CN104610045B - Method for producing dimer acid, and production apparatus automatically enforcing method - Google Patents
Method for producing dimer acid, and production apparatus automatically enforcing method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C57/00—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
- C07C57/26—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms containing rings other than six-membered aromatic rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/353—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by isomerisation; by change of size of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C55/00—Saturated compounds having more than one carboxyl group bound to acyclic carbon atoms
- C07C55/26—Saturated compounds having more than one carboxyl group bound to acyclic carbon atoms containing rings other than aromatic rings
- C07C55/28—Saturated compounds having more than one carboxyl group bound to acyclic carbon atoms containing rings other than aromatic rings monocyclic
Abstract
The invention provides a method for continuously producing dimer acid. The method comprises the following steps: 1, mixing unsaturated fatty acid with a catalyst, and carrying out vacuum degassing; 2, adding the mixture obtained in step 1 to a continuous reaction system, and reacting, wherein preferably 0-5wt% of water is added to the mixture; 3, acidifying the product obtained after the above reaction, and filtering to obtain crude dimer acid; and 4, purifying the crude dimer acid. The continuous reaction system comprises at least two groups of reaction devices, each of the reaction devices comprises a material inlet, a reactor and a material outlet, the first group of reaction devices is used for preheating raw materials, the second group of reaction devices is a reaction generator, and preferably, the system comprises a third group of reaction devices used for heat insulation. The invention also provides a polymerization reaction production apparatus.
Description
Technical field
The application is related to a kind of production equipment of polyreaction and the method producing dimeric dibasic acid using this equipment.
Technical background
Dimeric dibasic acid is a kind of important grease chemical article, and it is with 18 carbon unsaturated fatty acids in natural oil, such as oil
Acid, linoleic acid are raw material, the dicarboxylic acids being generated by diels-alder reaction.One kind as Fine Chemical is important
Intermediate, dimeric dibasic acid is mainly used to synthesizing polyamides resin, its be widely used in machinery, automobile, electronics, motor, Aero-Space,
In the fields such as building, printing, daily use chemicals, weaving, ship, coating, chemical industry.
The production technology of domestic dimeric dibasic acid mostly is autoclave batchwise polymerization (cn101838193a), this technological temperature and pressure at present
Power is wayward, leads to unstable product quality, energy consumption is also larger simultaneously.Compared to batchwise polymerization, continuous polymerization has more
Superiority, its power consumption is few, and product quality is stable.Abroad just occur in that a kind of technique of continuous thermal polymerization in nineteen fifty-three
(us2664429), having reached the effect of energy-conservation at that time, but thermal polymerization process reaction temperature higher (350-400 DEG C), product matter
Amount is poor, and it is larger to consume energy, and is gradually replaced by continuous catalysis polymerization (us3507890, us4069235) later.This continuously urges
Changing polymerization technique is that catalyst is made a certain size granule, and loads in fixed bed reactors.This process catalyst needs
Make the granule of certain particle diameter, and load in reactor, operation is more complicated, and dimeric dibasic acid product yield is low.
Content of the invention
One purpose of the application is exactly directed to the shortcoming that above-mentioned production technology exists, and has invented a kind of continuous production dimerization
The method of acid.The method is simple to operate, and power consumption is low, and catalyst can repeat to recycle.
Further object is to provide a kind of production equipment of polyreaction, is especially suitable for implementing side of the present invention
The production equipment of method.
This application provides a kind of continuous method producing dimeric dibasic acid, it comprises the following steps:
A. unsaturated fatty acid is mixed with catalyst, vacuum outgass；
B. make the mixture in a step enter in continuous reaction system to be reacted；
C. the product obtaining after reaction is carried out acidifying and filtration treatment to obtain dimeric dibasic acid crude product；
D. described dimeric dibasic acid crude product is purified,
Wherein said continuous reaction system includes at least two groups consersion units, and described consersion unit includes charging aperture, anti-
Answer device and discharging opening, first group of consersion unit is used for preheating material；Second group of consersion unit is reaction generator, and described two groups anti-
Equipment is answered to pass through charging aperture and discharging opening connection；Preferably, also include the 3rd group of consersion unit, it is used for being incubated.
Preferably, in certain embodiments of the present invention, adding in the mixture of step a has 0-5% percentage by weight
Water.
In some embodiments, the temperature of described first, second, and third group of consersion unit be respectively 100-220 DEG C,
220-280 DEG C and 220-255 DEG C.
In some embodiments, the flow velocity that raw material flows through described continuous reaction system is 0.5-2.5 ton/h, preferably
1.0-1.5 ton/h.
In some preferred embodiments, methods described is additionally included in the unsaturated fatty acid after degassing and catalyst
Mixture enter continuous reaction system before, be equipped with about 0-5%(percentage by weight) water step.
The application further relates to the dimerization acid product obtaining using said method, and its color and luster drops to 6(fe-co) below, not soap
Compound content is down to less than 1%.
The application further provides a kind of production equipment of polyreaction, comprising:
Continuous reaction system, filter, centrifuge and distilling apparatus, wherein said continuous reaction system is sequentially connected
Described filter, described centrifuge and described distilling apparatus, wherein, described continuous reaction system includes at least two groups reactions and sets
Standby, described consersion unit includes charging aperture, reactor and discharging opening, and first group of consersion unit is used for preheating material；Second group anti-
Equipment is answered to be reaction generator；Preferably, also include the 3rd group of consersion unit, it is used for being incubated.
In some embodiments of the present invention, the consersion unit of use includes at least one pipeline reactor, preferably
Horizontal pipeline reactor.It is preferably provided with agitator in described pipeline reactor.Described agitator is conventional in the art setting
Standby, its non-limitative example includes: gate stirrer, dasher, spiral agitator, turbine type agitator, rotary propeller type
Agitator, anchor agitator etc..Preferably, gate stirrer or anchor agitator are adopted in the pipeline reactor in the present invention.
The present processes create less than one or more beneficial technique effect compared to existing technology:
(1) employ the continuation method that continuous reaction system prepares dimeric dibasic acid, polyreaction all exists from start to end
Carry out in airtight response system, prevented the contact that raw material is with air, decrease air and the oxidation of unsaturated fatty acid is divided
Solution, reduces the color and luster of product, and the dimeric dibasic acid product color preparing can drop to 6(fe-co) below；
(2) employ the continuation method that continuous reaction system prepares dimeric dibasic acid, the temperature of response system, pressure all can be steady
Fixed control, considerably reduces temperature, pressure change product quality caused greatly in dimeric dibasic acid intermittent reaction method method
The factors of instability, improve the stability of product quality, and impurity content substantially reduces, and unsaponifiable matter content is down to less than 1%；
(3) prepared in the continuation method of dimeric dibasic acid using continuous reaction system, it is to avoid intermittent reaction method produces
During every batch of material will heat up the brought energy loss of cooling；Unsaturated fatty acid is exothermic reaction in polymerization simultaneously,
The reaction heat producing do not need to lower the temperature sustainable heated to cold material, greatly reduce and produce the energy of dimeric dibasic acid and disappear
Consumption.Be computed, compared with batch polymerization processes, this technique often process one ton of cottonseed oil fatty acid can save 60 tons of standard coals and
30 degree of electricity；
(4) compared with batch polymerization processes and fixed bed continuous catalysis polymerization technique, it not only increases unsaturated fatty acidss
The conversion ratio of acid and the yield of dimeric dibasic acid, also improve dimeric content in product.This technique employs continuous reaction system
System, is enable unsaturated fatty acid more effectively to be contacted with catalyst, improves the conversion that unsaturated fatty acid aggregates into dimeric dibasic acid
Rate, reaches 68.78%；This continuous producing method also reduces the usage amount of catalyst simultaneously, reduces unsaturated fatty acid poly-
Loss during conjunction, improves the yield of dimerization acid product, can reach 76.01%.This technique is by dimerization acid product simultaneously
Dimeric content brings up to 86.88%.
The equipment hinge structure of the present invention creates one or more technique effect beneficial as follows:
(1) feed stock conversion is high, and product yield is high, and catalyst amount is few.Employ continuous reaction system, make reactant
Can more effectively be fully contacted with catalyst, reaction efficiency increases substantially, improve the conversion ratio of polyreaction, in the present invention
Specific embodiments in, the conversion ratio of dimeric dibasic acid reaches 68.78%, and reduces the usage amount of catalyst.With employing by kettle
The production equipment of formula reactor or fixed bed reactors composition is compared, and conversion ratio and yield are all improved largely.
(2) steady quality.Material successive reaction in continuous reaction system, it is very steady that temperature, pressure can control
Fixed, considerably reduce the unstable product quality factor caused greatly of temperature, pressure change in dimeric dibasic acid intermittent reaction, carry
The high stability of product quality, impurity content substantially reduces, in specific embodiments of the present invention, the dimerization for preparing
The unsaponifiable matter content of acid is down to less than 1%.
(3) lighter color.Due to employing continuous reaction system, react all airtight to end from starting polyreaction
Carry out in reaction system, so that having prevented the contact that raw material is with air in high temperature polymerization course of reaction, decreasing air to former
The color and luster of dimerization acid product, in specific embodiments of the present invention, can be dropped to 6(fe-co by the oxidation Decomposition of material) below.
(4) consume energy less.Using continuous reaction system, it is to avoid in intermittent reaction method production process, every batch of material will
Heat up the unnecessary process of cooling, and raw material is exothermic reaction in polymerization, the reaction heat of generation do not need to lower the temperature sustainable to cold
Material heated, significantly reduce the energy resource consumption of production.In specific embodiments of the present invention, it is computed, with
Tank reactor is compared, and this equipment is often processed one ton of Oleic acid and can be saved 60 tons of standard coals and 30 degree of electricity.
Brief description
Fig. 1 shows the dimeric dibasic acid continuous production processes flow chart of an embodiment of the application.
Fig. 2 shows the block diagram of the polyreaction production equipment of an embodiment of the application.
Fig. 3 shows the structure chart of the continuous reaction system of an embodiment of the application, and it is set by three groups of reactions
Standby composition, wherein every group of consersion unit includes charging aperture, internal three end to end pipe reactions being provided with gate stirrer
Device and discharging opening, are connected by pipeline between every group of consersion unit, and every group of consersion unit also includes at least one Stress control
Device, is represented with pr, and each pipeline reactor also includes at least one temperature controller, is represented with tic.
Specific embodiment
This application provides a kind of continuous method producing dimeric dibasic acid, it comprises the following steps:
A. unsaturated fatty acid is mixed with catalyst, vacuum outgass；
B. make the mixture in a step enter in continuous reaction system to be reacted；
C. the product obtaining after reaction is carried out acidifying and filtration treatment to obtain dimeric dibasic acid crude product；
D. described dimeric dibasic acid crude product is purified,
Wherein said continuous reaction system includes at least two groups consersion units, and described consersion unit includes charging aperture, anti-
Answer device and discharging opening, first group of consersion unit is used for preheating material；Second group of consersion unit is reaction generator；Preferably, also
Including the 3rd group of consersion unit, it is used for being incubated.
In some embodiments, the consersion unit of the application includes at least one pipeline reactor, and pipeline reactor is excellent
Elect horizontal pipeline reactor as.It is preferably provided with agitator in described pipeline reactor.Described agitator is conventional in the art
Equipment, its non-limitative example includes: gate stirrer, dasher, spiral agitator, turbine type agitator, rotation oar
Formula agitator, anchor agitator etc..Preferably, gate stirrer or anchor agitator are adopted in the present invention.Using frame type stirring
When device or anchor agitator, blade outer rim shape is consistent with pipeline reactor inwall, leaves the gap of very little therebetween, and this can remove
The viscous reaction product being attached on cell wall or the solidss (as catalyst) being piled up in bottom land, keep good reactive state, and
And make reactor have more preferable heat-transfer effect.Additionally, for the heterogeneous catalysis adopting in the present invention, can be made it anti-
Answer and disperse in liquid evenly, to improve its reactivity, make the conversion ratio of raw material higher.
In particular embodiments, as shown in figure 1, described continuous reaction system includes three groups of consersion units, will not
After satisfied fatty acid is mixed homogeneously by a certain percentage with catalyst, carry out vacuum outgass, be preferably equipped with a certain amount of water again, enter
Reacted in the pipeline reactor (internal setting gate stirrer) of consersion unit.Acidified and filtration treatment obtains dimerization
Sour crude product, then obtain final dimerization acid product through washing, centrifugation and molecular distillation.
In some embodiments, the temperature of described first, second, and third group of consersion unit be respectively 100-220 DEG C,
220-280 DEG C and 220-255 DEG C.
It will be appreciated by persons skilled in the art that first group of consersion unit is mainly used in raw material is preheated, therefore,
As long as being capable of preheating, and the temperature that raw material reacts in a large number will not be made to be all optional.In second group of consersion unit
It is substantially carried out being polymerized the reaction generating dimeric dibasic acid, when only two groups of consersion units it is possible to realize continuous production dimeric dibasic acid, can
To adjust the charging rate of material, reaction raw materials consersion unit in reactor is made to have the enough response time.Preferably, permissible
Connect the 3rd group of consersion unit after second group of consersion unit, be mainly used in being incubated, be in order that polyreaction carries out more
Fully, the product mixtures in second group of consersion unit are made further to be converted.3rd group of consersion unit is at second group
Continue reaction, slightly below the temperature of reaction temperature is all optional on the basis of compositionss in consersion unit.Therefore include three
During the consersion unit of group or more than three groups, its reaction efficiency is higher, it is possible to achieve the effect that F.F. goes out soon, for large-scale production
Advantageously.
In some embodiments, the temperature of described first, second, and third group of consersion unit be respectively 130-210 DEG C,
245-255 DEG C and 240-250 DEG C.
In some embodiments, the flow velocity that raw material flows through described continuous reaction system is 0.5-2.5 ton/h, preferably
1.0-1.5 ton/h, the pressure energy of whole reaction system maintains 0.1-2mpa, preferably 0.1-0.8mpa, more preferably 0.2-
0.4mpa.
The disposal ability of the reaction method of the application, that is, the flow velocity of reactant is depending on reactor in continuous reaction system
Size, and also depend on the quantity of reactor.Reactor size such as internal diameter is bigger, in other factorses identical situation
Under, then the flow velocity of reactant can be bigger.The quantity of the reactor of series connection is more, then the time experiencing each reactor can be relatively
Shorter, can correspondingly improve the disposal ability of reaction raw materials.
In some embodiments of the application, in described reaction system, it is added without extra water.Preferably, real at some
Apply in scheme, the pressure of described reaction system is adjusted by adding the water of the 0-5% percentage by weight of raw material, when 213 DEG C
Water saturation vapour pressure is 2mpa, and when the temperature increases, pressure can be higher.It will be apparent to those skilled in the art that the side in the present invention
In method, add water and the pressure in reaction system can be made to maintain higher level, when not adding water, pressure can maintain relatively low water
Flat, the reaction pressure in reaction system can be improved when the water adding is more.In the catalyst being added, can exist a small amount of
Water of crystallization, therefore its effect are equivalent to and add a small amount of water.When extra addition water in the reaction system of the application, can lead to
Over-pressed force controller (as automatic limiting valve) carries out the control of pressure, makes the pressure energy of whole reaction system maintain 0.1-
2mpa, preferably 0.1-0.8mpa, more preferably 0.2-0.4mpa.Wherein pressure controller (as automatic limiting valve) is in prior art
Conventional device, can combine here by quoting the prior art of correlation.
In some embodiments, described continuous reaction system includes three groups of consersion units, and every group of consersion unit is by 1-6
Individual reactor composition, preferably 2-4 reactor composition, more preferably 3 reactors.Described reactor is preferably pipe reaction
Device, more preferably horizontal pipeline reactor.It is preferably provided with agitator inside pipeline reactor to be used for stirring.
In some embodiments, by washing, centrifugation and distillation, the dimeric dibasic acid crude product obtaining in step (c) is carried out
Purification.
In some embodiments, unsaturated fatty acid is the unsaturated fatty acid of 3-22 carbon atom composition, preferably
The unsaturated fatty acid of 12-21 carbon atom composition, the unsaturated fatty acid of more preferably 16-20 carbon atom, most preferably contain
The unsaturated fatty acid of 18 carbon atoms.Described unsaturated fatty acid, can contain one and more than one unsaturated double-bond,
Preferably comprise the unsaturated fatty acid of three or less than three unsaturated double-bonds.
In some embodiments, unsaturated fatty acid be palmitoleic acid, Oleic acid, linoleic acid, linolenic acid or other multiple
The mixture of unsaturated fatty acid.In some embodiments, the unsaturated fatty acid in the present invention can be hydrolyzing plant oil
The mixture rich in unsaturated fatty acid obtaining, for example, can be the hydrolyzate selected from one or more of vegetable oil:
Oleum Gossypii semen, soybean oil, Oleum Verniciae fordii, Petiolus Trachycarpi oil, Oleum Ricini, Testa oryzae oil, tall oil, Semen Lini oil, Oleum Brassicae campestriss, Oleum Helianthi, Semen arachidis hypogaeae
Oily Flos Carthami oil.
In some embodiments, methods described is additionally included in the mixing of the unsaturated fatty acid after degassing and catalyst
Before thing enters reactor, it is equipped with 0-5%, preferably 0.01-4%, more preferably 0.1-3%, most preferably 0.3-0.5%(weight
Percentage ratio) water step.The purposes of water is that donor system provides a normal pressure, makes the pressure energy of reaction system maintain 0.1-
Between 2mpa；The presence of water can suppress the decarboxylic reaction of unsaturated fatty acid, improve product quality simultaneously.
In some embodiments, the raw material used by acidification is mineral acid, such as phosphoric acid, hydrochloric acid, dilute sulfuric acid or it is mixed
Compound, consumption is the 1%-10% of unsaturated fatty acid quality, adds mineral acid to be to add in reaction system to remove and generate
Alkaline matter, make reaction system become alkalescence, neutral or acid.
In some embodiments, catalyst includes major catalyst and cocatalyst, and described major catalyst is hargil, is selected from
Neutral clay, Emathlite and/or alkaline hargil, described cocatalyst is alkaline matter.The neutrality that wherein major catalyst adopts
Hargil, Emathlite and alkaline hargil are the conventional catalysts prepared in dimeric dibasic acid, such as authorize in us3412039(1968),
Us3157681(1964 authorizes) and its patent quoted in point out that neutral clay, Emathlite and alkaline hargil can conducts
Prepare the catalyst of dimeric dibasic acid.During preparing dimeric dibasic acid, described alkaline matter is conventional selection in the art, such as
Cn10137636, us2955121, " synthesis of dimeric dibasic acid and commercial Application " (Zhang Shulin, Speciality Petrochemicals, nineteen ninety-five the 6th
Phase, 71-75 page) in described alkaline matter, its nonrestrictive example includes potassium hydroxide, calcium oxide, Barium monoxide, hydrogen-oxygen
Change calcium, magnesium hydroxide, Lithium hydrate, sodium hydroxide, barium hydroxide, potassium carbonate, lithium carbonate, sodium carbonate, sodium sulfate, magnesium chloride
Deng.The consumption of described major catalyst is the 7-25% of fatty acid wt, preferably 8-15%, and the consumption of alkaline matter is fatty acid weight
The 0.1-3% of amount, preferably 0.2-1%, more preferably 0.25%-1%, most preferably 0.25%-0.3%.
In some embodiments, filter and be divided into coarse filtration and two processes of fine straining, temperature controlling range is 40-100 DEG C.Cross
Catalyst is separated by filter with product, the catalyst being filtrated to get, recoverable after high temperature washing, reduces production cost,
To be realized using conventional pressure filter in the present invention, for example wherein coarse filtration can be realized using filter press, and fine straining can be adopted
Realized with bag type filtering machine.
In some embodiments, the color and luster of the dimerization acid product being prepared by as above method drops to 6(fe-co) with
Under, unsaponifiable matter content is down to less than 1%.
Present invention also provides using the dimerization acid product of the present processes acquisition, its color and luster drops to 6(fe-co) with
Under, unsaponifiable matter content is down to less than 1%.
Present invention also provides a kind of production equipment of polyreaction, described equipment includes: continuous reaction system, filtration
Machine, centrifuge and distillation equipment, wherein continuous reaction system connect filter, and filter connects centrifuge, and centrifuge connects
Distillation equipment, wherein, continuous reaction system includes at least two groups consersion units, and first group of consersion unit is used for preheating material；
Second group of consersion unit is reaction generator；Preferably, the 3rd group of consersion unit can also be included, it is used for being incubated.Described mistake
Filter all can be able to be adopted for various pressure filter known in the art, the equipment being capable of solid-liquid separation in prior art
With.Centrifuge is using conventional centrifugation apparatus.
In some embodiments, described production equipment also includes Scattered Kettle, mixing kettle, gassing tank and kettle to be filtered, wherein
Scattered Kettle connects mixing kettle, and mixing kettle connects gassing tank, and gassing tank connects continuous reaction system, and continuous reaction system connects
Kettle to be filtered, kettle to be filtered connects filter.Wherein Scattered Kettle, mixing kettle are conventional mixing arrangement, and Scattered Kettle can be by raw material in kettle
Inside sufficiently mixed, mixing kettle has good storge quality, uniform reaction raw materials can be made relief area, be continuously added into
To in continuous reaction system, reaction is enable continuously to carry out.Gassing tank can be using vacuum system by mixture system
Air is extracted out.Air-out, can select the reactor with vacuum.
In some embodiments, the filter of described equipment includes coarse filtration machine and strainer, and strainer and coarse filtration machine can
Selected from filter press and bag type filtering machine, they are applied in combination can make product and catalyst preferably separate.Art technology
Personnel are appreciated that being capable of product all conventional filter plants detached with catalyst is used equally to the application.
In some embodiments, described production equipment is used for producing dimeric dibasic acid.
In some embodiments, carry out polyreaction using the equipment of the application, it includes adding raw material and catalyst
Enter in Scattered Kettle fully dispersed, enter back in mixing kettle and mix further, mixed material enters gassing tank removing air,
Then it is equipped with certain water and enters continuous reaction system, reaction enters kettle to be filtered after terminating and is acidified, then sequentially pass through thick
Filter and strainer are filtered, and are washed subsequently into centrifuge and separate, and finally enter distillation equipment and carry out distillation point
From.
In the embodiment using the application device aggregation dimeric dibasic acid, it comprises the following steps: by raw material unsaturated lipid
Fat acid and catalyst are added in Scattered Kettle and are uniformly dispersed, and enter back in mixing kettle and mix further, and mixed material enters
Gassing tank vacuum removal air, is then equipped with first group of reaction that a certain amount of water sequentially enters in continuous reaction system and sets
Standby, second group of consersion unit and the 3rd group of consersion unit, finally enter kettle to be filtered and are acidified with phosphoric acid, the product after acidifying according to
Secondary filtered through coarse filtration machine and strainer, enter back into centrifuge and washed and separate, finally enter distillation equipment and carry out
Separated, detached product respectively enters mono-acid storage tank, dimerization acid storage tank and trimerization acid storage tank.Described kettle to be filtered is conventional
There is the reactor of agitating function, be used for acidified reaction mixture in this application, be also referred to as acidified kettle.
For the ease of skilled artisan understands that invention disclosed in the present application, with reference to embodiment the present invention is made into
One step description, its purpose is only that and more fully understands present disclosure it will be appreciated that present disclosure should not be limited to reality
Apply the scope of example, protection scope of the present invention is determined by the scope of the appended claims.
Embodiment
Raw material of fatty acid in following embodiments is the mixture of multiple fatty acids, from commercially available.According to source, will
The raw material of fatty acid wherein used correspondingly is referred to as cottonseed oil fatty acid (Jiangxi Province Yichun Yuanda Chemical Industry Co., Ltd.), Semen sojae atricolor
(benefit sea (Lianyun Harbour) oiling industry is limited for fatty acid oil (Yihai (Lianyungang) Oleochemical Industries Co., Ltd.), bean rape oil fatty acid
Company), its concrete composition see table:
Note: as c18-1 refers to containing 18 carbon atoms, and the Oleic acid containing a unsaturated double-bond；C18-2 refers to contain
There are 18 carbon atoms, the linoleic acid of two unsaturated double-bonds；Remaining defines according to this analogizes.
Additionally, it is as follows to some content introductions being related in following examples.
Horizontal pipeline reactor: the length of single reactor is 4500mm, internal diameter 490mm.Each reactor is provided with temperature
Degree controller, each horizontal pipeline inside reactor is provided with gate stirrer, every group of consersion unit is provided with a pressure control
Device processed.
The continuous reaction system that embodiment 7 adopts is made up of two groups of consersion units, and every group of consersion unit includes three head
The horizontal pipeline reactor that tail is connected, embodiment in addition, all using three groups of consersion units, every group of consersion unit is by three
End to end horizontal pipeline reactor composition.Scattered Kettle, mixing kettle and gassing tank are sequentially connected rear and continuous reaction system
Connect.Kettle to be filtered (or acidifying kettle) is connected, (coarse filtration machine is filter press to connect thereafter filtration system after continuous reaction system
Machine, Hangzhou Xingyuan Filter Technology Co., Ltd., model xmgz80/1000-uk；Strainer refers to bag type filtering machine, Jiangsu
Ju Neng Machinery Co., Ltd., model dl-4p2s).Other structures as shown in Fig. 2 be sequentially connected centrifuge, dimeric dibasic acid holding vessel and
Molecular distillation equipment.
In each example, the amount of the phosphoric acid adding at the end of reaction is the unsaturated fatty acid weight that added
2.5%.
The method of molecular distillation is: first carries out thin film evaporation using 190-200 DEG C and separates low-boiling point material, then carries out one-level
Short-path distillation (240 DEG C and 5pa), secondary distillation (t=280 DEG C and p=3pa) separates mono-acid, and finally condensation obtains the dimerization of purification
Acid product.
Dimeric conversion ratio is dimeric weight ratio in crude product.
Yield is the ratio of the dimerization acid product and unsaturated acids raw material obtaining.
Product color is detected using standard gb/t1722-92.
Dimerization acid content is detected using hplc.
Saponification number is detected using reference standard aocs tl1a-64 method.
Non-saponifiable matter detection is detected using reference standard aocs tk1a-64 method.
Embodiment 1
4 tons of cottonseed oil fatty acids, 480kg Emathlite and 12kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.3%(percentage by weight) water, entered with the flow velocity of 1.2 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-190 DEG C (in first group of consersion unit, the temperature of first reactor is 130 DEG C, and the temperature of second reactor is 160
DEG C, the temperature of the 3rd reactor is 190 DEG C), the temperature of second group of consersion unit is 245 DEG C, the temperature of the 3rd group of consersion unit
Spend for 240 DEG C, whole polymerization system pressure is 0.2mpa.React the product that obtains and enter in acidifying kettle, acidified after, send
To filtration system, product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity is 1050mpa.s/25 DEG C, Oleum Gossypii semen
The conversion ratio of fatty acid polyglycol dimer synthon is 63.45%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization
Acid product.Products obtained therefrom color and luster is 5.5(fe-co), yield is 70.94%, and dimer content is 83.06%, and saponification number is
195.5mg koh/g, unsaponifiable matter content is 0.94%.
Embodiment 2
4 tons of soya fatty acids, 480kg Emathlite and 12kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.4%(percentage by weight) water, entered with the flow velocity of 1.0 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-190 DEG C (with embodiment 1), the temperature of second group of consersion unit is 245 DEG C, and the temperature of the 3rd group of consersion unit is 240 DEG C,
Whole polymerization system pressure is 0.25mpa.React the product that obtains and enter in acidifying kettle, acidified after, deliver to filtration system
In system, product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity is 1270mpa.s/25 DEG C, soya fatty acid gathers
The conversion ratio of dimer synthon is 67.61%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization acid product.
Products obtained therefrom color and luster is 6.0(fe-co), yield is 74.58%, and dimer content is 84.79%, and saponification number is 197.1mg koh/
G, unsaponifiable matter content is 0.88%.
Embodiment 3
5 tons of cottonseed oil fatty acids, 600kg Emathlite and 15kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.3%(percentage by weight) water, entered with the flow velocity of 1.5 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-210 DEG C (in first group of consersion unit, the temperature of first reactor is 130 DEG C, and the temperature of second reactor is 170
DEG C, the temperature of the 3rd reactor is 210 DEG C), the temperature of second group of consersion unit is 255 DEG C, the temperature of the 3rd group of consersion unit
Spend for 250 DEG C, whole polymerization system pressure is 0.2mpa.React the product that obtains and enter in acidifying kettle, acidified after, send
To filtration system, product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity is 1028mpa.s/25 DEG C, Oleum Gossypii semen
The conversion ratio of fatty acid polyglycol dimer synthon is 63.23%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization
Acid product.Products obtained therefrom color and luster is 6.0(fe-co), yield is 71.01%, and dimer content is 82.57%, and saponification number is
194.2mg koh/g, unsaponifiable matter content is 0.99%.
Embodiment 4
5 tons of soya fatty acids, 600kg Emathlite and 15kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.5%(percentage by weight) water, entered with the flow velocity of 1.5 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-200 DEG C (with embodiment 3), the temperature of second group of consersion unit is 245 DEG C, and the temperature of the 3rd group of consersion unit is 240 DEG C,
Whole polymerization system pressure is 0.3mpa.React the product that obtains and enter in acidifying kettle, acidified after, deliver to filtration system
Middle product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity be 1280mpa.s/25 DEG C, soya fatty acid be polymerized
Dimeric conversion ratio is become to be 67.83%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization acid product.Institute
Obtaining product color is 6.0(fe-co), yield is 75.09%, and dimer content is 85.15%, and saponification number is 197.8mg koh/g,
Unsaponifiable matter content is 0.83%.
Embodiment 5
5 tons of soya fatty acids, 500kg Emathlite and 14kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.3%(percentage by weight) water, entered with the flow velocity of 1.2 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-200 DEG C (in first group of consersion unit, the temperature of first reactor is 130 DEG C, and the temperature of second reactor is 160
DEG C, the temperature of the 3rd reactor is 200 DEG C), the temperature of second group of consersion unit is 245 DEG C, the temperature of the 3rd group of consersion unit
Spend for 240 DEG C, whole polymerization system pressure is 0.2mpa.React the product that obtains and enter in acidifying kettle, acidified after, send
To filtration system, product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity is 1325mpa.s/25 DEG C, soybean oil
The conversion ratio of fatty acid polyglycol dimer synthon is 68.78%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization
Acid product.Products obtained therefrom color and luster is 6.5(fe-co), yield is 76.34%, and dimer content is 86.88%, and saponification number is
198.6mg koh/g, unsaponifiable matter content is 0.79%.
Embodiment 6
4 tons of bean rape oil fatty acids, 400kg Emathlite and 10kg lithium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.35%(percentage by weight) water, entered with the flow velocity of 1.4 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-200 DEG C (in first group of consersion unit, the temperature of first reactor is 130 DEG C, and the temperature of second reactor is 160
DEG C, the temperature of the 3rd reactor is 200 DEG C), the temperature of second group of consersion unit is 250 DEG C, the temperature of the 3rd group of consersion unit
Spend for 245 DEG C, whole polymerization system pressure is 0.25mpa.React the product that obtains and enter in acidifying kettle, acidified after,
Deliver in filtration system and product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity is 1147mpa.s/25 DEG C, bean dish
It is 65.01% that fatty acid oil aggregates into dimeric conversion ratio.Through deionized water wash, centrifugation and molecular distillation after, obtain two
Polyacids product.Products obtained therefrom color and luster is 5.5(fe-co), yield is 72.12%, and dimer content is 83.92%, and saponification number is
195.8mg koh/g, unsaponifiable matter content is 0.91%.
Embodiment 7
Using two groups of consersion units, one group is used for preheating, one group be used for polyreaction, by 4 tons of soya fatty acids,
480kg Emathlite and 12kg lithium carbonate are put in Scattered Kettle and are mixed, and after mix homogeneously, enter removing in gassing tank empty
Gas, is then equipped with 4%(percentage by weight) water, with 0.7 ton/h enter continuous reaction system in carry out successive reaction, wherein
The temperature of first group of consersion unit of described continuous reaction system is 130-200 DEG C of (three reactions of first group of consersion unit
The temperature of device is followed successively by 130 DEG C, 160 DEG C, 200 DEG C), the temperature of second group of consersion unit is 260 DEG C, whole polymerization system pressure
For 1.5mpa.React the product that obtains and enter in acidifying kettle, acidified after, deliver to product and catalyst in filtration system
Separate, obtain dimeric dibasic acid crude product, its viscosity is 1288mpa.s/25 DEG C, and soya fatty acid aggregates into dimeric conversion ratio
For 68.02%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization acid product.Products obtained therefrom color and luster is 6.0
(fe-co), yield is 75.23%, and dimer content is 85.08%, and saponification number is 196.2mg koh/g, and unsaponifiable matter content is
0.87%.
Embodiment 8
4 tons of cottonseed oil fatty acids, 600kg alkalescence hargil and 40kg sodium carbonate are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 3%(percentage by weight) water, entered even with the flow velocity of 1.4 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is 130- in continuous formula response system
150 DEG C (temperature of three reactors of first group of consersion unit is followed successively by 130 DEG C, 140 DEG C, 150 DEG C), second group of consersion unit
Temperature be 230 DEG C, the temperature of the 3rd group of consersion unit is 210 DEG C, and whole polymerization system pressure is 1.2mpa.Reaction obtains
Product enter acidifying kettle in, acidified after, deliver in filtration system and product separated with catalyst, obtain dimeric dibasic acid and slightly produce
Product, its viscosity is 929mpa.s/25 DEG C, and it is 60.23% that cottonseed oil fatty acid aggregates into dimeric conversion ratio.After through go from
Sub- water washing, centrifugation and molecular distillation, obtain dimerization acid product.Products obtained therefrom color and luster is 5.0(fe-co), yield is 69.38%,
Dimer content is 80.56%, and saponification number is 194.8mg koh/g, and unsaponifiable matter content is 0.82%.
Embodiment 9
4 tons of soya fatty acids, 400kg neutral clay and 10kg sodium hydroxide are put in Scattered Kettle and mixed, mixes
After closing uniformly, enter and in gassing tank, remove air, be then equipped with 1%(percentage by weight) water, entered with the flow velocity of 1.5 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
160-180 DEG C (temperature of three reactors is followed successively by 160 DEG C, 170 DEG C, 180 DEG C), the temperature of second group of consersion unit is 240
DEG C, the temperature of the 3rd group of consersion unit is 220 DEG C, and whole polymerization system pressure is 0.7mpa.React the product obtaining and enter acid
Change kettle in, acidified after, deliver in filtration system and product separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity
For 1098mpa.s/25 DEG C, it is 64.83% that soya fatty acid aggregates into dimeric conversion ratio.After through deionized water wash,
Centrifugation and molecular distillation, obtain dimerization acid product.Products obtained therefrom color and luster is 5.5(fe-co), yield is 71.38%, and dimer contains
Measure as 82.69%, saponification number is 196.9mg koh/g, unsaponifiable matter content is 0.93%.
Embodiment 10
5 tons of soya fatty acids, 600kg Emathlite and 15kg calcium oxide are put in Scattered Kettle and mixed, mixing
After uniformly, enter and in gassing tank, remove air, be then equipped with 0.8%(percentage by weight) water, entered with the flow velocity of 1.5 tons/h
Carry out successive reaction, the temperature of first group of consersion unit of wherein said continuous reaction system is in continuous reaction system
130-150 DEG C (with embodiment 8), the temperature of second group of consersion unit is 260 DEG C, and the temperature of the 3rd group of consersion unit is 240 DEG C,
Whole polymerization system pressure is 0.6mpa.React the product that obtains and enter in acidifying kettle, acidified after, deliver to filtration system
Middle product is separated with catalyst, obtain dimeric dibasic acid crude product, its viscosity be 1278mpa.s/25 DEG C, soya fatty acid be polymerized
Dimeric conversion ratio is become to be 67.99%.Through deionized water wash, centrifugation and molecular distillation after, obtain dimerization acid product.Institute
Obtaining product color is 6.0(fe-co), yield is 75.83%, and dimer content is 84.98%, and saponification number is 196.3mg koh/g,
Unsaponifiable matter content is 0.96%.
Embodiment 11 (intermittent reaction)
480kg Emathlite and 12kg lithium carbonate are added in reactor, be then equipped with 4 tons of cottonseed oil fatty acids and
0.3%(percentage by weight) water, after mix homogeneously, in reactor, logical nitrogen to remove air, heats up, controlling reaction temperature
At 240-250 DEG C, react three hours.The pressure controlling reactor in course of reaction is 0.3-0.4mpa.React the product obtaining
Enter acidifying kettle in, acidified after, deliver in filtration system and product separated with catalyst, obtain dimeric dibasic acid crude product,
Its viscosity is 890mpa.s/25 DEG C, and it is 58.63% that cottonseed oil fatty acid aggregates into dimeric conversion ratio.Through deionized water after
Washing, centrifugation and molecular distillation, obtain dimerization acid product.Products obtained therefrom color and luster is 7.5(fe-co), yield is 68.42%, dimerization
Body burden is 78.54%, and saponification number is 191.5mg koh/g, and unsaponifiable matter content is 1.24%.
Energy consumption comparison table:
Note: continuous way method (embodiment 1) and batch process (embodiment 11) are run 200 times, calculates continuous respectively
The amount of the averagely required coal of cottonseed oil fatty acid raw material per ton and electricity, the as number in energy consumption comparison in method and intermittent mode
According to.
The above, the only specific embodiment of the disclosure, but the protection domain of the disclosure is not limited thereto, and any
In technical scope disclosed by the disclosure for the those of ordinary skill in the art, any change that can expect without creative work
Change or replace, all should cover within the application scope of the claims.
Claims (39)
1. a kind of continuous method producing dimeric dibasic acid, comprises the following steps:
A. the unsaturated fatty acid of 3-22 carbon atom composition is mixed with catalyst, vacuum outgass；
B. make the mixture in step a enter in continuous reaction system to be reacted；
C. the product obtaining after reaction is carried out acidifying and filtration treatment to obtain dimeric dibasic acid crude product；And
D. described dimeric dibasic acid crude product is purified,
Wherein said continuous reaction system includes at least two groups consersion units, and it is anti-that described consersion unit includes charging aperture, pipeline
Answer device and discharging opening, first group of consersion unit is used for preheating material；Second group of consersion unit is reaction generator.
2. the method for claim 1, wherein said continuous reaction system also includes the 3rd group of consersion unit, and it is used for
Insulation.
3. the method for claim 1, wherein raw material flow through described continuous reaction system flow velocity be 0.5-2.5 ton/
H, the pressure energy of whole reaction system maintains 0.1-2mpa.
4. method as claimed in claim 3, wherein raw material flow through described continuous reaction system flow velocity be 1.0-1.5 ton/
h.
5. method as claimed in claim 3, the pressure energy of wherein whole reaction system maintains 0.1-0.8mpa.
6. method as claimed in claim 3, the pressure energy of wherein whole reaction system maintains 0.2-0.4mpa.
7. the method as any one of claim 1 to 6, the temperature of wherein said first group of consersion unit is 100-220
℃.
8. the method as any one of claim 1 to 6, the temperature of wherein said first group of consersion unit is 130-210
℃.
9. the method as any one of claim 1 to 6, the temperature of wherein said second group of consersion unit is 220-280
℃.
10. method as claimed in claim 9, the temperature of wherein said second group of consersion unit is 220-270 DEG C.
11. methods as claimed in claim 9, the temperature of wherein said second group of consersion unit is 245-255 DEG C.
12. methods as claimed in claim 2, the temperature of wherein said 3rd group of consersion unit is 220-255 DEG C.
13. methods as claimed in claim 12, the temperature of wherein said 3rd group of consersion unit is 240-250 DEG C.
14. methods as claimed in claim 1 or 2, wherein said continuous reaction system is only made up of three groups of consersion units.
15. methods as claimed in claim 1 or 2, wherein pass through washing, centrifugation and distillation to the dimerization obtaining in step (c)
Sour crude product is purified.
16. methods as claimed in claim 15, described unsaturated fatty acid is the unsaturated fatty acidss of 16-20 carbon atom composition
Acid.
17. methods as claimed in claim 15, described unsaturated fatty acid is the unsaturated fatty acid of 18 carbon atom compositions.
18. methods as claimed in claim 15, wherein said unsaturated fatty acid is palmitoleic acid, Oleic acid, linoleic acid, Caulis et Folium Lini
Acid or its combination in any.
19. methods as claimed in claim 15, wherein said unsaturated fatty acid is linoleic acid.
20. methods as any one of claim 1-6, wherein said catalyst includes major catalyst and cocatalyst,
Described major catalyst is hargil, and selected from neutral clay, Emathlite and alkaline hargil, described cocatalyst is alkaline matter.
21. methods as claimed in claim 20, wherein said alkaline matter is potassium hydroxide, magnesium chloride, calcium oxide, oxidation
Barium, lithium carbonate, sodium carbonate, sodium sulfate, potassium carbonate, Lithium hydrate, sodium hydroxide, calcium hydroxide, magnesium hydroxide or barium hydroxide.
22. methods as any one of claim 1-6, are wherein based on weight ratio meter and calculate, major catalyst consumption is insatiable hunger
With the 7-25% of fatty acid, cocatalyst consumption is the 0.1-3% of unsaturated fatty acid.
23. methods as claimed in claim 22, are wherein based on weight ratio meter and calculate, major catalyst consumption is unsaturated fatty acid
8-15%.
24. methods as claimed in claim 22, are wherein based on weight ratio meter and calculate, major catalyst consumption is unsaturated fatty acid
10-12%.
25. methods as claimed in claim 22, are wherein based on weight ratio meter and calculate, cocatalyst consumption is unsaturated fatty acid
0.2-1%.
26. methods as claimed in claim 22, are wherein based on weight ratio meter and calculate, cocatalyst consumption is unsaturated fatty acid
0.25-1%.
27. methods as any one of claim 1-6, wherein said method is additionally included in the mixture of step a and adds
Enter the water of 0-5% percentage by weight.
28. methods as claimed in claim 27, add 0.01-4% percentage by weight wherein in the mixture of step a
Water.
29. methods as claimed in claim 27, add the water of 0.1-3% percentage by weight wherein in the mixture of step a.
30. methods as claimed in claim 27, add 0.3-0.5% percentage by weight wherein in the mixture of step a
Water.
31. methods as any one of claim 1 to 6, the raw material used by wherein said acidification is mineral acid, choosing
From phosphoric acid, hydrochloric acid, dilute sulfuric acid or its mixing, consumption is the 1%-10% of unsaturated fatty acid quality.
32. methods as any one of claim 1 to 6, the color and luster of the dimerization acid product wherein preparing drops to
Below 6fe-co, and/or unsaponifiable matter content is down to less than 1%.
33. methods as any one of claim 1-6, wherein, described consersion unit includes at least one reactor, institute
Stating reactor is pipeline reactor, is provided with agitator inside described pipeline reactor.
34. methods as claimed in claim 33, wherein said reactor is horizontal pipeline reactor.
35. methods as claimed in claim 33, are provided with agitator inside wherein said pipeline reactor.
A kind of 36. production equipments of polyreaction, comprising:
Continuous reaction system, filter, centrifuge and distilling apparatus, wherein said four devices are sequentially connected, and wherein
Described continuous reaction system includes at least two groups consersion units, and described consersion unit includes charging aperture, pipeline reactor and goes out
Material mouth, first group of consersion unit is used for preheating material；Second group of consersion unit is reaction generator.
The production equipment of 37. polyreactions as claimed in claim 36, wherein said continuous reaction system also includes the 3rd
Group consersion unit, it is used for being incubated.
The production equipment of 38. polyreactions as described in claim 36 or 37, wherein said equipment is used for implementing claim 1
The method of described continuous production dimeric dibasic acid.
The production equipment of 39. polyreactions as described in claim 36 or 37, wherein said equipment also includes Scattered Kettle, mixing
Kettle, gassing tank and kettle to be filtered, wherein said Scattered Kettle is sequentially connected described mixing kettle, described gassing tank, described continuous reaction
System, described kettle to be filtered and described filter.
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| CN108579771A (en) * | 2018-03-23 | 2018-09-28 | 福州大学 | A kind of Catalyzed by Modified Bentonite agent of synthesis of dimmer acid |
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| CN201704238U (en) * | 2010-06-11 | 2011-01-12 | 九江力山环保科技有限公司 | Production equipment of dimer acid |
| CN103012110A (en) * | 2012-11-30 | 2013-04-03 | 江苏金马油脂科技发展有限公司 | Production method of dimer acid |
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| CN103012110A (en) * | 2012-11-30 | 2013-04-03 | 江苏金马油脂科技发展有限公司 | Production method of dimer acid |
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