CN205740836U - A kind of equipment preparing sulfonate - Google Patents
A kind of equipment preparing sulfonate Download PDFInfo
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- CN205740836U CN205740836U CN201620737638.8U CN201620737638U CN205740836U CN 205740836 U CN205740836 U CN 205740836U CN 201620737638 U CN201620737638 U CN 201620737638U CN 205740836 U CN205740836 U CN 205740836U
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Abstract
This utility model belongs to sulfonate field, particularly relates to a kind of equipment preparing sulfonate, including: neutralize still, described neutralization still is provided with charge door, the first recycle feed mouth and the first circulation discharging opening；And carbonization reactor, described carbonization reactor is provided with CO2Air inlet, the flux oil charging aperture of metal-containing compound, the second recycle feed mouth and the second circulation discharging opening；Described first circulation discharging opening is connected with described second recycle feed mouth by circulating pump, and described first recycle feed mouth and the second circulation discharging opening are connected.This equipment is provided with the flux oil charging aperture of metal-containing compound, metallic compound is made to enter reaction system with flux oil, improve metallic compound scattered uniformity in reaction system, simultaneously by being arranged on the circulation charging and discharging mouth neutralized on still and carbonization reactor, the reaction raw materials circulating contact making equipment inner chamber reacts, so that the sulfonate goods prepared have relatively low precipitation number and turbidity, and higher stability.
Description
Technical field
This utility model belongs to sulfonate field, particularly relates to a kind of equipment preparing sulfonate.
Background technology
Detersive is an indispensable class additive in lubricating oil.On the one hand it as surfactant, increase by it
The severe contamination harm that in molten, peptization or peace and quiet peptizaiton suppression internal combustion engine, Fuels And Lubricants causes, on the other hand can also
Offer alkalescence is stocked, and effectively neutralizes harmful mineral acid that fuel and lubricating oil inevitably generates under applying working condition and has
Machine acid, thus reach to slow down oil oxidation and decay, reduce engine corrosion abrasion, extend oil product and the mesh of service life of aeroengine
's.
Sulfonate is the detergent for lubricating oil that a class is important, and its alkalescence is peace and quiet effective to greasy filth, it is adaptable to modulate various
I. C. engine oil, including gasoline engine oil, diesel engine oil and grease etc., not only can reduce in engine chamber paint film and long-pending
The deposition of charcoal, keeps piston cleaning, it is also possible to avoid the sour corrosion of parts, and can extend its oil draining period.
In existing sulfonate production technology, use sulfonic acid, flux oil, solvent, accelerator and solid metal chemical combination more
The raw materials such as thing are first neutralized reaction at reactor, obtain reactant liquor；CO it is passed through the most again in reactor2, make reactant liquor with
CO2Carry out carbonation reaction, obtain sulfonate.But there is product precipitation number height, turbidity greatly in this mode of production, poor stability
Problem, particularly particularly evident in the production process making sulfonate with high base number product salt.
Utility model content
In view of this, the purpose of this utility model is to provide a kind of equipment preparing sulfonate, uses this utility model
The sulfonate goods that the equipment provided prepares have relatively low precipitation number and turbidity, and higher stability.
This utility model provides a kind of equipment preparing sulfonate, including:
Neutralize still, described neutralization still is provided with charge door, the first recycle feed mouth and the first circulation discharging opening；
And carbonization reactor, described carbonization reactor is provided with CO2Air inlet, the flux oil charging of metal-containing compound
Mouth, the second recycle feed mouth and the second circulation discharging opening；
Described first circulation discharging opening is connected with described second recycle feed mouth by circulating pump, described first recycle feed
Mouth is connected with the second circulation discharging opening.
Preferably, the inner chamber of described neutralization still is provided with the first agitating device；The inner chamber of described carbonization reactor is provided with
Second agitating device.
Preferably, described neutralization still is provided with the first temperature regulating device.
Preferably, described first temperature regulating device is coated on the sidewall neutralizing still.
Preferably, the inner chamber of described carbonization reactor is provided with the second agitating device.
Preferably, described carbonization reactor is provided with the second temperature regulating device.
Preferably, described second temperature regulating device is coated on the sidewall of carbonization reactor.
Preferably, the volume of described neutralization still is 10～50m3。
Preferably, described carbonization reactor is cylindrical carbonization reactor.
Preferably, a height of the 1000～10000mm of described carbonization reactor；The internal diameter of described carbonization reactor be 100～
1000mm。
Compared with prior art, this utility model provides a kind of equipment preparing sulfonate.This utility model provides
Equipment includes: neutralize still, and described neutralization still is provided with charge door, the first recycle feed mouth and the first circulation discharging opening；And carbon
Change reactor, described carbonization reactor is provided with CO2Air inlet, the flux oil charging aperture of metal-containing compound, the second circulation
Charging aperture and the second circulation discharging opening；Described first circulation discharging opening is connected with described second recycle feed mouth by circulating pump,
Described first recycle feed mouth and the second circulation discharging opening are connected.When described equipment enables, first by sulfonic acid, solvent, accelerator
Neutralization still inner chamber with the flux oil of part metal-containing compound joins described equipment by charge door, reacts, obtains
Reactant liquor；Start the circulating pump of described equipment afterwards, and respectively to described CO2The flux oil of air inlet and metal-containing compound enters
Material mouth adds CO2With the flux oil of surplus metal-containing compound, each raw material is by the first recycle feed mouth, the first circulation discharging
Mouth, the second recycle feed mouth and the second circulation discharging opening circulate in neutralizing still and carbonization reactor and react, and obtain sulphur
Hydrochlorate.The equipment that this utility model provides is provided with the flux oil charging aperture of metal-containing compound, makes metallic compound with dilution
Oil enter reaction system, improve metallic compound scattered uniformity in reaction system, simultaneously by be arranged on neutralization still and
Circulation charging and discharging mouth on carbonization reactor, makes the reaction raw materials circulating contact of equipment inner chamber react, and improves each reaction further
The mixing uniformity of raw material, so that the sulfonate goods prepared have relatively low precipitation number and turbidity, and higher stablizing
Property.Test result indicate that, base number 509mgKOH/g, 100 DEG C of motions that the equipment using this utility model to provide prepares are viscous
Degree 175mm2The turbidity of the sulfonate of/s is 10.75NTU, and mean diameter is that these sulfonate goods of 29.5nm, 10g are dissolved in three class oil
Middle room temperature keeps 180 days, and oil sample is bright to be produced without precipitation without muddy.
Accompanying drawing explanation
In order to be illustrated more clearly that this utility model embodiment or technical scheme of the prior art, below will be to embodiment
Or the required accompanying drawing used is briefly described in description of the prior art, it should be apparent that, the accompanying drawing in describing below is only
It is embodiment of the present utility model, for those of ordinary skill in the art, on the premise of not paying creative work, also
Other accompanying drawing can be obtained according to the accompanying drawing provided.
Fig. 1 is the device structure schematic diagram preparing sulfonate that this utility model embodiment provides.
Detailed description of the invention
Below in conjunction with the accompanying drawing in this utility model embodiment, the technical scheme in this utility model embodiment is carried out
Clearly and completely describe, it is clear that described embodiment is only a part of embodiment of this utility model rather than whole
Embodiment.Based on the embodiment in this utility model, those of ordinary skill in the art are not under making creative work premise
The every other embodiment obtained, broadly falls into the scope of this utility model protection.
This utility model provides a kind of equipment preparing sulfonate, including:
Neutralize still, described neutralization still is provided with charge door, the first recycle feed mouth and the first circulation discharging opening；
And carbonization reactor, described carbonization reactor is provided with CO2Air inlet, the flux oil charging of metal-containing compound
Mouth, the second recycle feed mouth and the second circulation discharging opening；
Described first circulation discharging opening is connected with described second recycle feed mouth by circulating pump, described first recycle feed
Mouth is connected with the second circulation discharging opening.
Seeing Fig. 1, Fig. 1 is the device structure schematic diagram preparing sulfonate that this utility model embodiment provides.In Fig. 1,1
Be neutralize still, 2 be carbonization reactor, 3 be circulating pump, 1-1 be charge door, 1-2 be the first recycle feed mouth, 1-3 be first to follow
Ring discharging opening, 1-4 be the first agitating device, 1-5 be the first temperature regulating device, 2-1 be CO2Air inlet, 2-2 are metal-containing compounds
Flux oil charging aperture, 2-3 be the second recycle feed mouth, 2-4 be the second circulation discharging opening, 2-5 be the second agitating device, 2-6
It it is the second temperature regulating device.
The equipment preparing sulfonate that this utility model provides includes neutralizing still 1 and carbonization reactor 2.Wherein, still 1 is neutralized
Flux oil for sulfonic acid, solvent, accelerator and part metal-containing compound reacts, be provided with charge door 1-1,
One recycle feed mouth 1-2 and first circulation discharging opening 1-3.In the embodiment that this utility model provides, neutralize the interior of still 1
Chamber is additionally provided with the first agitating device 1-4.In the embodiment that this utility model provides, neutralize and be additionally provided with the on still 1
One temperature regulating device 1-5.The neutralization still 1 that this utility model provides is provided with in the embodiment of the first temperature regulating device 1-5,
First temperature regulating device 1-5 is coated on the sidewall neutralizing still 1.In the embodiment that this utility model provides, neutralize still 1
Volume is 10～50m3；In another embodiment that this utility model provides, the volume neutralizing still 1 is 25～30m3。
In this utility model, carbonization reactor 2 is for neutralizing product and CO prepared by still2And metal-containing compound
Flux oil be circulated reaction and prepare sulfonate, be provided with CO2Air inlet 2-1, the flux oil of metal-containing compound enter
Material mouth 2-2, the second recycle feed mouth 2-3 and second circulation discharging opening 2-4.In the embodiment that this utility model provides,
The inner chamber of carbonization reactor 2 is additionally provided with the second agitating device 2-5.In the embodiment that this utility model provides, carbonization
The second temperature regulating device 2-6 it is additionally provided with on reactor 2.The carbonization reactor 2 that this utility model provides is provided with the
In the embodiment of two temperature regulating device 2-6, the second temperature regulating device 2-6 is coated on the sidewall of carbonization reactor 2.At this utility model
In the embodiment provided, carbonization reactor 2 is cylindrical carbonization reactor, and a height of 1000～10000mm, internal diameter is 100
～1000mm；In another embodiment that this utility model provides, carbonization reactor a height of 5000～6000mm, internal diameter is
500～600mm.
In this utility model, the first circulation discharging opening 1-3 is connected with the second recycle feed mouth 2-3 by circulating pump 3, institute
State the first recycle feed mouth 1-2 and second circulation discharging opening 2-4 to be connected.Realize material by this connected mode and neutralize still 1
With the circular response in carbonization reactor 2.This utility model provide an embodiment in, first circulation discharging opening 1-3 and
It is additionally provided with discharging opening, for the sulfonate for preparing being derived described sulfonate of preparing on the connecting line of circulating pump 3
Equipment.
When described equipment enables, first by the flux oil of sulfonic acid, solvent, accelerator and part metal-containing compound by adding
Material mouth joins the neutralization still inner chamber of described equipment, reacts, obtains reactant liquor；Start the circulating pump of described equipment afterwards,
And respectively to described CO2The flux oil charging aperture of air inlet and metal-containing compound adds CO2With surplus metal-containing compound
Flux oil, each raw material is by the first recycle feed mouth, the first circulation discharging opening, the second recycle feed mouth and the second circulation discharging opening
Circulate in neutralizing still and carbonization reactor and react, obtaining sulfonate.
The equipment that this utility model provides is provided with the flux oil charging aperture of metal-containing compound, makes metallic compound with dilute
Release oil and enter reaction system, improve metallic compound scattered uniformity in reaction system, simultaneously by being arranged on neutralization still
With the circulation charging and discharging mouth on carbonization reactor, making the reaction raw materials circulating contact of equipment inner chamber react, raising is each instead further
Answering the mixing uniformity of raw material, so that the sulfonate goods prepared have relatively low precipitation number and a turbidity and higher is steady
Qualitative.
This utility model provides the preparation method of a kind of sulfonate, comprises the following steps:
A), the flux oil of sulfonic acid, solvent, accelerator and part metal-containing compound is mixed in neutralizing still, carry out anti-
Should, obtain reactant liquor；
B) reactant liquor, in described neutralization still is pumped to carbonization reactor by circulating pump, returns again to neutralize still, and in
It is circulated with in the system of still, circulating pump and carburizing reagent still composition；CO is added in the reactant liquor of circulation2With containing of surplus
The flux oil of metallic compound, reacts, and obtains sulfonate.
In the preparation method that this utility model provides, first by sulfonic acid, solvent, accelerator and part metal-containing compound
Flux oil mix neutralizing in still.Wherein, described sulfonic acid preferably includes alkyl benzene sulphonate, more preferably includes C15～C25 long-chain
LINER ALKYL BENZENE SULPHONIC ACID SOFT 96, most preferably includes C16～C18 long-chain linear alkylbenzene sulfonic acid and/or C20～C24 long-chain linear alkyl
Benzenesulfonic acid.The described sulfonic acid provided at this utility model includes C16～C18 long-chain linear alkylbenzene sulfonic acid and C20～C24
In the embodiment of long-chain linear alkylbenzene sulfonic acid, described C16～C18 long-chain linear alkylbenzene sulfonic acid and C20～C24 long-chain linear
The mass ratio of alkyl benzene sulphonate is for being preferably (30～80): (70～20), more preferably (50～70): (50～30).
In this utility model, described solvent preferably includes boiling range 100～the hydrocarbon of 200 DEG C, more preferably include boiling range 110～
The alkane of 190 DEG C and/or boiling range 110～the aromatic hydrocarbons of 190 DEG C, most preferably include boiling range 150～the alkane of 190 DEG C and/or boiling range
The aromatic hydrocarbons of 110～120 DEG C.The described solvent provided at this utility model includes boiling range 150～the alkane of 190 DEG C and boiling range
In the embodiment of the aromatic hydrocarbons of 110～120 DEG C, the matter of the aromatic hydrocarbons of described boiling range 150～the alkane of 190 DEG C and boiling range 110～120 DEG C
Amount ratio is preferably (20～80): (80～20), more preferably (40～60): (60～40).In this utility model, described sulfonic acid
Be preferably (2000～5000) with the mass ratio of solvent: (4000～7000), more preferably (3000～4500): (5000～
6500)。
In this utility model, described accelerator includes but not limited to alcohols accelerator, phenol accelerant, amine type accelerator
With one or more in anhydride accelerator；Wherein, described alcohols accelerator preferably includes methanol；Described phenol accelerant is excellent
Choosing include dodecylphenol and/or calcium sulfenyl phenolate, the total base number (TBN) of described calcium sulfenyl phenolate be preferably 0～
300mgKOH/g；Described amine type accelerator preferably includes tetramethylethylenediamine and/or ethylenediamine；Described anhydride accelerator is preferably wrapped
Including alkene acid anhydride, the number-average molecular weight of described alkene acid anhydride is preferably 1000～2000.The described accelerator that this utility model provides
In embodiment including alcohols accelerator, phenol accelerant and amine type accelerator, described alcohols accelerator, phenol accelerant and amine
The mass ratio of class accelerator is preferably, more preferably (1275～1620): (300～350): (50～60).At this utility model
In, the mass ratio of described sulfonic acid and accelerator is preferably (2000～5000): (1500～2000), more preferably (3000～
4500): (1625～1980).
In this utility model, the flux oil of described metal-containing compound is by mixing that metallic compound and flux oil form
Compound, wherein, described metallic compound includes one or more in slaine, metal hydroxides and metal oxide；
Described slaine includes but not limited to one or more in calcium salt, magnesium salt, sodium salt, barium salt and lithium salts；Described metallic hydrogen aoxidizes
Thing includes but not limited to one or more in calcium hydroxide, magnesium hydroxide, sodium hydroxide, barium hydroxide and Lithium hydrate；Institute
State metal-oxide and include but not limited to one or more in calcium oxide, magnesium oxide, sodium oxide, Barium monoxide and lithium oxide；Institute
State the granularity of metallic compound preferably≤20 μm.In this utility model, described flux oil preferably includes hydrogenated base oil, is not added with
One or more in hydrogen base oil, Poly alpha Olefins (PAO) artificial oil (PAO) and natural gas synthetic oil (GTL), more preferably include 150N
One or more in hydrogenated base oil, 150SN not hydrogenated base oil, PAO-4 artificial oil and GTL artificial oil.New in this practicality
In type, the content of the metallic compound in the flux oil of described metal-containing compound is preferably 20～80wt%, more preferably 40
～60wt%.In this utility model, the mass ratio of the flux oil of described sulfonic acid and part metal-containing compound is preferably (2000
～5000): (300～3000), more preferably (3000～4500): (500～2500).
In this utility model, the most also adding kicker to described neutralization still, described kicker includes but does not limits
One or more in ammonia, acetic acid, ammonium carbonate and calcium chloride.In this utility model, described sulfonic acid and kicker
Mass ratio is preferably (2000～5000): (150～400), more preferably (3000～4500): (200～320).
In this utility model, described neutralization still is preferably provided with agitating device, neutralizes in still running, agitating device
Stir speed (S.S.) be preferably 60～120 revs/min, more preferably 80～100 revs/min, most preferably 90 revs/min.
Above-mentioned raw materials after mixing, reacts in neutralizing still.Wherein, the temperature of described reaction is preferably 45～65 DEG C,
More preferably 51～55 DEG C, most preferably 51～54 DEG C or 53～55 DEG C；The time of described reaction is preferably 30～90min, more
It is preferably 40～50min, most preferably 45min.After reaction terminates, obtain reactant liquor.
Afterwards, the reactant liquor in described neutralization still is pumped to carbonization reactor by circulating pump, returns again to neutralize still, and
It is circulated in the system neutralizing still, circulating pump and carburizing reagent still composition；In the reactant liquor of circulation, add CO simultaneously2With
The flux oil of the metal-containing compound of surplus.In this utility model, described carbonization reactor is preferably provided with agitating device, carbon
Changing in reactor running, the stir speed (S.S.) of agitating device is preferably 70～130 revs/min, more preferably 90～110 turns/
Minute, most preferably 100 revs/min.In this utility model, described sulfonic acid, solvent, accelerator, metal-containing compound dilute
Release oil and CO2Mass ratio be preferably (2000～5000): (4000～7000): (1500～2000): (5000～10000):
(1500～4000), more preferably (3000～4500): (5000～6500): (1625～1980): (6300～8500):
(1700～3500).
In this utility model, the flow of described circulating pump, CO2The flow added and the flux oil of metal-containing compound add
The ratio of the flow entered is preferably (1500～5000): (5～40): (50～200), more preferably (1500～3500): (10～
30): (100～150), most preferably 2000:(10～30): (100～150).In this utility model, the stream of described circulating pump
Amount is preferably 1500～5000kg/min, more preferably 1500～3500kg/min, most preferably 2000kg/min.In this practicality
In novel, described CO2Addition temperature be preferably-10～35 DEG C, more preferably 5～20 DEG C；Described metal-containing compound dilute
The addition temperature releasing oil is preferably 0～40 DEG C, more preferably 20～40 DEG C.In this utility model, by controlling described circulation
The flow of pump, CO2The ratio of the flow that the flow added and the flux oil of metal-containing compound add, and CO2Addition temperature and
The addition temperature of the flux oil of metal-containing compound, controls the feed back in carbonization reactor and extremely neutralizes the temperature of still, institute
The temperature stating material is preferably controlled in 45～65 DEG C, more preferably controls, at 51～55 DEG C, most preferably to control at 51～54 DEG C or 53
～55 DEG C.In this utility model, described reactant liquor, CO2With the flux oil of the metal-containing compound of surplus carry out reacting time
Between be preferably 80～150min, more preferably 90～140min, most preferably 97～130min.After reaction terminates, reacted
Product, described product obtains sulfonate through post processing.In this utility model, the mode of described post processing preferably includes
Described product sequentially passes through vacuum distilling, remove the gred and reduce pressure distillation, obtains sulfonate.Wherein, the temperature of described vacuum distilling
Degree is preferably 80～100 DEG C, more preferably 85～100 DEG C；The pressure of described vacuum distilling is preferably 0～-0.09MPa.
The preparation method that this utility model provides, by making metallic compound enter reaction system with flux oil, improves metal
Compound is the scattered uniformity in reaction system, and simultaneously by making reaction raw materials circulating contact react, raising is each instead further
Answering the mixing uniformity of raw material, so that the sulfonate goods prepared have relatively low precipitation number and a turbidity and higher is steady
Qualitative.
Preferably prepare in scheme what this utility model provided, use the flux oil of suitable metal-containing compound to add temperature
Degree and speed, and CO2Ventilation air and speed, make circular response be maintained at optimum response state, improves product further
Quality.
Preferably prepare in scheme what this utility model provided, after using the mode of distillation that the product of circular response is carried out
Process, can faster the water in product and accelerator be distilled off, reduce the destruction to the sulfonate colloid formed,
Improve the quality of product further.
Test result indicate that, the base number 509mgKOH/g that the method using this utility model to provide prepares, 100 DEG C of fortune
Kinetic viscosity 175 (mm2/ s) the turbidity of sulfonate be 10.75NTU, mean diameter is that these sulfonate goods of 29.5nm, 10g are dissolved in
In three class oil, room temperature keeps 180 days, and oil sample is bright to be produced without precipitation without muddy.
For the sake of becoming apparent from, it is described in detail below by following example.
C16～the C18 long-chain linear alkylbenzene sulfonic acid used in following embodiment is prepared in accordance with the following methods:
In reactor, add 30kg aluminum chloride and 1500kg toluene, drip in 50～60 DEG C of downhill reaction stills
1000kg C16～C18 alpha-olefin (mass ratio of C16 Yu C18 is 20～60:80～40), continue reaction one section after completion of dropwise addition
Time, static 2～4h layerings, take supernatant liquid filtering, then through unreacted toluene is distilled off, obtain the long chain line of C16～C18
Property alkylbenzene；
According to C16～C18 long-chain linear alkylbenzene and oleum (0..85～1.1): the mass ratio of 1, to C16～C18
Long-chain linear alkylbenzene drips oleum, sulfonating reaction 2h at 40～60 DEG C, the most aging point of acid, obtains C16～C18
Long-chain linear alkylbenzene sulfonic acid (mean molecule quantity 410～420, activity substance content 87～95wt%).
C20～the C24 long-chain linear alkylbenzene sulfonic acid used in following embodiment is prepared in accordance with the following methods:
In reactor, add 30kg aluminum chloride and 1500kg toluene, drip in 50～60 DEG C of downhill reaction stills
1000kg C20～C24 alpha-olefin (C20, C22 are 40～60:20～40:10～30 with the mass ratio of C24), after completion of dropwise addition
Continue reaction a period of time, static 2～4h layerings, take supernatant liquid filtering, then through unreacted toluene is distilled off, obtain
C20～C24 long-chain linear alkylbenzene；
According to C20～C24 long-chain linear alkylbenzene and oleum (0..85～1.1): the mass ratio of 1, to C20～C24
Long-chain linear alkylbenzene drips oleum, sulfonating reaction 2h at 40～60 DEG C, the most aging point of acid, obtains C20～C24
Long-chain linear alkylbenzene sulfonic acid (mean molecule quantity 465～490, activity substance content 80～95wt%).
The part material source used in following embodiment is as follows:
| Title | Source |
| Boiling range 150～190 DEG C of alkane | Qilu Petrochemical |
| Boiling range 110～145 DEG C of aromatic hydrocarbons | Qilu Petrochemical |
| Branched alkyl phenol | Rui Feng new material limited company of Xinxiang City |
| Calcium sulfenyl phenolate | Rui Feng new material limited company of Xinxiang City |
| 150N hydrogenated base oil | Platform is moulded |
| GTL artificial oil | Shell XHVI 5 |
| PAO-4 artificial oil | PAO-4 floats in Exxon U.S.A |
Embodiment 1
Prepare the equipment of sulfonate
A kind of its structure of equipment preparing sulfonate as it is shown in figure 1, Fig. 1 be this utility model embodiment provide prepare sulphur
The device structure schematic diagram of hydrochlorate.This equipment preparing sulfonate includes neutralizing still 1 and carbonization reactor 2.Wherein, still 1 is neutralized
Volume be 25m3, above it is provided with charge door 1-1, the first recycle feed mouth 1-2 and the first circulation discharging opening 1-3, neutralizes still 1
Inner chamber is additionally provided with the first agitating device 1-4, neutralizes and is coated with the first temperature regulating device 1-5 on the sidewall of still 1.
Carbonization reactor 2 is cylindrical, and a height of 5000mm, internal diameter is 500mm, is above provided with CO2Air inlet 2-1, containing gold
Belong to the flux oil charging aperture 2-2 of compound, the second recycle feed mouth 2-3 and the second circulation discharging opening 2-4, carbonization reactor 2
Inner chamber is provided with the second agitating device 2-5, and carbonization reactor 2 sidewall is coated with the second temperature regulating device 2-6.
First circulation discharging opening 1-3 is connected with the second recycle feed mouth 2-3 by circulating pump 3, described first recycle feed
Mouth 1-2 and second circulation discharging opening 2-4 is connected.Material is realized in neutralizing still 1 and carbonization reactor 2 by this connected mode
Circular response.It is additionally provided with discharging opening, for being prepared on the connecting line of the first circulation discharging opening 1-3 and circulating pump 3
To sulfonate derive the described equipment preparing sulfonate.
When described equipment enables, first by the flux oil of sulfonic acid, solvent, accelerator and part metal-containing compound by adding
Material mouth joins the neutralization still inner chamber of described equipment, reacts, obtains reactant liquor；Start the circulating pump of described equipment afterwards,
And respectively to described CO2The flux oil charging aperture of air inlet and metal-containing compound adds CO2Dilute with surplus metal-containing compound
Releasing oil, each raw material is existed by the first recycle feed mouth, the first circulation discharging opening, the second recycle feed mouth and the second circulation discharging opening
Neutralize still circulation interior with carbonization reactor and react, obtaining sulfonate.
Embodiment 2
Equipment described in embodiment 1 is used to prepare alkyl benzene calcium sulfonate.
Still adds 5000kg mixed solvent (by 60wt% boiling range 150～190 DEG C of alkane and 40wt% boiling range to neutralizing
110～120 DEG C of aromatic hydrocarbons composition), 3000kg benzene mixed sulfonic acid (by 30wt%C20-C24 long-chain linear alkylbenzene sulfonic acid and
70wt%C16-C18 long-chain linear alkylbenzene sulfonic acid form), 1500kg 85wt% methanol aqueous solution, 300kg 60wt% acetic acid
Aqueous solution, 300kg branched alkyl phenol, 50kg tetramethylethylenediamine and the 500kg 150SN hydrogenated base oil containing 40wt%CaO
(CaO granularity ＜ 20 μm), neutralizing still stir speed (S.S.) is 90 revs/min, reacts 45min, obtain reactant liquor at 53～55 DEG C；
Then starting the second agitating device and circulating pump, carbonization reactor stir speed (S.S.) 100 revs/min, flow set is
2000kg/min, pumps into carbonization reactor by above-mentioned reactant liquor, adds to described carbonization reactor with 100kg/min flow simultaneously
150SN hydrogenated base oil (the CaO granularity ＜ 20 μm) 5800kg containing 40wt%CaO of 40 DEG C, simultaneously with 20kg/min flow to
Described carbonization reactor adds the CO of 20 DEG C21500kg, adds CO with 10kg/min flow the most again2200kg, is further continued for following
Ring reacts stopped reaction after 5 minutes, obtains product, and the temperature of charge in whole process carbonization reactor is maintained at 53～55
℃；
By above-mentioned product after discharging opening is derived, under the conditions of 90 DEG C, 0～-0.09MPa, vacuum distilling removes reaction
Most of accelerator in product and water, remove the gred the most by centrifugation, and further decompression be distilled off in product molten
Agent, obtains alkyl benzene sulphonate calcium product.
Detecting above-mentioned prepared alkyl benzene sulphonate calcium product, result is as follows: product base number 325mgKOH/g, and 100
DEG C kinematic viscosity 48mm2/ s, product turbidity 8NTU, mean diameter 15.8nm, infrared spectrum detection has feature at 861cm (-1) place
Peak, calcium carbonate is amorphous state, 10g product is dissolved in 100 DEG C of constant temperature in 90g150BS base oil and keeps 90 days, the bright nothing of oil sample
Muddy without precipitation generation.
Embodiment 3
Equipment described in embodiment 1 is used to prepare alkyl benzene calcium sulfonate.
(evaporated with 60wt% by 40wt% boiling range 150～190 DEG C of alkane solvents to neutralizing addition 6000kg mixing solvent in still
Journey 110～120 DEG C of aromatic hydrocarbons composition), 4000kg benzene mixed sulfonic acid (by 50wt%C20-C24 long-chain linear alkylbenzene sulfonic acid and
50wt%C16-C18 long-chain linear alkylbenzene sulfonic acid form), 1800kg 90wt% methanol aqueous solution, 400kg 60wt% carbonic acid
Amine molten water liquid, 300kg calcium sulfenyl phenolate (total base number 300mgKOH/g), 60kg tetramethylethylenediamine and 1500kg contain 40wt%
The GTL250 artificial oil (CaO granularity ＜ 20 μm) of CaO, neutralizing still stir speed (S.S.) is 90 revs/min, reacts at 53～55 DEG C
45min, obtains reactant liquor；
Then the second agitating device and startup circulating pump, carbonization reactor stir speed (S.S.) 100 revs/min, flow set is
2000kg/min, pumps into carbonization reactor by above-mentioned reactant liquor, adds to described carbonization reactor with 100kg/min flow simultaneously
GTL250 artificial oil (the CaO granularity ＜ 20 μm) 6000kg containing 40wt%CaO of 30 DEG C, simultaneously with 25kg/min flow to described
Carbonization reactor adds the CO of 5 DEG C21800kg, adds CO with 10kg/min flow the most again2200kg, is further continued for circular response
Stopped reaction after 5 minutes, obtains product, and the temperature of charge in whole process carbonization reactor is maintained at 51～54 DEG C；
By above-mentioned product after discharging opening is derived, under the conditions of 95 DEG C, 0～-0.09MPa, vacuum distilling removes reaction
Most of accelerator in product and water, remove the gred the most by centrifugation, and further decompression be distilled off in product molten
Agent, obtains alkyl benzene sulphonate calcium product.
Detecting above-mentioned prepared alkyl benzene sulphonate calcium product, result is as follows: product base number 418mgKOH/g, and 100
DEG C kinematic viscosity 81mm2/ s, product turbidity 9.5NTU, mean diameter 18.6nm, infrared spectrum detection has spy at 862cm (-1) place
Levying peak, calcium carbonate is amorphous state, 10g product is dissolved in PAO-4 room temperature in 90g artificial oil and keeps 180 days, and oil sample is bright without muddy
Turbid without precipitation generation.
Embodiment 4
Equipment described in embodiment 1 is used to prepare alkyl benzene calcium sulfonate.
(evaporated with 50wt% by 50wt% boiling range 150～190 DEG C of alkane solvents to neutralizing addition 6500kg mixing solvent in still
Journey 110～120 DEG C of aromatic hydrocarbons composition), 4500kg benzene mixed sulfonic acid (by 60wt%C20-C24 long-chain linear alkylbenzene sulfonic acid and
40wt%C16-C18 long-chain linear alkylbenzene sulfonic acid form), 1800kg 75wt% methanol solution, 500kg 40wt% calcium chloride
Aqueous solution, 300kg calcium sulfenyl phenolate (total base number 250mgKOH/g), 60kg ethylenediamine hydrate and 2500kg aoxidize containing 50wt%
The PAO-4 artificial oil (CaO granularity ＜ 20 μm) of calcium, neutralizing still stir speed (S.S.) is 90 revs/min, reacts 45 points at 53～55 DEG C
Clock, obtains reactant liquor；
Then starting the second agitating device and circulating pump, carbonization reactor stir speed (S.S.) 100 revs/min, flow set is
2000kg/min, pumps into carbonization reactor by above-mentioned reactant liquor, adds to described carbonization reactor with 100kg/min flow simultaneously
PAO-4 artificial oil (the CaO granularity ＜ 20 μm) 6000kg containing 50wt% calcium oxide of 20 DEG C, simultaneously with 30kg/min flow to institute
State the CO that carbonization reactor adds 20 DEG C23000kg, adds CO with 20kg/min flow the most again2500kg, is further continued for circulation
Stopped reaction after reacting 5 minutes, obtains product, and the temperature of charge in whole process carbonization reactor is maintained at 58～62
℃；
By above-mentioned product after discharging opening is derived, under the conditions of 100 DEG C, 0～-0.09MPa, vacuum distilling removes anti-
Answer the most of accelerator in product and water, remove the gred the most by centrifugation, and decompression is distilled off in product further
Solvent, obtains alkyl benzene sulphonate calcium product.
Detecting above-mentioned prepared alkyl benzene sulphonate calcium product, result is as follows: product base number 509mgKOH/g, and 100
DEG C kinematic viscosity 175mm2/ s, product turbidity 10.75NTU, mean diameter 29.5nm, infrared spectrum detects at 864cm (-1) place
Having characteristic peak, calcium carbonate is amorphous state, 10g product is dissolved in room temperature in three class oil and keeps 180 days, and oil sample is bright without muddy nothing
Precipitation produces.
The above is only preferred implementation of the present utility model, it is noted that for the common skill of the art
For art personnel, on the premise of without departing from this utility model principle, it is also possible to make some improvements and modifications, these improve and
Retouching also should be regarded as protection domain of the present utility model.
Claims (10)
1. prepare an equipment for sulfonate, including:
Neutralize still, described neutralization still is provided with charge door, the first recycle feed mouth and the first circulation discharging opening；
And carbonization reactor, described carbonization reactor is provided with CO2Air inlet, the flux oil charging aperture of metal-containing compound,
Two recycle feed mouths and the second circulation discharging opening；
Described first circulation discharging opening is connected with described second recycle feed mouth by circulating pump, described first recycle feed mouth and
Second circulation discharging opening is connected.
Equipment the most according to claim 1, it is characterised in that the inner chamber of described neutralization still is provided with the first agitating device.
Equipment the most according to claim 1, it is characterised in that be provided with the first temperature regulating device on described neutralization still.
Equipment the most according to claim 3, it is characterised in that described first temperature regulating device is coated on the sidewall neutralizing still
On.
Equipment the most according to claim 1, it is characterised in that the inner chamber of described carbonization reactor is provided with the second stirring dress
Put.
Equipment the most according to claim 1, it is characterised in that be provided with the second temperature regulating device on described carbonization reactor.
Equipment the most according to claim 6, it is characterised in that described second temperature regulating device is coated on the side of carbonization reactor
On wall.
Equipment the most according to claim 1, it is characterised in that the volume of described neutralization still is 10～50m3。
Equipment the most according to claim 1, it is characterised in that described carbonization reactor is cylindrical carbonization reactor.
Equipment the most according to claim 9, it is characterised in that a height of the 1000 of described carbonization reactor～10000mm；
The internal diameter of described carbonization reactor is 100～1000mm.
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| CN201620737638.8U CN205740836U (en) | 2016-07-13 | 2016-07-13 | A kind of equipment preparing sulfonate |
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| CN201620737638.8U CN205740836U (en) | 2016-07-13 | 2016-07-13 | A kind of equipment preparing sulfonate |
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