CN1834214A - Process of continuous drying surfactant esp drying aliphatic acid methyl ester sulfsalte - Google Patents

Process of continuous drying surfactant esp drying aliphatic acid methyl ester sulfsalte Download PDF

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Publication number
CN1834214A
CN1834214A CN 200610057171 CN200610057171A CN1834214A CN 1834214 A CN1834214 A CN 1834214A CN 200610057171 CN200610057171 CN 200610057171 CN 200610057171 A CN200610057171 A CN 200610057171A CN 1834214 A CN1834214 A CN 1834214A
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tensio
active agent
drying
fluidized bed
additive
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CN100500819C (en
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黄亚茹
方银军
邹欢金
葛赞
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Praise Technology Group Limited by Share Ltd
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Zancheng Science & Technology Co Ltd Zhejiang Prov
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Abstract

This invention discloses a continuous drying surfactant, especially for drying fatty acid methyl ester sulfonate. The surfactant is manufactured by: (1) introducing surfactant into a vacuum heat-conductive stirring drier of 90-160 deg.C for deoxygenating and desolventing, (2) passing through a screw conveyer into a twin-screw extruder with additive for homogenizing, dehydrating, expanding and adjusting, (3) drying at 50-160 deg.C and 3-8 MPa, (4) cooling, aging and molding in a vibrational fluidized bed (the temperature of the cooling wind is 0-35 deg.C), and (5) packaging in a feed bin. The surfactant in this invention has such advantages as good water solubility, high surface area, rapid dissolution, good fluidity and even distribution of each component. Moreover, according to different client requirements, surfactants with different densities can be manufactured.

Description

A kind of successive drying tensio-active agent, the particularly method of drying fatty acid methyl ester sulfonate
One, technical field
The present invention relates to a kind of method of successive drying tensio-active agent, more particularly relate to a kind of drying fatty acid methyl ester sulfonate, make it become bulk sheet or granular method.
Two, background technology
Green, the environmental protection tensio-active agent of the excellent property that to be raw material with the animal-plant oil make through technologies such as hydrogenation, transesterify, sulfonation, bleaching, neutralization and dryings that fatty acid methyl ester sulfonate (be called for short MES) is are mainly used in fields such as articles for washing.MES is in removing the drying process of solvent, material has experienced by lotion, high viscosity fluid, the phase change of Zhongdao flow solids particulate three phases, existing drying process, as turbulent flow drying etc., the product density that makes is big, be difficult for dispersing and dissolving in water, and will in articles for washing, add, need have good water-soluble, particularly be added in the powder washing composition outstanding apparent important.
The method and apparatus patent that many desiccated surface promoting agents are arranged in the prior art.As U.S. Pat-the 5723433rd, remove solvent in the tensio-active agent with the tubular type steam seasoning.Japanese Patent WO2004/111166 is injected to slip liquid in the reduction vaporization jar, and is sent to wall by the centrifugal force of paddle and forces to carry out filming and material is concentrated, and pulverizes the flash distillation film drying technology of granulation afterwards again.Chinese patent CN-1111710C discloses a kind of spraying drying tower process.But all there is big, the easy stamping device of remollescent material of energy consumption in above method, and makes operate continuously be difficult to keep, or the uneven shortcoming of dry materials is arranged, and the product of dry gained dissolve in water and needs higher temperature and time of length.And owing to be added with inflammable, explosive solvent in the MES production technique, also there is bigger fire and explosive risks in spraying drying.
Three, summary of the invention
One of purpose of the present invention provides a kind of method of successive drying tensio-active agent.
Two of purpose of the present invention provides a kind of method of successive drying fatty acid methyl ester sulfonate.
Three of purpose of the present invention provides a kind of method of successive drying alkenyl sulphonate.
This and other purpose of the present invention will and be described and further set forth by following detailed description.
In the method for successive drying tensio-active agent of the present invention, with being sent to the heating medium temperature after the tensio-active agent metering is deoxidation in 90 ℃~160 ℃ the vacuum thermal conduction formula stirring drier, desolventizing, send into homogeneous in the twin-screw extruder together through screw rod conveyor and additive then, dehydration, expanded and adjust, high pressure (pressure is to increase gradually from 3-8 in the process) and heating medium temperature at 3MPa~8MPa is 50 ℃~160 times dryings simultaneously, adjusted material is through vibration fluidized bed cooling, wear out and typing, vibration fluidized bed cooling air temperature is 0 ℃~35 ℃, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.
In the method for successive drying tensio-active agent of the present invention, described additive can be yellow soda ash, sodium bicarbonate, Trisodium Citrate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, sodium hydrogen phosphate, Sulfothiorine, sodium sulfate, S-WAT, sodium bisulfite, sugar or starch, can be used alone, also can use their mixture.The addition of described additive is 3%~30% of a tensio-active agent total amount, is preferably, and the addition of additive is 5%~15% of a tensio-active agent total amount.
In the method for successive drying tensio-active agent of the present invention, described tensio-active agent is in the tensio-active agent production process, the material that contains volatile solvent such as methyl alcohol, ethanol, water, hydrogen peroxide etc. after the neutralization.In described vacuum thermal conduction formula stirring drier, the needed heat of drying process is all provided by heat transfer wall, and heating medium does not directly contact with material, need not use and carry air.
The method of drying fatty acid methyl ester sulfonate of the present invention, to contain methyl alcohol 0%~40%, the MES product of water about 10%~50, be input to the heating medium temperature and be in 90 ℃~160 ℃ the vacuum thermal conduction formula stirring drier, after tentatively removing solvent, with 3%~30% additive, be input to homogeneous in the twin-screw extruder, dehydration, expanded and adjust, high pressure (pressure is to increase gradually in the process) and heating medium temperature at 3MPa~8MPa is 50 ℃~160 ℃ dryings down simultaneously, enter vibration fluidized bed aging typing again, vibration fluidized bed cooling air temperature is 0 ℃~35 ℃, material temperature is plummeted to the following aging moulding of zero pour, packs out finished product at last.
The method of dry alkenyl sulphonate of the present invention, be to be that to be 20%~30% olefin sulfonic acid salt sludge join in the twin-screw extruder with 3%~30% additive for 25 ℃~50 ℃, water content with temperature, high pressure and heating medium temperature at 3MPa~8MPa are 90 ℃~180 ℃ dryings down, enter vibration fluidized bed aging typing again, vibration fluidized bed cooling air temperature is 0 ℃~35 ℃, pack out at last finished product, product moisture 3%.
In the method for successive drying fatty acid methyl ester sulfonate of the present invention or dry alkenyl sulphonate, described additive can be yellow soda ash, sodium bicarbonate, Trisodium Citrate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, sodium hydrogen phosphate, Sulfothiorine, sodium sulfate, S-WAT, sodium bisulfite, sugar or starch, can be used alone, also can use their mixture, the addition of described additive is 3%~30% of a tensio-active agent total amount, be preferably, the addition of additive is 5%~15% of a tensio-active agent total amount.
In the present invention, with in tensio-active agent (particularly MES) production process, the material that contains volatile solvent (as methyl alcohol, ethanol, water, hydrogen peroxide etc.) after the neutralization, earlier after vacuum thermal conduction formula stirring drier removes the solvent of a certain amount of (as total amount 20%~30%), with additive, be input in the twin-screw extruder, finish homogeneous, dehydration and expanded, then through fluidized-bed cooling, aging and typing, mould when the shape of dried material depends on extrusion molding, can be flaky, also can be granular or corynebacterium.The adding additive is for the density of adjusting product and pH value etc., if there is not inflammable, explosive solvent in the material, also can directly carry out drying at twin-screw extruder without vacuum thermal conduction formula stirring drier.
The vacuum thermal conduction formula stirring drier and the twin-screw extruder of Shi Yonging all has from descaling function in the present invention, can guarantee continuous production.
The product that makes with method of the present invention can solve water-soluble problem, and has huge surface-area, and dispersing and dissolving is rapid, and local too high levels or low excessively phenomenon can not appear in good fluidity, and each component uniform distribution in the prescription.Can also produce simultaneously the product of various different densities according to client's needs.
Four, description of drawings
The drying installation synoptic diagram of Fig. 1 for using in the method for successive drying tensio-active agent of the present invention.
Fig. 2 is the process flow sheet of successive drying MES method of the present invention.
Fig. 3 is the process flow sheet of successive drying AOS method of the present invention.
In Fig. 1, material enters vacuum thermal conduction formula stirring drier 1 drying, and the needed heat of drying process is all provided by heat transfer wall, and heating medium does not directly contact with material, need not use and carry air, compare with transmission of heat by convection formula moisture eliminator, the thermo-efficiency height can reclaim the solvent that evaporates in the drying process, secluding air, can control the diffusion of explosive material effectively, prevent from that explosive material from contacting with air to cause fire failure, satisfy environmental protection requirement simultaneously.Enter in the twin-screw extruder by screw rod conveyor 2.In the material of AOS, do not need recovered solvent, can directly enter next step drying process.
In twin-screw extruder 3, with conveying, pulverizing, mixing, shearing, fusion, supercharging with a series of unit operation such as extrude, on twin screw, carry out simultaneously, one step finished, a series of production lines of forming by many chemical equipments have been replaced with a machine equipment, replacing batch production with continuous production, is a kind of mechanical means that saves time, economizes ground, high-level efficiency, less energy-consumption.Material places under the high pressure conditions of extrusion machine, be subjected to the pushing effect of screw rod and the reverse retardation of throttling set simultaneously in inner barrel, thermal source comprises indirect heating and contacts screw rod, the heat of friction that cylindrical shell etc. produce, add the chemical heat release of additive etc., material is under the temperature of the high pressure of 3Mpa~8MPa and 100 ℃~160 ℃, this pressure has surpassed the saturated vapor pressure under the extrusion temperature, moisture etc. can explosive evaporatoin, under this temperature, material presents molten state, material is extruded once the mould mouth, pressure reduces suddenly, and moisture sharply evaporates, and product expands thereupon.In vibration fluidized bed 4 cooling air, material temperature is plummeted to the following aging moulding of zero pour.Additive helps the foaming and the steady bubble of material, reach the product that the slip surface-area that makes unit weight increases and then obtain having desired density, variation has taken place in the material internal structure in the puffing process, and it is easy to use that product is finally had, the fast characteristics of dissolving in the water.
From vibration fluidized bed 4 air-flows that come out, behind cyclonic separator 5 separation of material, enter sack cleaner 6, wet cleaner 7, qualified discharge after the dedusting.Cooling air is provided by cold blast engine 8, cold blast engine 9.Aging typing back material is stored in feed bin 10 in short-term, is finished product after the packing.
All raw material of Shi Yonging and equipment etc. all are conventional uses in the present invention, can buy from market.In the present invention, refer in particular to as non-, all amount, per-cents are weight unit.
Below in conjunction with embodiment the present invention is carried out concrete description.As known by the technical knowledge, the present invention can realize by other the embodiment that does not break away from its spirit or essential feature.Therefore, following embodiment with regard to each side, all just illustrates, and is not only.All within the scope of the present invention or the change that is equal in the scope of the present invention all be included in the invention.
Five, embodiment
Embodiment 1
With fatty acid methyl ester sulfonate (methanol content 7% before dry, water-content 25% before dry) being sent to the heating medium temperature after the metering is deoxidation in 110 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (0.3% S-WAT then, 1.5% yellow soda ash and 2.2% sodium sulfate, starch 5%) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa (pressure increases gradually in the process) is 140 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 10 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.6% in the product, and methanol content is less than 0.04%, product density 46g/100ml.
Embodiment 2
With fatty acid methyl ester sulfonate (methanol content 10% before dry, water-content 25% before dry) being sent to the heating medium temperature after the metering is deoxidation in 130 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (1.0% sodium bicarbonate then, 1.5% Trisodium Citrate, 4% starch, 0.5% sodium sulfate) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 130 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 10 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.7% in the product, and methanol content is less than 0.04%, product density 48g/100ml.
Embodiment 3
With fatty acid methyl ester sulfonate (methanol content 13% before dry, water-content 25% before dry) being sent to the heating medium temperature after the metering is deoxidation in 140 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (0.2% S-WAT then, 2.0% sodium bicarbonate, 8.0% sodium sulfate) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 120 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 10 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.8% in the product, and methanol content is less than 0.04%, product density 58g/100ml.
Embodiment 4
With fatty acid methyl ester sulfonate (methanol content 16% before dry, water-content 16% before dry) being sent to the heating medium temperature after the metering is deoxidation in 120 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (1.5% sodium phosphate then, 2.5% SODIUM PHOSPHATE, MONOBASIC, 2.0% sodium sulfate, 15% starch) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 150 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 20 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.5% in the product, and methanol content is less than 0.04%, product density 53g/100ml.
Embodiment 5
With fatty acid methyl ester sulfonate (methanol content 25% before dry, water-content 16% before dry) being sent to the heating medium temperature after the metering is deoxidation in 130 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (0.2% Sulfothiorine then, 1.5% Trisodium Citrate, 3.5% sodium sulfate) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 100 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 20 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.5% in the product, and methanol content is less than 0.04%, product density 60g/100ml.。
Embodiment 6
With fatty acid methyl ester sulfonate (methanol content 32% before dry, water-content 16% before dry) being sent to the heating medium temperature after the metering is deoxidation in 150 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (1.5% yellow soda ash then, 3.5% Trisodium Citrate, 1.5% sodium sulfate, 3.5% starch) send into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 140 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 20 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.6% in the product, and methanol content is less than 0.04%, product density 42g/100ml.
Embodiment 7
With fatty acid methyl ester sulfonate (methanol content 40% before dry, water-content 16% before dry) being sent to the heating medium temperature after the metering is deoxidation in 160 ℃ the vacuum thermal conduction formula stirring drier 1, desolventizing, pass through screw rod conveyor and additive (5.0% yellow soda ash then, 1.5% sodium sulfate, 3.5% white sugar) sends into homogeneous in the twin-screw extruder 3 together, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 90 ℃ of dryings down simultaneously, adjusted material is through vibration fluidized bed 4 coolings, wear out and typing, vibration fluidized bed cooling air temperature is 25 ℃, material temperature is plummeted to the following aging moulding of zero pour, enters the feed bin packing at last.From the vibration fluidized bed air-flow that comes out, behind the cyclonic separator separation of material, enter sack cleaner, wet cleaner 7, qualified discharge after the dedusting.Water-content 1.6% in the product, and methanol content is less than 0.04%, product density 40g/100ml.
Embodiment 8
Adopt alkenyl sulphonate (being called for short AOS) slurry, about 40 ℃ of temperature, moisture about 27%, enter in the twin-screw extruder 3, add (1.5% S-WAT and 2.0% sodium sulfate) additive, high pressure and heating medium temperature at 3MPa~8MPa are 150 ℃ of dryings down, and vibration fluidized bed 4 cooling air temperature is 30 ℃.Product is moisture 3%, and methanol content is less than 0.04%, product density 45g/100ml.

Claims (10)

1, a kind of method of successive drying tensio-active agent, it is characterized in that with being sent to the heating medium temperature after the tensio-active agent metering be deoxidation in 90 ℃~160 ℃ the vacuum thermal conduction formula stirring drier, desolventizing, send into homogeneous in the twin-screw extruder together through screw rod conveyor and additive then, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 50 ℃~160 ℃ dryings down simultaneously, adjusted material is through vibration fluidized bed cooling, wear out and typing, vibration fluidized bed cooling air temperature is 0~35 ℃, enters the feed bin packing at last.
2, the method for successive drying tensio-active agent according to claim 1, it is characterized in that described additive can be yellow soda ash, sodium bicarbonate, Trisodium Citrate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, sodium hydrogen phosphate, Sulfothiorine, sodium sulfate, S-WAT, sodium bisulfite, sugar or starch, can be used alone, also can use their mixture.
3, the method for successive drying tensio-active agent according to claim 3, the addition that it is characterized in that described additive is 3%~30% of a tensio-active agent total amount.
4, the method for successive drying tensio-active agent according to claim 4, the addition that it is characterized in that described additive is 5%~15% of a tensio-active agent total amount.
5,, it is characterized in that described tensio-active agent is in the tensio-active agent production process, the material that contains volatile solvent such as methyl alcohol, ethanol, water, hydrogen peroxide etc. after the neutralization according to the method for the described successive drying tensio-active agent of one of claim 1-4.
6, according to the method for the described successive drying tensio-active agent of one of claim 1-5, it is characterized in that in described vacuum thermal conduction formula stirring drier, the needed heat of drying process is all provided by heat transfer wall, and heating medium does not directly contact with material, need not use and carry air.
7, a kind of method of drying fatty acid methyl ester sulfonate, it is characterized in that to contain methyl alcohol 0~40%, the MES product of water about 10~50%, be input to the heating medium temperature and be in 90 ℃~160 ℃ the vacuum thermal conduction formula stirring drier, after tentatively removing solvent, with 3%~30% additive, be input to homogeneous in the twin-screw extruder, dehydration, expanded and adjust, high pressure and heating medium temperature at 3MPa~8MPa is 50 ℃~160 ℃ dryings down simultaneously, enter vibration fluidized bed aging typing again, vibration fluidized bed cooling air temperature is 0 ℃~35 ℃, and material temperature is plummeted to the following aging moulding of zero pour, packs out finished product at last.
8, a kind of method of dry alkenyl sulphonate, it is characterized in that with temperature being that to be 20%~30% olefin sulfonic acid salt sludge join in the twin-screw extruder with 3%~30% additive for 25 ℃~50 ℃, water content, high pressure and heating medium temperature at 3MPa~8MPa are 90 ℃~180 ℃ dryings down, enter vibration fluidized bed aging typing again, vibration fluidized bed cooling air temperature is 0 ℃~35 ℃, pack out at last finished product, product moisture 3%.
9, according to Claim 8 or 9 described drying meanss, it is characterized in that described additive can be yellow soda ash, sodium bicarbonate, Trisodium Citrate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, sodium hydrogen phosphate, Sulfothiorine, sodium sulfate, S-WAT, sodium bisulfite, sugar or starch, can be used alone, also can use their mixture, addition is 3%~30% of a tensio-active agent total amount.
10, according to Claim 8 or 9 described drying meanss, it is characterized in that described addition is 5%~15% of a tensio-active agent total amount.
CNB2006100571713A 2006-03-13 2006-03-13 Process of continuous drying for aliphatic acid methyl ester sulfsalte Expired - Fee Related CN100500819C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102277238A (en) * 2011-07-13 2011-12-14 杭州迪康生物技术有限公司 Granular fatty acid methyl ester sulfonate (MES)-containing composite
CN107253924A (en) * 2017-06-09 2017-10-17 常州大学 A kind of preparation method of MES pulvis surfactant

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102277238A (en) * 2011-07-13 2011-12-14 杭州迪康生物技术有限公司 Granular fatty acid methyl ester sulfonate (MES)-containing composite
CN102277238B (en) * 2011-07-13 2012-10-03 杭州迪康生物技术有限公司 Granular fatty acid methyl ester sulfonate (MES)-containing composite
CN107253924A (en) * 2017-06-09 2017-10-17 常州大学 A kind of preparation method of MES pulvis surfactant
CN107253924B (en) * 2017-06-09 2019-11-12 常州大学 A kind of preparation method of MES pulvis surfactant

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