous to health and pollute the environment.
在流化床设备内,采用喷射含固体量60~80%(重量)的高浓度浆料,以喷雾造粒、附聚成型和逐层涂覆的方式制得粒状的阴离子表面活性剂。如,中国专利:ZL 200510048907.6所公开的制造方法。还有,欧洲专利6140301公开了一种使用液体粘结剂和粉同时喷雾,附聚成颗粒状洗涤剂的方法。依据上述方法制取的是一种近似球形的,较大粒径的颗粒状阴离子表面活性剂。但是均存在粒径不易控制,颗粒大小不匀,粒径分布宽,颗粒强度低易于粉化,颗粒致密度低影响溶解等问题。In the fluidized bed equipment, the granular anionic surfactant is prepared by spraying granulation, agglomeration molding and layer-by-layer coating by spraying high-concentration slurry with a solid content of 60-80% (weight). For example, the manufacturing method disclosed in Chinese patent: ZL 200510048907.6. Also, European Patent No. 6140301 discloses a method for agglomerating a granular detergent by spraying simultaneously a liquid binder and a powder. Prepared according to the above-mentioned method is an approximately spherical, granular anionic surfactant with a larger particle size. However, there are problems such as difficult control of particle size, uneven particle size, wide particle size distribution, low particle strength and easy pulverization, and low particle density affecting dissolution.
日本专利特开平2-222498公开了一种用含水20%~35%(重量)的高浓度浆料,经真空薄膜连续干燥的工艺。美国专利US5723433公开了用湍流管式干燥器(TTD)先进行两相湍流传热,再进行真空闪蒸来干燥脂肪酸甲酯磺酸盐等阴离子表面活性剂的方式,但该方法常使管道堵塞,影响生产。关键是上述方法没有解决产品造粒技术。Japanese Patent Laid-Open No. 2-222498 discloses a process of continuously drying a vacuum film with a high-concentration slurry with a water content of 20% to 35% (weight). U.S. Patent No. 5,723,433 discloses a method of using a turbulent tube dryer (TTD) to carry out two-phase turbulent heat transfer, and then carry out vacuum flash evaporation to dry anionic surfactants such as fatty acid methyl ester sulfonate, but this method often causes pipeline blockage ,affect production. The key is that the above method does not solve the product granulation technology.
日本专利特开平5-331496公开了一种,在处于真空环境下的圆筒状外壳内部,输入高密度洗涤剂用膏状原料,利用可旋转板式桨叶的头部在内壁上形成高粘度薄膜,同时,使其快速干燥,得到一种片状干燥物的方法。此法制取的是片状干燥物,流动性差,同时由于高温还存在原料分解的风险。Japanese Patent Laid-Open No. 5-331496 discloses a method in which a high-density detergent paste raw material is input into a cylindrical shell in a vacuum environment, and a high-viscosity film is formed on the inner wall by the head of a rotatable plate blade. , At the same time, make it dry quickly to obtain a method of flake dry matter. What this method produces is flake dry matter, fluidity is poor, and there is the risk of raw material decomposition because of high temperature simultaneously.
美国专利US-A5646107和日本专利JP-A2002-508783,公开了一种用闪蒸干燥器,一边干燥一边造粒的方法。此法造粒压力高,干燥温度也高,不宜用于生产热敏性的阴离子表面活性剂,还存在重新粉化、粒径分布宽等问题。U.S. Patent US-A5646107 and Japanese Patent JP-A2002-508783 disclose a method of granulating while drying with a flash dryer. This method has high granulation pressure and high drying temperature, so it is not suitable for the production of heat-sensitive anionic surfactants, and there are also problems such as re-powdering and wide particle size distribution.
专利WO 2004/111166公开了一种用先将浆体制片或制粒,再经粉碎制成平均粒径为100~150μm的粉体的方法。Patent WO 2004/111166 discloses a method of first tableting or granulating the slurry, and then pulverizing it into a powder with an average particle size of 100-150 μm.
WO-A95/01959公开了一种粉末颗粒烷基硫酸酯的制造方法。WO-A95/01959 discloses a process for the manufacture of powdered and granular alkyl sulfates.
此外,目前在国内外还有一种针(圆条)状烷基硫酸酯制造技术。它是以粉末状烷基硫酸酯为原料,以水作为粘合剂,在螺杆挤出机中,以较高的压力挤出,然后被旋转的切刀切断成长短基本一致的短圆条状物,再经过后续干燥后制取产品。此方法需要较高的挤出压力,发热量大易产生高温,存在产品受热分解的风险。同时制取的产品流动性不好,视密度高,易于粉化,溶解比较困难。In addition, there is currently a needle (round bar)-shaped alkyl sulfate manufacturing technology at home and abroad. It is made of powdered alkyl sulfate and water is used as a binder. It is extruded at a high pressure in a screw extruder, and then cut into long and short round strips by a rotating cutter. material, and then the product is produced after subsequent drying. This method requires high extrusion pressure, high heat generation is easy to generate high temperature, and there is a risk of thermal decomposition of the product. At the same time, the prepared product has poor fluidity, high apparent density, is easy to pulverize, and is difficult to dissolve.
发明内容 Contents of the invention
本发明要解决已有阴离子表面活性剂生产方法不能生产粒径易控制、颗粒大小均匀、颗粒密度与强度适宜的圆球形阴离子表面活性剂,导致阴离子表面活性剂溶解较困难,生产与使用时易污染环境的问题,并解决已有生产方法造粒压力高、干燥温度高而不适合制造热敏性阴离子表面活性剂的问题,以及已有生主方法因发热量大而使产品存在热分解风险的问题,为此提供本发明的一种圆球形阴离子表面活性剂的制造方法,本方法在产品制造和使用全过程中可以实现无粉尘化,消除了污染并改善了劳动条件;本方法制造的产品球形粒子强度适宜,容易溶解且不易粉化;本方法成型时间短、温度低,消除了热敏性物料的分解风险。The present invention aims to solve the problem that the existing anionic surfactant production methods cannot produce spherical anionic surfactants with easy-to-control particle size, uniform particle size, and suitable particle density and strength, which leads to difficulty in dissolving the anionic surfactant and making it difficult to produce and use. The problem of polluting the environment, and solving the problem that the existing production method has high granulation pressure and high drying temperature, which is not suitable for the manufacture of heat-sensitive anionic surfactants, and the problem that the existing production method has a risk of thermal decomposition of the product due to the high calorific value , provide a kind of manufacture method of spherical anionic surfactant of the present invention for this reason, this method can realize dust-free in the whole process of product manufacture and use, has eliminated pollution and improved working condition; The product spherical shape that this method manufactures The particle strength is suitable, easy to dissolve and not easy to pulverize; this method has short molding time and low temperature, which eliminates the risk of decomposition of heat-sensitive materials.
为解决上述问题,本发明采用的技术方案其特殊之处在于:采用挤出、滚圆的造粒工艺;具体为,将阴离子表面活性剂主料与造粒辅料混合后,送入具有螺杆送料器、挤压筒和网孔板组成的挤出机内,在螺杆送料器和挤压筒的共同挤压下,物料通过网孔板形成长短不一的圆条状物料;将所述圆条状物料送入滚圆造粒机,圆条状物料先被滚圆造粒机旋转的离心转盘上的破断齿切断成长短一致的短圆柱状物料颗粒,而后在离心转盘、物料颗粒、造粒机筒壁、造粒机筒壁间的气体共同作用下,所有物料颗粒被搓揉成圆球形颗粒;所述圆球形颗料经干燥、冷却,得到固体含量95~99.5%(重量)的圆球形阴离子表面活性剂。In order to solve the above problems, the special feature of the technical solution adopted by the present invention is that it adopts the granulation process of extrusion and spheronization; specifically, after mixing the anionic surfactant main material and the granulation auxiliary material, it is sent into the In the extruder composed of extrusion barrel and mesh plate, under the co-extrusion of screw feeder and extrusion barrel, the material passes through the mesh plate to form round strip materials of different lengths; the round strip shape The material is fed into the spheronizer, and the round strip material is first cut off by the broken teeth on the centrifugal turntable rotating the spheronizer into long and short cylindrical material granules, and then the material granules in the centrifugal turntable, material granules, and the barrel wall of the granulator are cut. 1. Under the joint action of the gas between the cylinder walls of the granulator, all the material particles are kneaded into spherical particles; the spherical particles are dried and cooled to obtain a spherical anion surface with a solid content of 95-99.5% (weight). active agent.
所述阴离子表面活性剂主料可以是脂肪醇硫酸盐、α-烯基磺酸盐、烷基苯磺酸盐、脂肪醇醚硫酸盐、脂肪酸甲酯磺酸盐中的一种或一种以上的混合物。The main ingredient of the anionic surfactant can be one or more of fatty alcohol sulfate, α-alkenylsulfonate, alkylbenzenesulfonate, fatty alcohol ether sulfate, fatty acid methyl estersulfonate mixture.
所述阴离子表面活性剂主料中的烷基或烯基的碳原子数为8~24。所述主料中,这种碳原子数,对于脂肪醇硫酸盐的最好为12~14,α-烯基磺酸盐的最好为14~18,烷基苯磺酸盐的最好为10~14,脂肪醇醚硫酸盐的最好为12~14,脂肪酸甲酯磺酸盐的最好为16~18。所述盐可以为碱金属盐、碱土金属盐、铵盐、烷醇胺盐。The number of carbon atoms of the alkyl group or alkenyl group in the main material of the anionic surfactant is 8-24. Among the main ingredients, the number of carbon atoms is preferably 12-14 for fatty alcohol sulfate, 14-18 for α-alkenyl sulfonate, and preferably 14-18 for alkylbenzene sulfonate. 10-14, preferably 12-14 for fatty alcohol ether sulfate, and 16-18 for fatty acid methyl ester sulfonate. Said salts may be alkali metal salts, alkaline earth metal salts, ammonium salts, alkanolamine salts.
所述造粒辅料可以是对甲苯磺酸钠、硫酸钠、亚硫酸钠、碳酸钠、碳酸氢钠、柠檬酸、柠檬酸钠(钾)、磷酸钠、磷酸氢钠、磷酸二氢钠、醋酸钠(钾)、氯化钠、羟丙基甲基纤维素、甲基纤维素、羧甲基纤维素钠、淀粉浆、明胶溶液、阿拉伯胶溶液、聚维酮、水、乙醇、丙醇、异丙醇、高级脂肪醇、聚乙二醇中的一种或一种以上的混合物。The granulation auxiliary material can be sodium p-toluenesulfonate, sodium sulfate, sodium sulfite, sodium carbonate, sodium bicarbonate, citric acid, sodium citrate (potassium), sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, sodium acetate ( potassium), sodium chloride, hydroxypropylmethylcellulose, methylcellulose, sodium carboxymethylcellulose, starch slurry, gelatin solution, gum arabic solution, povidone, water, ethanol, propanol, isopropyl One or more mixtures of alcohols, higher fatty alcohols, and polyethylene glycols.
本发明造粒前的表面活性剂主料含水率宜为1.5~25%,优选为3~20%,更优选为5~15%。The moisture content of the surfactant main material before granulation in the present invention is preferably 1.5-25%, preferably 3-20%, more preferably 5-15%.
本发明进入挤出机的阴离子表面活性剂主料与造粒辅料的混合物的固体总含量为85%~97%。The total solid content of the mixture of the anionic surfactant main material and the granulation auxiliary material entering the extruder of the present invention is 85%-97%.
圆球形阴离子表面活性剂的粒径为优选为 The particle size of the spherical anionic surfactant is preferably
本发明可以在成型后的圆球形阴离子表面活性剂外表,再包覆0~25%(重量)的一层厚度均匀的包衣层。In the present invention, the surface of the formed spherical anionic surfactant can be coated with a layer of coating layer with a uniform thickness of 0-25% (by weight).
本发明所述挤出机的螺杆送料器是由单枝、双枝或更多枝螺杆组成的。The screw feeder of the extruder of the present invention is composed of single, double or more screws.
所述挤出机的螺杆送料器的螺杆转速为10~150rpm,优选在25~100rpm。The screw speed of the screw feeder of the extruder is 10-150 rpm, preferably 25-100 rpm.
所述挤出机的网孔板上,均匀布满直径为的圆孔,优选为的圆孔。The mesh plate of the extruder is evenly covered with a diameter of round hole, preferably round hole.
本发明所述挤出机的网孔板是按轴向分布包覆在挤压筒的端面上,或者是以径向分布包覆在挤压筒的外柱面上;所述轴向分布的网孔板是平板或半圆球形状的,径向分布的网孔板是圆筒形、半圆筒形或圆弧形筒状的。The mesh plate of the extruder according to the present invention is coated on the end surface of the extrusion cylinder according to the axial distribution, or is coated on the outer cylindrical surface of the extrusion cylinder with the radial distribution; The mesh plate is in the shape of a flat plate or a hemisphere, and the radially distributed mesh plates are in the shape of a cylinder, a semi-cylindrical or an arc.
所述挤出机上的网孔板是单块的或者由多块拼合而成的。The mesh plate on the extruder is a single piece or assembled from multiple pieces.
本发明所述滚圆造粒机中离心转盘的转速为25~3000r/min,优选为50~1500r/min之间。The rotational speed of the centrifugal turntable in the spheronizer of the present invention is 25-3000r/min, preferably 50-1500r/min.
所述挤出机的挤出温度为10~50℃,优选为20~40℃。The extrusion temperature of the extruder is 10-50°C, preferably 20-40°C.
本发明由于采用挤出机和滚圆造粒机制造圆球形阴离子表面活性剂,故在表面活性剂制造和使用的全过程中可以实现无粉尘化,大大改善了劳动条件;本发明还具有产品成品率高,球形粒子强度适宜,不易粉化的特点;由于本发明挤出和滚圆步骤无需高温处理,且型速度快,故消除了表面活性剂热敏性物料的分解风险;本发明容易做到产品球径一致且大小可选;本发明的产品真球度高,表面光滑,不易搭桥和结块,流动性极好;本发明由于能实现优化的一致粒径和视密度,产品溶解性优于现有的其它同类固态产品。另外,本发明还可以对产品进行包衣处理,不仅能实现缓释的特殊目的,还能进一步提高防结块性,溶解性等性能。Because the present invention adopts extruder and tumbling granulator to manufacture spherical anionic surfactant, it can realize dust-free in the whole process of surfactant manufacture and use, greatly improving working conditions; the present invention also has finished product High efficiency, suitable spherical particle strength, not easy to pulverize; because the extrusion and spheronization steps of the present invention do not require high temperature treatment, and the forming speed is fast, the risk of decomposition of surfactant heat-sensitive materials is eliminated; the present invention is easy to achieve product spherical Consistent diameter and optional size; the product of the present invention has high true sphericity, smooth surface, is not easy to bridge and agglomerate, and has excellent fluidity; because the present invention can realize optimized consistent particle diameter and apparent density, the product solubility is better than existing There are other similar solid state products. In addition, the present invention can also carry out coating treatment on the product, which can not only realize the special purpose of sustained release, but also further improve performances such as anti-caking property and solubility.
本发明的造粒前的阴离子表面活性剂主料,可以采用直接来自磺化生产装置的具有超高活性物含量(活性物含量60%~80%)的阴离子表面活性剂主料;也可以是前述物料又经过预先干燥达到造粒所需含水量后的;还可以是干料。另外,还允许加入少量造粒干燥后筛分时筛余下来的碎粒。采用来自磺化生产装置的具有超高活性物含量(活性物含量60%~80%)的阴离子表面活性剂主料来造粒,其节能降耗的优势是不言而喻的。The anionic surfactant main material before granulation of the present invention can adopt the anionic surfactant main material directly from the sulfonation production unit with super high active matter content (active matter content 60%~80%); It can also be The aforementioned materials are pre-dried to reach the water content required for granulation; they can also be dry materials. In addition, it is also allowed to add a small amount of granules remaining after sieving after granulation and drying. The advantages of energy saving and consumption reduction are self-evident by adopting the anionic surfactant main material with ultra-high active matter content (active matter content 60% to 80%) from the sulfonation production plant for granulation.
本发明对阴离子表面活性剂主料预先干燥的形式没有特殊要求,可以是喷雾干燥、流化床造粒干燥、湍流加热闪蒸除湿等形式。The present invention has no special requirements on the form of pre-drying of the main material of the anionic surfactant, which may be in the form of spray drying, fluidized bed granulation drying, turbulent heating flash dehumidification and the like.
本发明所用的造粒辅料用量为造粒原料的0.5~30%(重量)。The dosage of the granulation auxiliary material used in the present invention is 0.5-30% (weight) of the granulation raw material.
本发明对阴离子表面活性剂主料与造粒辅料混合所用机械,没有特殊限定,螺旋式、耙式等均可。In the present invention, there is no special limitation on the machine used for mixing the main material of the anionic surfactant and the granulation auxiliary material, and the machine can be a screw type, a rake type, or the like.
本发明所用的挤出机主要功能部件是螺杆送料器、挤压筒和网孔板。其中:The main functional components of the extruder used in the present invention are a screw feeder, an extrusion cylinder and a mesh plate. in:
1.螺杆送料器是由单枝、双枝或更多枝螺杆组成的。常用的是单螺杆和双螺杆的挤出机。螺杆送料器是由电机驱动的,其转速可调,转速在10~150rpm之间;优选在25~100rpm之间。调速的方法可以是齿轮、皮带、蜗轮蜗杆等机械调速形式,更优选的是采用变频电机调速的形式,如此不仅可以方便地实现无级调速,还可以节约能耗;1. The screw feeder is composed of single, double or more screws. Commonly used are single-screw and twin-screw extruders. The screw feeder is driven by a motor, and its rotating speed is adjustable, and the rotating speed is between 10-150rpm; preferably between 25-100rpm. The method of speed regulation can be in the form of mechanical speed regulation such as gears, belts, worm gears, etc., and it is more preferable to adopt the form of variable frequency motor speed regulation, so that not only can conveniently realize stepless speed regulation, but also save energy consumption;
2.挤压筒内安装螺杆送料器,而网孔板则是装在挤压筒的一端的端面上,或者是包覆在挤压筒的外柱面上。装在挤压筒端面上的网孔板,采用的是平面或者是半球面形式的;而装在挤压筒外柱面上的网孔板是单块或是多块,形状为圆筒形、半圆筒形,或者是圆弧形的。网孔板上均匀分布着直径为优选为的圆孔;2. The screw feeder is installed in the extrusion barrel, and the mesh plate is installed on the end surface of one end of the extrusion barrel, or covered on the outer cylindrical surface of the extrusion barrel. The mesh plate installed on the end surface of the extrusion cylinder is in the form of a plane or hemispherical surface; while the mesh plate installed on the outer cylindrical surface of the extrusion cylinder is single or multi-piece, and the shape is cylindrical , semi-cylindrical, or arc-shaped. Evenly distributed on the mesh plate with a diameter of preferably round hole;
3.为了调节挤压温度,挤压筒上还可以装有夹套,通过流过夹套的介质,达到调节挤压温度的目的。3. In order to adjust the extrusion temperature, a jacket can also be installed on the extrusion cylinder, and the purpose of adjusting the extrusion temperature can be achieved by the medium flowing through the jacket.
本发明所用的造粒机主要功能部件是造粒筒体和离心转盘。造粒筒体为一圆筒并开口向上,上端开口处有筒盖;离心转盘安装在造粒筒体的下部,其上端面布满了破断齿。离心转盘是由电机驱动的,其转速可调,转速依据离心转盘的不同直径,可在25~3000r/min之间,最好在50~1500r/min之间。调速的方法可以是齿轮、皮带、蜗轮蜗杆等机械调速形式,更优选的是采用变频电机调速的形式,如此不仅可以方便地实现无级调速,还可以节约能耗。为了调节造粒温度,造粒筒上还可以装有夹套,通过流过夹套的介质,达到调节造粒温度的目的。The main functional components of the granulator used in the present invention are a granulation cylinder and a centrifugal turntable. The granulation cylinder is a cylinder with an opening upward, and there is a cylinder cover at the upper opening; the centrifugal turntable is installed at the lower part of the granulation cylinder, and its upper end is covered with broken teeth. The centrifugal turntable is driven by a motor, and its rotating speed is adjustable. The rotating speed can be between 25-3000r/min, preferably between 50-1500r/min according to the different diameters of the centrifugal turntable. The method of speed regulation can be in the form of mechanical speed regulation such as gears, belts, worm gears, etc. It is more preferable to adopt the form of frequency conversion motor speed regulation, which can not only realize stepless speed regulation conveniently, but also save energy consumption. In order to adjust the granulation temperature, a jacket can also be installed on the granulation cylinder, and the purpose of adjusting the granulation temperature can be achieved by the medium flowing through the jacket.
本发明对在造粒机中完成造粒后的球形物料,需要进一步进行干燥、冷却和定形。这里对干燥形式没有特殊要求,可以使用如流化干燥、真空干燥、带式干燥等形式的设备。In the present invention, the spherical material after granulation in the granulator needs to be further dried, cooled and shaped. There is no special requirement for the drying form, and equipment such as fluidized drying, vacuum drying, and belt drying can be used.
本发明对上述完成干燥、冷却和定形后的干料,可以再进行筛分,以除去极少量(≤5%重量)影响外观的碎粒。筛分后的产品即可进入料仓进行包装。筛分出来的碎粒混入造粒原料中回用。In the present invention, the dry material after drying, cooling and shaping can be further sieved to remove a very small amount (≤5% by weight) of broken particles that affect the appearance. The screened products can enter the silo for packaging. The sieved crumbs are mixed into the granulation raw materials for reuse.
本发明制造的球形阴离子表面活性剂,其颗粒直径可以在优选为的范围内,根据需要任意选择。The spherical anionic surfactant that the present invention makes, its particle diameter can be in preferably Within the range, you can choose arbitrarily according to your needs.
本发明的产品圆球形阴离子表面活性剂的堆密度在300~800g/l范围,而颗粒的视密度在600~1600g/l范围。The bulk density of the product spherical anionic surfactant of the present invention is in the range of 300-800g/l, and the apparent density of the particles is in the range of 600-1600g/l.
本发明制造的圆球形阴离子表面活性剂,如果需要具有缓释功能,或者希望进一步改善溶解性,或者需要提高其抗结块性,或者需要提高抗氧化性,或者需要掩盖不良气味时,可以选择合适的包衣材料对产品进行包衣处理。具体的方法是:先将造粒机的离心转盘换成具有粗糙端面的,再将干燥后的球形产品放入造粒机内,通过喷头将包衣材料定量均匀喷涂在球形产品的外表。包衣后可能仍需再次进行干燥处理。If the spherical anionic surfactant produced by the present invention needs to have a sustained release function, or it is desired to further improve solubility, or it needs to improve its anti-caking property, or it needs to improve its oxidation resistance, or it needs to cover up bad smell, you can choose Appropriate coating materials are used to coat the product. The specific method is: first replace the centrifugal disc of the granulator with a rough end surface, then put the dried spherical product into the granulator, and spray the coating material quantitatively and evenly on the surface of the spherical product through the nozzle. Drying may still be required after coating.
本发明制造的球形阴离子表面活性剂,主要用在民用、工业用清洗剂,建材发泡剂等产品配方中。如民用的牙膏、洗洁精、洗手液、洗衣粉(液)、沐浴露、香波等;工业用的各类清洗剂、功能性助剂等;建材行业的混凝土发泡剂、石膏板发泡剂等。尤其是,可以将其采用后配的形式应用于一般的,或浓缩的,甚至是超浓缩的洗衣粉中,可以提高活性物含量,减少洗衣粉的生产成本,还有利于保护环境。The spherical anionic surfactant manufactured by the present invention is mainly used in product formulas such as civil and industrial cleaning agents, foaming agents for building materials, and the like. Such as civilian toothpaste, detergent, hand sanitizer, washing powder (liquid), shower gel, shampoo, etc.; industrial cleaning agents, functional additives, etc.; concrete foaming agent and gypsum board foaming in the building materials industry agent etc. In particular, it can be applied to general, concentrated, or even super-concentrated washing powder in the form of post-mixing, which can increase the content of active substances, reduce the production cost of washing powder, and help protect the environment.
具体实施方式 Detailed ways
以下百分数除指明外,均为重量百分比。The following percentages are by weight unless otherwise indicated.
实施例1.Example 1.
(1).将136.5千克含水率为1.5%的烷基碳原子数为12~14的脂肪醇硫酸钠,1.5千克的甲基纤维素和12.5千克的水进行混合后,以300千克/小时的速度加入到双螺杆挤出机中,设定螺杆转速为100r/min,挤出温度30℃,物料从网孔直径为按径向分布的网孔板中,挤出成圆条状湿料。持续30分钟后,得到150千克的圆条状湿料。(1). After 136.5 kilograms of fatty alcohol sodium sulfate with 1.5% alkyl carbon number of 1.5% are mixed, 1.5 kilograms of methyl cellulose and 12.5 kilograms of water are mixed, and 300 kilograms/hour The speed is added to the twin-screw extruder, the screw speed is set to 100r/min, the extrusion temperature is 30°C, and the material is fed from the mesh with a diameter of The wet material is extruded into round strips in the radially distributed mesh plate. After continuing for 30 minutes, 150 kg of round strip-shaped wet material was obtained.
(2).将上述圆条状物料,按每批30千克加入到滚圆造粒机中,设定离心转盘转速为400rpm,滚动造粒120秒钟后,得到30千克圆球形状湿料。共进行5批次后,共得到150千克的圆球形状湿料。(2). Add 30 kg of the above-mentioned round strip materials to the spheronizer in batches, set the rotating speed of the centrifugal turntable to 400 rpm, and roll and granulate for 120 seconds to obtain 30 kg of spherical wet material. After carrying out 5 batches altogether, obtain the spherical shape wet material of 150 kilograms altogether.
(3).将150千克的圆球形状湿料,按300千克/小时的速度送入流化床干燥设备中,经过120分钟的干燥、冷却后,得到137千克含水率为0.8%,堆密度为329g/l的干料。(3). Send 150 kilograms of spherical wet materials into the fluidized bed drying equipment at a speed of 300 kilograms per hour. After 120 minutes of drying and cooling, 137 kilograms of wet materials with a moisture content of 0.8% and a bulk density of 137 kilograms are obtained. It is 329g/l dry material.
(4).将上述136千克干料进行筛分后,得到134千克,合格的圆球形脂肪醇硫酸钠阴离子表面活性剂。(4). After sieving the above 136 kg of dry material, 134 kg was obtained, qualified Spherical fatty alcohol sodium sulfate anionic surfactant.
(5).将筛下的碎粒回掺到造粒原料中。(5). Mix the crumbs under the sieve back into the granulation raw materials.
实施例2.Example 2.
(1).将142千克含水率为15%的烷基碳原子数为16~18的脂肪醇硫酸钠,7.5千克无水硫酸钠和0.75千克的羟丙基甲基纤维素进行混合后,以300千克/小时的速度加入到双螺杆挤出机中,设定螺杆转速为50r/min,挤出温度30℃,物料从网孔直径为按径向分布的网孔板中,挤出成圆条状湿料。持续30分钟后,得到150千克的圆条状湿料。。(1). After 142 kilograms of fatty alcohol sodium sulfate with 15% alkyl carbon number of 16~18 moisture content, 7.5 kilograms of anhydrous sodium sulfate and 0.75 kilogram of hydroxypropyl methyl cellulose are mixed, with The speed of 300 kg/hour is added to the twin-screw extruder, the screw speed is set to 50r/min, the extrusion temperature is 30°C, and the material is fed from the mesh with a diameter of The wet material is extruded into round strips in the radially distributed mesh plate. After continuing for 30 minutes, 150 kg of round strip-shaped wet material was obtained. .
(2).将挤压出来的圆条状物料,按每批30千克加入到滚圆造粒机中,设定温度20℃,离心转盘转速为600rpm,滚动造粒90秒钟,得到一批圆球形状湿料30千克。进行5批次投料后,得到150千克的圆球形状湿料。(2). Put the extruded round strip material into the spheronizer according to each batch of 30 kg, set the temperature at 20°C, and the rotating speed of the centrifugal turntable at 600rpm, and roll and granulate for 90 seconds to obtain a batch of spheronizers. 30 kg of spherical wet material. After carrying out 5 batches of feeding, obtain 150 kilograms of spherical shape wet material.
(3).将150千克的圆球形状湿料,按300千克/小时的速度送入流化床干燥设备中,圆球形状湿料经过干燥、吹冷等程序后出料。60分钟后,得到134千克含水率为2%,颗粒视密度为1567g/l的干料。(3). Send 150 kg of spherical wet material into the fluidized bed drying equipment at a speed of 300 kg/hour. The spherical wet material is discharged after drying, blowing and cooling. After 60 minutes, 134 kg of dry material with a moisture content of 2% and an apparent particle density of 1567 g/l were obtained.
(4).将上述134千克干料进行筛分后,得到132千克合格的圆球形脂肪醇硫酸钠阴离子表面活性剂。(4). After sieving the above-mentioned 134 kilograms of dry materials, 132 kilograms of qualified Spherical fatty alcohol sodium sulfate anionic surfactant.
(5).将筛下的碎粒回掺到造粒原料中。(5). Mix the crumbs under the sieve back into the granulation raw materials.
实施例3.Example 3.
(1).将10.75千克含水率为5%的烯基碳原子数为18~24的α-烯基磺酸盐,3.5千克对甲苯磺酸钠和0.75千克乙醇,混合均匀后,以10千克/小时的速度,将其加入到单螺杆挤出机中,设定螺杆转速为15r/min,挤出温度100℃,物料从网孔直径为,按径向分布的网孔板中挤出成圆条状湿料。持续30分钟后,得到15千克的圆条状湿料。(1). 10.75 kilograms of α-alkenyl sulfonate with a water content of 5% and 18 to 24 alkenyl carbon atoms, 3.5 kilograms of sodium p-toluenesulfonate and 0.75 kilograms of ethanol are mixed uniformly and mixed with 10 kilograms The speed per hour is added to the single-screw extruder, the screw speed is set to be 15r/min, the extrusion temperature is 100°C, and the material from the mesh diameter is , and extrude into a round bar-shaped wet material according to the radial distribution of the mesh plate. After continuing for 30 minutes, 15 kg of round strip-shaped wet material was obtained.
(2).将挤压出来的圆条状物料,按每批0.5千克加入到滚圆造粒机中,设定温度20℃,离心转盘转速为3000rpm,滚动造粒30秒钟,得到一批圆球形状湿料0.5千克。共进行30批投料,得到15千克的圆球形状湿料。(2). Put the extruded round strip material into the spheronizer according to 0.5 kg per batch, set the temperature at 20°C, rotate the centrifugal disc at 3000rpm, roll and granulate for 30 seconds, and obtain a batch of spheronizers. 0.5 kg of spherical wet material. Carry out 30 batches of feeding altogether, obtain 15 kilograms of spherical shape wet materials.
(3).将15千克的圆球形状湿料,按每批3千克,持续120分钟/批的速度在流化床干燥设备中干燥5批后,得到13千克含水率为1.5%,堆密度为615g/l的干料。(3). With 15 kilograms of spherical wet materials, 3 kilograms per batch, after drying 5 batches in the fluidized bed drying equipment at a speed of 120 minutes/batch, 13 kilograms of moisture content is 1.5%, and the bulk density is obtained. It is 615g/l dry material.
(4).将上述13千克干料进行筛分后,得到12千克合格的圆球形α-烯基磺酸盐阴离子表面活性剂。(4). After sieving the above-mentioned 13 kilograms of dry materials, 12 kilograms of qualified Spherical α-olefin sulfonate anionic surfactant.
(5).将筛下的碎粒回掺到造粒原料中。(5). Mix the crumbs under the sieve back into the granulation raw materials.
实施例4.Example 4.
(1).将149.25千克含水率为10%的烯基碳原子数为14~16的α-烯基磺酸盐,0.75千克的羟丙基甲基纤维素混合均匀后,以300千克/小时的速度,将其加入到双螺杆挤出机中,设定螺杆转速为80r/min,挤出温度40℃,物料从网孔直径为,按径向分布的网孔板中挤出成圆条状湿料。持续30分钟后,得到150千克的圆条状湿料。(1). After mixing 149.25 kilograms of 149.25 kilograms of alkenyl carbon atoms with 14 to 16 alkenyl carbon atoms and 0.75 kilograms of hydroxypropyl methylcellulose evenly, at 300 kilograms/hour The speed is added to the twin-screw extruder, the screw speed is set to 80r/min, the extrusion temperature is 40°C, and the material is fed from the mesh with a diameter of , and extrude into a round bar-shaped wet material according to the radial distribution of the mesh plate. After continuing for 30 minutes, 150 kg of round strip-shaped wet material was obtained.
(2).将挤压出来的圆条状物料,按每批30千克加入到滚圆造粒机中,设定温度20℃,离心转盘转速为300rpm,滚动造粒30秒钟,得到一批圆球形状湿料30千克。共进行5批投料,得到150千克的圆球形状湿料。(2). Put the extruded round strip material into the spheronizer according to each batch of 30 kg, set the temperature at 20°C, and the rotating speed of the centrifugal turntable at 300rpm, and roll and granulate for 30 seconds to obtain a batch of spheronizers. 30 kg of spherical wet material. Carry out 5 batches of feed intake altogether, obtain the spherical shape wet material of 150 kilograms.
(3).将150千克的圆球形状湿料,按300千克/小时的速度送入连续式流化床干燥设备中,60分钟后,得到147千克含水率为2%,颗粒视密度为1167g/l的干料。(3). Send 150 kilograms of spherical wet material into the continuous fluidized bed drying equipment at a speed of 300 kilograms per hour. After 60 minutes, 147 kilograms are obtained with a moisture content of 2% and an apparent particle density of 1167g. /l dry material.
(4).将上述147千克干料进行筛分后,得到145千克合格的圆球形脂肪酸甲酯磺酸钠阴离子表面活性剂。(4). After sieving the above-mentioned 147 kilograms of dry materials, 145 kilograms of qualified Spherical sodium fatty acid methyl ester sulfonate anionic surfactant.
(5).将筛下的碎粒回掺到造粒原料中。(5). Mix the crumbs under the sieve back into the granulation raw materials.
实施例5.Example 5.
(1).将135千克含水率为4%的烷基碳原子数为16~18的脂肪酸甲酯磺酸钠,15千克水混合均匀后,以300千克/小时的速度,将其加入到双螺杆挤出机中,设定螺杆转速为120r/min,挤出温度80℃,物料从网孔直径为,按径向分布的网孔板中挤出成圆条状湿料。持续30分钟后,得到150千克的圆条状湿料。(1). After 135 kilograms of sodium fatty acid methyl ester sulfonate with a water content of 4% and 16 to 18 alkyl carbon atoms, 15 kilograms of water are mixed uniformly, with a speed of 300 kilograms/hour, it is added to the biscuit In the screw extruder, the screw speed is set to 120r/min, the extrusion temperature is 80°C, and the material from the mesh diameter is , and extrude into a round bar-shaped wet material according to the radial distribution of the mesh plate. After continuing for 30 minutes, 150 kg of round strip-shaped wet material was obtained.
(2).将挤压出来的圆条状物料,按每批30千克加入到滚圆造粒机中,设定温度20℃,离心转盘转速为500rpm,滚动造粒30秒钟,得到一批圆球形状湿料30千克。共进行5批投料,得到150千克的圆球形状湿料。(2). Put the extruded round strip material into the spheronizer according to each batch of 30 kg, set the temperature at 20°C, and rotate the centrifugal disc at 500rpm, and roll and granulate for 30 seconds to obtain a batch of spheronizers. 30 kg of spherical wet material. Carry out 5 batches of feed intake altogether, obtain the spherical shape wet material of 150 kilograms.
(3).将150千克的圆球形状湿料,按300千克/小时的速度送入连续式流化床干燥设备中,90分钟后,得到143千克含水率为4.5%,堆密度为767g/l的干料。(3). 150 kilograms of spherical shape wet materials are sent into the continuous fluidized bed drying equipment at a speed of 300 kilograms per hour. After 90 minutes, 143 kilograms of wet materials are obtained with a moisture content of 4.5%, and a bulk density of 767g/hour. l dry material.
(4).将上述143千克干料进行筛分后,得到140千克,合格的圆球形脂肪酸甲酯磺酸钠阴离子表面活性剂。(4). After sieving the above 143 kg of dry material, 140 kg is obtained, qualified Spherical sodium fatty acid methyl ester sulfonate anionic surfactant.
(5).将筛下的碎粒回掺到造粒原料中。(5). Mix the crumbs under the sieve back into the granulation raw materials.
实施例6.Example 6.
(1).将111.5千克含水率为3%的烷基碳原子数为8~14的脂肪醇硫酸钠,37千克含水率为25%的烷基碳原子数为12~14的脂肪醇醚硫酸盐,1.5千克的水混合均匀后,以300千克/小时的速度,将其加入到双螺杆挤出机中,设定螺杆转速为75r/min,挤出温度30℃,物料从网孔直径为按径向分布的网孔板中挤出成圆条状湿料。持续30分钟后,得到150千克的圆条状湿料。(1). 111.5 kilograms of fatty alcohol sodium sulfate with 3% alkyl carbon atoms and 12 to 14 fatty alcohol ether sulfuric acid with 25% alkyl carbon atoms in 37 kilograms of water content After mixing salt and 1.5 kg of water evenly, add it into the twin-screw extruder at a speed of 300 kg/hour, set the screw speed to 75r/min, extrude at 30°C, and feed the material from the mesh with a diameter of The wet material is extruded into round strips from the radially distributed mesh plate. After continuing for 30 minutes, 150 kg of round strip-shaped wet material was obtained.
(2).将挤压出来的圆条状物料,按每批30千克加入到滚圆造粒机中,设定温度30℃,离心转盘转速为1000rpm,滚动造粒30秒钟,得到一批圆球形状湿料30千克。共进行5批投料,最终得到150千克的圆球形状湿料。(2). Put the extruded round strip material into the spheronizer according to each batch of 30 kg, set the temperature at 30°C, rotate the centrifugal disc at 1000rpm, roll and granulate for 30 seconds, and obtain a batch of spheronizers. 30 kg of spherical wet material. Carry out 5 batches of feeding altogether, finally obtain 150 kilograms of spherical shape wet materials.
(3).将150千克的圆球形状湿料,按300千克/小时的速度送入连续式流化床干燥设备中,30分钟后,得到140千克含水率为3%,堆密度为463g/l,颗粒视密度为625g/l的干料。(3). 150 kilograms of spherical shape wet materials are sent into the continuous fluidized bed drying equipment at a speed of 300 kilograms per hour. After 30 minutes, 140 kilograms of wet materials are obtained with a moisture content of 3% and a bulk density of 463g/hour. l, dry material with a particle apparent density of 625g/l.
(4).将上述140千克干料进行筛分后,得到139千克,合格的圆球形脂肪醇硫酸钠和脂肪醇醚磺酸钠的混合物阴离子表面活性剂。(4). After sieving the above 140 kilograms of dry material, 139 kilograms were obtained, qualified A mixture of spherical fatty alcohol sodium sulfate and fatty alcohol ether sodium sulfonate anionic surfactant.
(5).筛下的碎粒和细粉回用。(5). The crumbs and fine powder under the sieve are reused.
实施例7.Example 7.
紧接实施例1之(4)步骤后,将滚圆造粒机中的离心转盘换成粗糙的没有破断齿的盘,称取30千克合格的圆球形脂肪醇硫酸钠,将其放入滚圆造粒机中,设定温度30℃,离心转盘转速为500rpm,在10秒钟时间里,从喷雾嘴向滚圆造粒机中的圆球形脂肪醇硫酸钠,匀速喷入羟丙甲纤维素包衣液0.3千克,再滚动20秒钟后出料,得到30千克外层有包衣的脂肪醇硫酸钠。Immediately after the (4) step of Example 1, the centrifugal disc in the spheronizer is replaced with a rough disk without broken teeth, and 30 kilograms of qualified spherical fatty alcohol sodium sulfate is weighed, and it is put into the spheronizer. In the granulator, set the temperature at 30°C, and the rotational speed of the centrifugal disc at 500rpm. Within 10 seconds, spray the hypromellose coating at a uniform speed from the spray nozzle to the spherical fatty alcohol sodium sulfate in the spheronizer. 0.3 kilogram of liquid, and then roll out after 20 seconds, obtain 30 kilograms of outer layers and have the fatty alcohol sodium sulfate of coating.
实施例8.Example 8.
紧接实施例1之(4)步骤后,将滚圆造粒机中的离心转盘换成粗糙的没有破断齿的盘,称取30千克合格的圆球形脂肪醇硫酸钠阴离子表面活性剂,将其放入滚圆造粒机中,设定温度30℃,离心转盘转速为500rpm,在10秒钟时间里,从喷雾嘴向滚圆造粒机中的圆球形脂肪醇硫酸钠阴离子表面活性剂匀速喷入阿拉伯树胶包衣液0.65千克,而后滚动20秒钟后出料,得到31千克外层有包衣的脂肪醇硫酸钠。Immediately after the (4) step of embodiment 1, the centrifugal rotating disk in the spheronizer is changed into a rough dish without broken teeth, and 30 kilograms of qualified spherical fatty alcohol sodium sulfate anionic surfactants are weighed, and its Put it into the spheronizer, set the temperature at 30°C, and the rotating speed of the centrifugal turntable is 500rpm. Within 10 seconds, spray the spherical fatty alcohol sodium sulfate anionic surfactant from the spray nozzle to the spheronizer at a uniform speed. 0.65 kilogram of gum arabic coating liquid, then discharge after rolling 20 seconds, obtain 31 kilograms of outer layers and have the fatty alcohol sodium sulfate of coating.
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WO2012048947A1 (en) | 2010-10-14 | 2012-04-19 | Unilever Plc | Laundry detergent particles |
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