CN105254542A - Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation - Google Patents
Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation Download PDFInfo
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- CN105254542A CN105254542A CN201510726853.8A CN201510726853A CN105254542A CN 105254542 A CN105254542 A CN 105254542A CN 201510726853 A CN201510726853 A CN 201510726853A CN 105254542 A CN105254542 A CN 105254542A
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- liquid
- sulfonation
- vacuum ejector
- evaporating pot
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Abstract
The invention relates to a method and device for producing a leather fatliquoring agent by liquid SO3 sulfonation, and aims at providing the method with the characteristic of simple process and providing the device with the characteristic of high operation stability. The method has the technical scheme that the method for producing the leather fatliquoring agent by liquid SO3 sulfonation sequentially comprises the following steps that 1, animal and plant grease sulfonation circulation reuse materials enter a vacuum ejector; 2, liquid SO3 enters an SO3 evaporating tank according to a certain flow rate; 3, SO3 vapor and grease are primarily mixed in the vacuum ejector, and then enter a homogeneous pump; 4, animal and plant grease sulphonate is obtained. The device for producing the leather fatliquoring agent by liquid SO3 sulfonation is used in the following process including the steps that 1, the animal and plant grease enters a fluid inlet of the vacuum ejector, the liquid SO3 is conveyed into the SO3 evaporating tank, and the SO3 gas evaporated in the SO3 evaporating tank simultaneously enters an air suction opening of the vacuum ejector; 2, an vacuum ejector outlet is sequentially connected with the homogeneous pump and a heat exchanger through a pipeline.
Description
Technical field
The present invention relates to chemical field, be specially a kind of employing liquid SO
3the method of sulfonation production leather fat and device.
Background technology
Leather fat can give leather good to moisten, to fill, the performance such as plentiful, soft and for shelf-stable, be the key element in leather production, leather quality and use properties played a decisive role.Current conventional leather fat product mainly contains sulphonated oil, is generally to obtain by carrying out sulfonation processing to animal-plant oil.Existing comparatively ripe process for sulfonation generally adopts gas phase SO
3process for sulfonation, mainly comprises SO
3generation systems, sulfonation system, exhaust treatment system.
Existing conventional SO
3generation systems technique mainly contains combustion sulphur method and liquid SO
3method of evaporation.Combustion sulphur method refers to that sulfur burning obtains SO
2be catalytically converted into sulphur trioxide through catalyst again, period is mixed into a large amount of dry air and finally obtains the dense sulfur trioxide gas about 2-5% of gas for sulfonation; Liquid SO
3method of evaporation adopts existing liquid SO
3, sulfan in vaporizer after direct heating evaporation, then is diluted to the dense sulfur trioxide gas for 2-5% of gas with dry air.These two kinds of methods all need to use a large amount of dry air, and equipment is complicated, and energy consumption is large.Conventional sulfonation system generally adopts film sulfonator, organic material is formed liquid film and SO
3gas directly contacts and reacts, and equipment requirements is higher, and quality of forming film and gas diffusion velocity will directly affect sulfonation quality.In addition owing to introducing large quantity of air, after sulfonation reaction, these air can entrainment portions organic material drop and part unreacted SO
3, therefore need exhaust treatment system; Because air quantity is comparatively large, cause exhaust treatment system pressure comparatively large, generally can produce more electrostatic demist nigrotic acid, environmental benefit is poor.
Use liquid SO
3directly contact with animal-plant oil and carry out sulfonation reaction; Due to liquid SO
3molecular structure is Trimeric structures, directly contacts with animal-plant oil and can produce excessive sulfonation, cause grease carbonization blackening even coking phenomenon.Also have and use solvent method to utilize solvent cut grease to reduce liquid SO
3contact to control sulfonation degree with grease, but also face the problems such as solvent treatment, environmental effect is poor.
Summary of the invention
The object of the invention is to overcome the deficiency in above-mentioned background technology, provide a kind of and adopt liquid SO
3the method of sulfonation production leather fat and device thereof.The method has the advantages that technique is simple, be easy to control, energy-conserving and environment-protective, constant product quality excellence; This device have equipment requirements not high, install simple and easy, for ease of maintenaince and stable feature.
Technical scheme provided by the invention is:
A kind of employing liquid SO
3the method of sulfonation production leather fat, comprises the following steps successively:
1) animal-plant oil loops back materials by certain flow and sulfonation and enters a vacuum ejector by transferpump, and the negative pressure producing certain vacuum degree sucks SO
3steam; Certain vacuum degree is 1-50kpa;
2) liquid SO
3sO is entered by certain flow
3evaporating pot, simultaneously SO
3evaporating pot evaporation SO
3steam is supplied to vacuum ejector, and vaporization temperature is 40 ~ 70 DEG C; SO
3evaporating pot adds appropriate amount oleum or the vitriol oil in advance, SO when making steady running
3vapor temperature, vacuum tightness and SO
3velocity of evaporation maintain balance;
3) SO
3steam and grease enter a Homogenizing pump and mix further, then enter interchanger and remove sulfonation reaction heat after tentatively mixing in vacuum ejector, and controlling sulfonation system temperature is 40 ~ 70 DEG C;
4) interchanger out after material be the sulphonate of animal-plant oil, part loops back before materials are delivered to transferpump as sulfonation and continues to enter vacuum ejector, and part goes neutralization to obtain sulphonated oil product.
Described step 1) in, animal-plant oil can be in rapeseed oil, plam oil, lard and Tallow Inedible Grade one or more.
Animal-plant oil flow needs to determine according to sulfonation production capacity, is generally 0.1-5t/h.
Described step 1) in, cyclically utilizing stream amount is determined by vacuum ejector parameter, makes the total flux entering vacuum ejector that vacuum ejector can be made to produce vacuum tightness needed for technique; When vacuum ejector type number mates rationally with grease stream material, grease flow directly can meet vacuum level requirement, and cyclically utilizing inventory can be 0, namely without the need to cyclically utilizing.
Described step 2) in, liquid SO
3pan feeding flow relevant to the flow of animal-plant oil, general control liquid SO
3flow is 1 ~ 10% of animal-plant oil flow.
Described step 2) in, liquid SO
3velocity of evaporation need control and liquid SO
3pan feeding flow consistent, maintain SO through but not limited to use weight scale
3the constant method of evaporating pot tank body gross weight controls.
Described step 2) in, add-on vacuum tightness, SO needed for technique of oleum or the vitriol oil
3gas temperature and SO
3evaporating pot volume determines, general control is: when reaching steady concentration, oleum or vitriol oil volume are SO
3evaporating pot volume 30-60%.
A kind of employing liquid SO
3the device of sulfonation production leather fat, is characterized in that this device comprises:
1) animal-plant oil is conducted through pipeline by impeller pump and enters vacuum ejector fluid intake, liquid SO
3sO is conveyed into by second pipe
3evaporating pot, SO
3the SO of evaporation in evaporating pot
3gas enters vacuum ejector suction opening by the first pipeline simultaneously;
2) vacuum ejector outlet connects Homogenizing pump, interchanger successively by pipeline; In heat exchanger exit material, partial material is fed back to impeller pump entrance by the 3rd piping loop, and partial material removes lower stepping single step reaction by Cemented filling.
Described SO
3evaporating pot configuration heating unit, includes but not limited to spiral heater or jacketed type well heater.
Described SO
3evaporating pot also configures whipping appts, includes but not limited to mechanical stirrer or magnetic stirring apparatus.
Thinking of the present invention is under utilizing vacuum, SO
3gaseous phase is close to the SO after drying Dilution air
3gaseous phase, coordinates vacuum ejector and Homogenizing pump to carry out Forced Mixing, there will not be directly utilize SO for sulfonation
3the oversulfonate phenomenon that liquid causes, the more conventional membrane-type sulfonation of sulfonation effect is more excellent.
For SO under vacuum
3extremely evaporable feature, at SO
3inside add part of sulfuric acid and make SO
3form oleum system in evaporating pot, make system gas phase SO needed for sulfonation
3steady-state evaporation can be realized under temperature (40 ~ 70 DEG C), certain vacuum (1-50kpa).As long as control vacuum tightness, gas phase SO in actual motion
3stablizing, along with liquid SO of temperature
3stablely to add, SO
3in evaporating pot, oleum system can reach equilibrium concentration rapidly automatically, the SO of maintenance
3steady-state evaporation.When in evaporating pot, oleum concentration is higher, make the corresponding decline of its boiling point, gas phase SO
3temperature and then declines, and causes evaporation to be accelerated, due to liquid SO
3add constant flow, oleum concentration can decline rapidly and reach target value; Otherwise when oleum concentration in evaporating pot is on the low side also can corresponding automatic adjustment, finally make vacuum tightness, gas phase SO
3temperature, gas phase SO
3velocity of evaporation reaches process goal value.
The present invention compared with prior art, has following outstanding advantages and positively effect:
1) contrast conventional gas-phase process for sulfonation, eliminate the complicated complex appts such as dry gas generation, tail gas absorption, equipment is simple, energy consumption is low.
2) vacuum ejector is utilized to produce negative pressure of vacuum evaporation SO
3, obtain the SO under high vacuum
3gas, its state performance is close to the dense 2-5% gas phase SO of gas
3, can well avoid directly using liquid SO for sulfonation
3the oversulfonate problem that sulfonation causes, the sulfonated product color and luster obtained is good.
3) utilize vacuum ejector and Homogenizing pump to SO
3realize Forced Mixing with animal-plant oil, relatively traditional membrane-type sulfonation, sulfonation reaction is more stable, and product quality is better.
4) less investment of the present invention, not high to equipment requirements, all devices configured is the matured product of outsourcing, installs simple and easy, and for ease of maintenaince, simultaneity factor is stable, is easy to control.
Accompanying drawing explanation
Fig. 1 is the apparatus structure schematic diagram of employing liquid SO3 sulfonation production leather fat of the present invention.Wherein 1 is animal-plant oil, and 2 is SO
3, 3 is transferpump, and 4 is SO
3evaporating pot, 5 is vacuum ejector, and 6 is Homogenizing pump, and 7 is interchanger, and 8 is sulphonate (sulfuric ester).
Embodiment
Use liquid SO provided by the invention
3carry out the device of sulfonation, comprising:
1) animal-plant oil 1 is conducted through by transferpump 3 fluid intake that pipeline enters vacuum ejector 5, liquid SO
32 deliver into SO by second pipe
3evaporating pot 4, SO
3the SO of evaporation in evaporating pot
3gas enters vacuum ejector suction opening by the first pipeline simultaneously;
Described SO
3evaporating pot is configured with heating unit, and heating unit recommends spiral heater or jacketed type well heater;
Described SO
3evaporating pot is also configured with whipping appts, and whipping appts recommends mechanical stirrer or magnetic stirring apparatus;
2) vacuum ejector outlet connects Homogenizing pump 6, interchanger 7 successively by pipeline; In heat exchanger exit material, partial material is by the 3rd pipe section cyclically utilizing to transferpump entrance, and partial material 8 removes lower stepping single step reaction by Cemented filling.
Further illustrate below by way of specific embodiment.
Embodiment 1
The sulfonation of 1t/h rapeseed oil
SO
350L conventional belt coil pipe stirred autoclave selected by evaporating pot, adds the about 10L vitriol oil in advance.
Rapeseed oil enters vacuum ejector by the flow of 1t/h, liquid SO
3sO is entered by the flow of 55kg/h
3evaporating pot.After steady running, control interchanger Posterior circle reuse mass flow and make vacuum ejector form the vacuum of 40kpa, SO
3evaporating pot 55 DEG C, under 40kpa condition for the velocity-stabilization press 50kg/h evaporates SO
3(control weight by weight scale to maintain, SO
3evaporating pot is about 40%), material by vacuum ejector out after through by the further hybrid reaction of Homogenizing pump, the interchanger control temperature system that enters, to after 45 DEG C, neutralizes by the speed of about 1.05t/h and liquid caustic soda and obtains sulphonated oil product, the product obtained meets top grade product index, specific as follows:
| Project | Index |
| Outward appearance (25 DEG C) | Yellowish brown liquid |
| Binding capacity, % | 5.2 |
| Vitriol, % | 0.9 |
| Color and luster, Hazen (5% hexane solution) | 352 |
Embodiment 2
The palmitic sulfonation of 2t/h
SO
350L conventional belt coil pipe stirred autoclave selected by evaporating pot, adds the about 10L vitriol oil in advance.
Rapeseed oil enters vacuum ejector by the flow of 2t/h, liquid SO
3sO is entered by the flow of 120kg/h
3evaporating pot.After steady running, control interchanger Posterior circle reuse mass flow and make vacuum ejector form the vacuum of 45kpa, SO
3evaporating pot 60 DEG C, under 45kpa condition for the velocity-stabilization press 120kg/h evaporates SO
3(control weight by weight scale to maintain, SO
3evaporating pot is about 40%), material by vacuum ejector out after through by the further hybrid reaction of Homogenizing pump, the interchanger control temperature system that enters, to after 50 DEG C, neutralizes by the speed of about 2.1t/h and liquid caustic soda and obtains sulphonated oil product, the product obtained meets top grade product index, specific as follows:
| Project | Index |
| Outward appearance (25 DEG C) | Yellowish brown liquid |
| Binding capacity, % | 5.3 |
| Vitriol, % | 1.1 |
| Color and luster, Hazen (5% hexane solution) | 309 |
Embodiment 3
The sulfonation of 1t/h lard
SO
350L conventional belt coil pipe stirred autoclave selected by evaporating pot, adds the about 10L vitriol oil in advance.
Rapeseed oil enters vacuum ejector by the flow of 1t/h, liquid SO
3sO is entered by the flow of 60kg/h
3evaporating pot.After steady running, control interchanger Posterior circle reuse mass flow and make vacuum ejector form the vacuum of 45kpa, SO
3evaporating pot 55 DEG C, under 45kpa condition for the velocity-stabilization press 60kg/h evaporates SO
3(control weight by weight scale to maintain, SO
3evaporating pot is about 40%), material by vacuum ejector out after through by the further hybrid reaction of Homogenizing pump, the interchanger control temperature system that enters, to after 50 DEG C, neutralizes by the speed of about 1.1t/h and liquid caustic soda and obtains sulphonated oil product, the product obtained meets top grade product index, specific as follows:
| Project | Index |
| Outward appearance (25 DEG C) | Yellowish brown liquid |
| Binding capacity, % | 5.3 |
| Vitriol, % | 1.1 |
| Color and luster, Hazen (5% hexane solution) | 412 |
Claims (9)
1. one kind adopts liquid SO
3the method of sulfonation production leather fat, comprises the following steps successively:
1) animal-plant oil loops back materials by certain flow and sulfonation and enters a vacuum ejector by transferpump, and the negative pressure producing certain vacuum degree sucks SO
3steam; Described certain vacuum degree is 1-50kpa;
2) liquid SO
3sO is entered by certain flow
3evaporating pot, simultaneously SO
3evaporating pot evaporation SO
3steam is supplied to vacuum ejector, and vaporization temperature is 40 ~ 70 DEG C; SO
3appropriate amount oleum or the vitriol oil is added in advance, SO when making steady running in evaporating pot
3vapor temperature, vacuum tightness and SO
3velocity of evaporation maintain balance;
3) SO
3steam and grease enter a Homogenizing pump and mix further, then enter interchanger and remove sulfonation reaction heat after tentatively mixing in vacuum ejector, and controlling sulfonation system temperature is 40 ~ 70 DEG C;
4) interchanger out after material be the sulphonate of animal-plant oil, part loops back before materials are delivered to transferpump as sulfonation and continues to enter vacuum ejector, and part goes neutralization to obtain sulphonated oil product.
2. employing liquid SO according to claim 1
3the method of sulfonation production leather fat, is characterized in that: described step 1) in, animal-plant oil can be in rapeseed oil, plam oil, lard and Tallow Inedible Grade one or more.
3. employing liquid SO according to claim 1
3the method of sulfonation production leather fat, is characterized in that: described step 1) in the certain flow of animal-plant oil be 0.1-5t/h.
4. employing liquid SO according to claim 1
3the method of sulfonation production leather fat, is characterized in that: described step 2) middle liquid SO
3pan feeding flow be 1 ~ 10% of animal-plant oil flow.
5. employing liquid SO according to claim 1
3the method of sulfonation production leather fat, is characterized in that: described step 2) middle liquid SO
3velocity of evaporation and liquid SO
3pan feeding flow consistent, maintain SO by using weight scale
3the constant method of evaporating pot tank body gross weight controls.
6. employing liquid SO according to claim 1
3the method of sulfonation production leather fat, is characterized in that: described step 2) in the add-on of oleum or the vitriol oil control be: when reaching steady concentration, oleum or vitriol oil volume are SO
3the 30-60% of evaporating pot volume.
7. one kind adopts liquid SO
3the device of sulfonation production leather fat, is characterized in that this device comprises:
1) animal-plant oil (1) is conducted through pipeline by impeller pump (3) and enters vacuum ejector (5) fluid intake, liquid SO
3(2) SO is conveyed into by second pipe
3evaporating pot (4), SO
3the SO of evaporation in evaporating pot
3gas enters vacuum ejector suction opening by the first pipeline simultaneously;
2) vacuum ejector outlet connects Homogenizing pump (6), interchanger (7) successively by pipeline; In heat exchanger exit material, partial material is fed back to impeller pump entrance by the 3rd piping loop, and partial material removes lower stepping single step reaction by Cemented filling.
8. employing liquid SO according to claim 7
3the device of sulfonation production leather fat, is characterized in that: described SO
3the heating unit of evaporating pot configuration comprises spiral heater or jacketed type well heater.
9. employing liquid SO according to claim 8
3the device of sulfonation production leather fat, is characterized in that: described SO
3the whipping appts of evaporating pot configuration comprises mechanical stirrer or magnetic stirring apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510726853.8A CN105254542A (en) | 2015-10-30 | 2015-10-30 | Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510726853.8A CN105254542A (en) | 2015-10-30 | 2015-10-30 | Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation |
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|---|---|
| CN105254542A true CN105254542A (en) | 2016-01-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510726853.8A Pending CN105254542A (en) | 2015-10-30 | 2015-10-30 | Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693422A (en) * | 2005-04-30 | 2005-11-09 | 江苏高科石化股份有限公司 | Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter |
| CN101423482A (en) * | 2008-11-27 | 2009-05-06 | 中国日用化学工业研究院 | Integrated method of sulphonation and neutralization reaction |
| CN101690852A (en) * | 2009-10-19 | 2010-04-07 | 浙江赞宇科技股份有限公司 | Evaporation technique for liquid sulfur trioxide |
-
2015
- 2015-10-30 CN CN201510726853.8A patent/CN105254542A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693422A (en) * | 2005-04-30 | 2005-11-09 | 江苏高科石化股份有限公司 | Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter |
| CN101423482A (en) * | 2008-11-27 | 2009-05-06 | 中国日用化学工业研究院 | Integrated method of sulphonation and neutralization reaction |
| CN101690852A (en) * | 2009-10-19 | 2010-04-07 | 浙江赞宇科技股份有限公司 | Evaporation technique for liquid sulfur trioxide |
Non-Patent Citations (1)
| Title |
|---|
| 兰云军等: "磺化技术在生产皮革加脂剂中的应用", 《中国皮革》 * |
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Application publication date: 20160120 |
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