CN106279473A - A kind of synthetic method of macromolecule boronation polyisobutylene succinamide - Google Patents
A kind of synthetic method of macromolecule boronation polyisobutylene succinamide Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
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Abstract
The synthetic method of a kind of macromolecule boronation polyisobutylene succinamide, under the conditions of uniform temperature, polyisobutylene and maleic anhydride carry out the hot addition reaction of block, generate polyisobutenyl succinic anhydride；Macromolecule polyisobutenyl succinic anhydride is reacted with polyamines polyene, generates polyisobutylene succinamide and water, steams the water of generation the most again through decompression, then carry out boronation with boric acid, obtain product.Advantage is: rational technology, and safety and environmental protection is easy and simple to handle, and maleic anhydride conversion rate is high, good product performance, is suitable for industrialized production.
Description
Technical field
The present invention relates to the synthetic method of a kind of macromolecule boronation polyisobutylene succinamide.
Background technology
Polyisobutylene succinamide (i.e. ashless dispersant) is a kind of broad-spectrum lube oil additive, excellent with it
Good oil-soluble, excellent low temperature dispersity solves the peace and quiet dispersion of metal mold insurmountable low temperature greasy filth scattering problem, with
Bright have High Temperature Disperse performance and good compatibility, adjustable with ZDDP and other additives makes various high-grade internal combustion engine
Oil, is one of host modulating top grade and the top I. C. engine oil in the world.Also it is widely used in the people's quick-fried emulsion industry simultaneously.In
Between product alkene acid anhydride be also the raw material of other chemical products.
The different polyisobutylene succinamide of polyphosphazene polymer, except the oil soluble that holding polyisobutylene succinamide is excellent
Property, excellent low temperature dispersity, solve the peace and quiet dispersion of metal mold insurmountable low temperature greasy filth scattering problem, there is height simultaneously
Outside temperature dispersive property and good compatibility, the viscosity-temperature characteristics good with it and film strength, at home and abroad top-grade lubricating oil,
Particularly heavy-duty oil is used widely.
At present, macromolecule polyisobutylene succinamide is to utilize direct hot adduction technique under certain condition, makes to gather
Isobutene. and maleic anhydride hydrocarbonylation adduction obtain macromolecule polyisobutenyl succinic anhydride (being called for short alkene acid anhydride), and alkene acid anhydride is many with polyenoid again
Amine carries out aminating reaction, generates polyphosphazene polymer different polyisobutenyl imidodicarbonic diamide.The method have less demanding to consersion unit,
Course of reaction does not use the advantage that chlorine, chlorinity are low, but, the method is higher to the Active pharmaceutical of reaction raw materials, and gathers
Isobutene conversion is relatively low, and not exclusively, product yield is low in reaction.
Research shows, boron modification macromolecule polyisobutylene succinamide, can keep polyphosphazene polymer isobutenyl fourth
The original good characteristic of imidodicarbonic diamide, has again the detergent-dispersant additive of antibacterial abrasion resistance, and boric acid can be with the anaerobism in lubricating oil
Bacterium plays good resistancing action and extends the service life of lubricating oil, simultaneously boron molecule in lubricating oil with half glue spherical particle
Exist.In the reciprocating motion of piston, between piston ring casing wall, form the particle membrane of a kind of hemicolloid spherical particle, decrease
Piston direct friction to cylinder body at the volley serves wear-resistant effect.Simultaneously because hemicolloid spherical particle rolls changes work
Friction mode between plug and casing wall, is become multiple spot friction from original linear friction, decreases frictional resistance and the resistance of start,
Reach energy-saving and cost-reducing purpose.Therefore, boron modification type ashless dispersant macromolecule boronation polyisobutylene succinamide
Synthetic method is current primary study direction.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of rational technology, safety and environmental protection, and polyisobutenyl succinic acid
Acid anhydride conversion ratio is good, the synthetic method of the macromolecule boronation polyisobutylene succinamide that can use as lube oil additive.
The technical problem to be solved in the present invention is:
The synthetic method of a kind of macromolecule boronation polyisobutylene succinamide, it specifically comprises the following steps that
(1), block adduction
Under the conditions of uniform temperature, polyisobutylene and maleic anhydride carry out the hot addition reaction of block, generate polyisobutenyl fourth two
Anhydride；The polyphosphazene polymer isobutene. of 0.2mol is added in the four-hole bottle of band stirring, install cooling tube, then low by 0.1mol
The polyisobutenyl succinic anhydride of molecular weight adds in four-hole bottle as initiator, the polyisobutenyl fourth two of described low-molecular-weight
The molecular weight of acyl acid anhydride is 1000-1300, is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip 0.6mol in four-hole bottle
The maleic anhydride melted, time for adding maintains 3 hours-5 hours, after 30 minutes, by remaining 0.3mol polyphosphazene polymer
Isobutene. adds in bottle, and the molecular weight of described polyphosphazene polymer isobutene. is 2300-2500, maintains the temperature at 220 DEG C-230 DEG C, continues
Continuous being dripped by remaining maleic anhydride, maintain the temperature at 220 DEG C-230 DEG C after whole completion of dropwise addition, constant temperature 10 hours-12 is little
Time, obtain macromolecule polyisobutenyl succinic anhydride；
(2) amination
Macromolecule polyisobutenyl succinic anhydride is reacted with polyamines polyene, generates polyisobutylene succinamide and water, then
The water of generation is steamed again through decompression, then through being filtrated to get product；
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds base oil and is diluted, base oil addition Ying Yibao
Card product viscosity >=300 centistokes(cst), macromolecule polyisobutenyl succinic anhydride gross weight 3.0%-3.15% polyamines polyene is normal with accounting for
Pressure reaction, controls temperature and reacts 2 hours at 80 DEG C-140 DEG C, generate polyisobutylene succinamide and water, steam through decompression
Water outlet, filters, obtains polyisobutylene succinamide；
(3) boronation
By polyisobutylene succinamide, or the polyisobutylene succinamide refined without dehydration, carry out boron with boric acid
Change, steam water through decompression the most again, collect as recycle-water, then through filtering, obtain macromolecule boronation polyisobutenyl succinyl
Imines.
During boronation reaction, described polyisobutylene succinamide is 1:1-1:2 with the mol ratio of boric acid, and reaction temperature is
80 DEG C-140 DEG C response time are 2 hours.
Before carrying out boronation reaction, the recycle-water obtained with the reaction decompression distillation of step (3) boronation carries out soaking boric acid, described
Boric acid is 1:1 with the mass ratio of recycle-water, so that the polarity of boric acid is activated, boric acid conversion ratio can improve the biggest.
The free maleic anhydride content of sampling detection, acid number and viscosity, MA≤0.6%, acid number >=85KOHmg/g, viscosity >=
3500 centistokes(cst)s, the most qualified after turn amination.
Described polyamines polyene is diethylenetriamine, triethylene tetramine, TEPA or five hexamine.
During aminating reaction, reaction temperature is 120 DEG C-130 DEG C.
Described base oil is 150SN base oil.
Beneficial effects of the present invention:
(1) raw material is polyisobutylene, maleic anhydride and polyamines polyene, and raw material is easy to get, and manufacturer is numerous, and raw material sources are extensive；
(2) the hot addition reaction of block generates polyisobutenyl succinic anhydride, mainly by the polyisobutenyl fourth of low-molecular-weight
Two acyl acid anhydride end alkene molecules ripple alive, as initiator, promotes and the addition reaction of polyphosphazene polymer isobutene. with maleic anhydride, solves
Macromolecule polyisobutene molecular weight is big, and viscosity is big, and activity is low, is difficult to reaction, and material reaction is incomplete, muddy the asking of transparency
Topic；Maleic anhydride conversion rate is made to be greatly improved；
(3) easy and simple to handle, amination controls 80-140 DEG C after terminating, and the boric acid being slowly added to soak carries out boronation, under part reuse
Secondary immersion boric acid, the evaporation loss in remaining addition circulating water pool replenishment cycles pond, whole reaction need not use solvent or fat
Fat alcohol, solves other by the production waste gas of solvent or fatty alcohol, waste water, the problem that COD content is high.
Accompanying drawing explanation
Fig. 1 is to utilize the present invention (corresponding embodiment 4) block adduction and conventional method direct adduction synthesizing polyisobutylene base
The maleic anhydride synthetic ratio curve chart of succinic anhydride.
Detailed description of the invention
Embodiment
Material choice:
1, polyisobutylene (PIB)
A: density: 0.855-0.900g/cm3；
B: viscosity (100 DEG C) >=500 centistokes(cst)s；
C: molecular weight: 2300-2500；
D: flash-point >=160 DEG C；
E: moisture: 0.03%
F: outward appearance: water white, no suspended substance；
2, maleic anhydride
A: color: white；
B: outward appearance: crystalline solid (lamellar, spherical)；
C: purity (%) ＞ 98；
D: maleic content (%) ＜ 2.1；
E: fusing point DEG C ＞ 51.5；
3, polyamines polyene:
(1) triethylene tetramine (2) TEPA
A: density 0.975-0.995 0.985-1.00
B: colourity ＜ 0.5 ＜ 0.5
C: directly base number 1350-1450mgKOH/g 1250-1350mgKOH/g
D: purity (%) ＞ 97 ＞ 97
E: diethylenetriamine ＜ 2.0 ＜ 2.0
F: moisture content ＜ 1.50 ＜ 1.50
G: nitrogen content (%) 35-37 33-35
H: oil-soluble speckle is without precipitation nothing precipitation
4, base oil: 150SN base oil.
The synthetic method of macromolecule boronation polyisobutylene succinamide, it specifically comprises the following steps that
(1), block adduction
Under the conditions of uniform temperature, polyisobutylene and maleic anhydride carry out the hot addition reaction of block, generate polyisobutenyl fourth two
Anhydride；The polyphosphazene polymer isobutene. of 0.2mol is added in the four-hole bottle of band stirring, install cooling tube, then low by 0.1mol
The polyisobutenyl succinic anhydride of molecular weight adds in four-hole bottle as initiator, the polyisobutenyl fourth two of described low-molecular-weight
The molecular weight of acyl acid anhydride is 1000-1300, is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip 0.6mol in four-hole bottle
The maleic anhydride melted, time for adding maintains 3 hours-5 hours, after 30 minutes, by remaining 0.3mol polyphosphazene polymer
Isobutene. adds in bottle, and the molecular weight of described polyphosphazene polymer isobutene. is 2300-2500, maintains the temperature at 220 DEG C-230 DEG C, continues
Continuous being dripped by remaining maleic anhydride, maintain the temperature at 220 DEG C-230 DEG C after whole completion of dropwise addition, constant temperature 10 hours-12 is little
Time, obtain macromolecule polyisobutenyl succinic anhydride；The free maleic anhydride content of sampling detection, acid number and viscosity, MA≤
0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst)；Maleic anhydride synthetic ratio is 98.5%；
(2) amination
Macromolecule polyisobutenyl succinic anhydride is reacted with polyamines polyene, generates polyisobutylene succinamide and water, then
The water of generation is steamed again through decompression, then through being filtrated to get product；
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds 150SN base oil and is diluted, product viscosity >=300
Centistokes(cst), and accounts for macromolecule polyisobutenyl succinic anhydride gross weight 3.0%-3.15% polyamines polyene synthesis under normal pressure, described polyenoid
Polyamines is diethylenetriamine, triethylene tetramine, TEPA or five hexamine；Control temperature to react at 80 DEG C-140 DEG C
2 hours, reaction temperature preferably 120 DEG C-130 DEG C, generate polyisobutylene succinamide and water, steam water through decompression, filter,
Obtain polyisobutylene succinamide；
(3) boronation
The recycle-water obtained with boronation reaction decompression distillation carries out soaking boric acid, and described boric acid is 1:1 with the mass ratio of recycle-water,
So that the polarity of boric acid is activated, boric acid conversion ratio can improve the biggest；
By polyisobutylene succinamide, or the polyisobutylene succinamide refined without dehydration, soak with recycle-water
Boric acid 80 DEG C-140 DEG C carry out boronation react 2 hours, described polyisobutylene succinamide with the mol ratio of boric acid is
1:1-1:2, steams water through decompression the most again, collects as recycle-water, and next time is soaked boric acid in part reuse, and remaining adds recirculated water
The evaporation loss in replenishment cycles pond, pond, then through filtering, obtain macromolecule boronation polyisobutylene succinamide.
Embodiment 1
(1), block adduction
The polyphosphazene polymer isobutene. that 0.2mol molecular weight is 2300-2500 is added in the four-hole bottle of band stirring, install cooling
Pipe, then the polyisobutenyl succinic anhydride of the low-molecular-weight that 0.1mol molecular weight is 1000-1300 is added four as initiator
In mouth bottle, it is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip the maleic acid melted of 0.6mol in four-hole bottle
Acid anhydride, time for adding maintains 5 hours, after 30 minutes, by the polyphosphazene polymer isobutene. that residue 0.3mol molecular weight is 2300-2500
Add in bottle, maintain the temperature at 220 DEG C-230 DEG C, continue to drip remaining maleic anhydride, keep after whole completion of dropwise addition
Temperature at 220 DEG C-230 DEG C, constant temperature 12 hours, obtain macromolecule polyisobutenyl succinic anhydride；The free maleic acid of sampling detection
Acid anhydride content, acid number and viscosity, MA (free maleic anhydride content)≤0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst)；
Maleic anhydride synthetic ratio is 98.5%；
(2) amination
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds 150SN base oil and is diluted, makes polyphosphazene polymer isobutyl
Enetutanedioic acid anhydride viscosity is 350 centistokes(cst)s, and macromolecule polyisobutenyl succinic anhydride weight 3.15% diethylenetriamine is normal with accounting for
Pressure reaction, controls temperature and reacts 2 hours at 120 DEG C-130 DEG C, generate polyisobutylene succinamide and water, steam through decompression
Water outlet, filters, obtains polyisobutylene succinamide；
(3) boronation
The recycle-water obtained with boronation reaction decompression distillation carries out soaking boric acid, and boric acid is 1:1 with the mass ratio of recycle-water；Will be poly-
The boric acid that isobutenyl succimide and recycle-water soak carries out boronation at 120 DEG C-130 DEG C and reacts 2 hours, described poly-isobutyl
Allyl butyrate imidodicarbonic diamide is 1:2 with the mol ratio of boric acid, steams water through decompression the most again, collects as recycle-water, then through filtering,
Obtain macromolecule boronation polyisobutylene succinamide.
Embodiment 2
(1), block adduction
The polyphosphazene polymer isobutene. that 0.2mol molecular weight is 2300-2500 is added in the four-hole bottle of band stirring, install cooling
Pipe, then the polyisobutenyl succinic anhydride of the low-molecular-weight that 0.1mol molecular weight is 1000-1300 is added four as initiator
In mouth bottle, it is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip the maleic acid melted of 0.6mol in four-hole bottle
Acid anhydride, time for adding maintains 4 hours, after 30 minutes, by the polyphosphazene polymer isobutene. that residue 0.3mol molecular weight is 2300-2500
Add in bottle, maintain the temperature at 220 DEG C-230 DEG C, continue to drip remaining maleic anhydride, keep after whole completion of dropwise addition
Temperature at 220 DEG C-230 DEG C, constant temperature 11 hours, obtain macromolecule polyisobutenyl succinic anhydride；The free maleic acid of sampling detection
Acid anhydride content, acid number and viscosity, MA≤0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst)；
(2) amination
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds 150SN base oil and is diluted to viscosity 300 centistokes(cst),
With account for macromolecule polyisobutenyl succinic anhydride gross weight 3.05% triethylene tetramine synthesis under normal pressure, control temperature 130 DEG C-
React 2 hours at 140 DEG C, generate polyisobutylene succinamide and water, steam water through decompression, filter, obtain polyisobutylene
Base succimide；
(3) boronation
The recycle-water obtained with boronation reaction decompression distillation carries out soaking boric acid, and boric acid is 1:1 with the mass ratio of recycle-water；Will be poly-
The boric acid that isobutenyl succimide and recycle-water soak carries out boronation at 130 DEG C-140 DEG C and reacts 2 hours, described poly-isobutyl
Allyl butyrate imidodicarbonic diamide is 1:1.5 with the mol ratio of boric acid, steams water through decompression the most again, collects as recycle-water, then passes through
Filter, obtains macromolecule boronation polyisobutylene succinamide.
Embodiment 3
(1), block adduction
The polyphosphazene polymer isobutene. that 0.2mol molecular weight is 2300-2500 is added in the four-hole bottle of band stirring, install cooling
Pipe, then the polyisobutenyl succinic anhydride of the low-molecular-weight that 0.1mol molecular weight is 1000-1300 is added four as initiator
In mouth bottle, it is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip the maleic acid melted of 0.6mol in four-hole bottle
Acid anhydride, time for adding maintains 4 hours, after 30 minutes, by the polyphosphazene polymer isobutyl that remaining 0.3mol molecular weight is 2300-2500
Alkene adds in bottle, maintains the temperature at 220 DEG C-230 DEG C, continues to drip remaining maleic anhydride, protects after whole completion of dropwise addition
Hold temperature at 220 DEG C-230 DEG C, constant temperature 11 hours, obtain macromolecule polyisobutenyl succinic anhydride；The free Malaysia of sampling detection
Anhydride content and acid number, viscosity, MA≤0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst)；Maleic anhydride synthetic ratio is
97.1%；
(2) amination
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds 150SN base oil and is diluted to viscosity 400 centistokes(cst),
With account for macromolecule polyisobutenyl succinic anhydride gross weight 3.0% TEPA synthesis under normal pressure, control temperature at 120 DEG C-130
React 2 hours at DEG C, generate polyisobutylene succinamide and water, steam water through decompression, filter, obtain polyisobutenyl fourth
Imidodicarbonic diamide；
(3) boronation
The recycle-water obtained with boronation reaction decompression distillation carries out soaking boric acid, and boric acid is 1:1 with the mass ratio of recycle-water；Will be poly-
Isobutenyl succimide, carries out boronation with the boric acid of recycle-water immersion at 120 DEG C-130 DEG C and reacts 2 hours, described poly-different
Cyclobutenyl succimide is 1:1 with the mol ratio of boric acid, steams water through decompression the most again, collects as recycle-water, then passes through
Filter, obtains macromolecule boronation polyisobutylene succinamide.
Embodiment 4
(1), block adduction
The polyphosphazene polymer isobutene. that 0.2mol molecular weight is 2300-2500 is added in the four-hole bottle of band stirring, install cooling
Pipe, then the polyisobutenyl succinic anhydride of the low-molecular-weight that 0.1mol molecular weight is 1000-1300 is added four as initiator
In mouth bottle, it is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip the maleic acid melted of 0.6mol in four-hole bottle
Acid anhydride, time for adding maintains 3 hours, after 30 minutes, by the polyphosphazene polymer isobutyl that remaining 0.3mol molecular weight is 2300-2500
Alkene adds in bottle, maintains the temperature at 220 DEG C-230 DEG C, continues to drip remaining maleic anhydride, protects after whole completion of dropwise addition
Hold temperature at 220 DEG C-230 DEG C, constant temperature 10 hours, obtain macromolecule polyisobutenyl succinic anhydride；The free Malaysia of sampling detection
Anhydride content and acid number, viscosity, MA≤0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst)；Maleic anhydride synthetic ratio is
98.3%；
(2) amination
Macromolecule polyisobutenyl succinic anhydride imports amination still, adds 150SN base oil and is diluted to viscosity 320 centistokes(cst),
With account for macromolecule polyisobutenyl succinic anhydride gross weight 3.0% 5 hexamine synthesis under normal pressure, control temperature at 80 DEG C-90 DEG C
Lower reaction 2 hours, generates polyisobutylene succinamide and water, steams water through decompression, filters, obtains polyisobutenyl fourth two
Acid imide；
(3) boronation
The recycle-water obtained with boronation reaction decompression distillation carries out soaking boric acid, and boric acid is 1:1 with the mass ratio of recycle-water；Will be poly-
The boric acid that isobutenyl succimide and recycle-water soak carries out boronation at 80 DEG C-90 DEG C and reacts 2 hours, described polyisobutylene
Base succimide is 1:1 with the mol ratio of boric acid, steams water through decompression the most again, collects as recycle-water, then through filtering,
To macromolecule boronation polyisobutylene succinamide.
The Testing index table of the macromolecule boronation polyisobutylene succinamide of table 1 embodiment of the present invention 1-embodiment 4
The Testing index table of the macromolecule polyisobutenyl succinic anhydride of table 2 embodiment of the present invention 1-embodiment 4
Table 3 domestic like product quality index
| Viscosity cst | Open flash point DEG C | Nitrogen content % | Boron contents % | Moisture % | Transparency | Total base number | |
| T161B | ≥300 | ≥170 | 1.0-1.0 | 0.35 | ≤0.3 | Transparent | 18.0-22.0 |
Actual production product uses proof in diesel engine oil CF-4, CH-4 and heavy-duty diesel engine automobile oil, can replace completely
For the similar additive of import, receive promising result.
These are only the specific embodiment of the present invention, be not limited to the present invention, for those skilled in the art
For Yuan, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a synthetic method for macromolecule boronation polyisobutylene succinamide, is characterized in that:
Specifically comprise the following steps that
(1), block adduction
The polyphosphazene polymer isobutene. of 0.2mol is added in four-hole bottle, then by the polyisobutenyl fourth two of the low-molecular-weight of 0.1mol
Acyl acid anhydride adds in four-hole bottle as initiator, and the molecular weight of the polyisobutenyl succinyl acid anhydride of described low-molecular-weight is 1000-
1300, it is warmed up to 220 DEG C simultaneously, after stirring 30 minutes, starts to drip the maleic anhydride melted of 0.6mol in four-hole bottle,
Time for adding maintains 3 hours-5 hours, after 30 minutes, is added by remaining 0.3mol polyphosphazene polymer isobutene. in bottle, described
The molecular weight of polyphosphazene polymer isobutene. is 2300-2500, maintains the temperature at 220 DEG C-230 DEG C, continues remaining maleic anhydride
Drip, after whole completion of dropwise addition, maintain the temperature at 220 DEG C-230 DEG C, constant temperature 10 hours-12 hours, obtain polyphosphazene polymer isobutyl
Enetutanedioic acid anhydride；
(2) amination
Macromolecule polyisobutenyl succinic anhydride being imported in amination still, add base oil and be diluted, base oil addition should
To ensure product viscosity >=300 centistokes(cst), macromolecule polyisobutenyl succinic anhydride gross weight 3.0%-3.15% polyenoid is many with accounting for
Amine synthesis under normal pressure, controls temperature and reacts 2 hours at 80 DEG C-140 DEG C, generate polyisobutylene succinamide and water, through subtracting
Pressure steams water, filters, obtains polyisobutylene succinamide；
(3) boronation
By polyisobutylene succinamide, or the polyisobutylene succinamide refined without dehydration, carry out boron with boric acid
Change, steam water through decompression the most again, collect as recycle-water, then through filtering, obtain macromolecule boronation polyisobutenyl succinyl
Imines.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: boron
When changing reaction, described polyisobutylene succinamide is 1:1-1:2 with the mol ratio of boric acid, and reaction temperature is 80 DEG C-140
DEG C, the response time is 2 hours.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: enter
Before the reaction of row boronation, the recycle-water obtained with the reaction decompression distillation of step (3) boronation carries out soaking boric acid, described boric acid and recovery
The mass ratio of water is 1:1, so that the polarity of boric acid is activated, boric acid conversion ratio can improve the biggest.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: take
The free maleic anhydride content of sample detection, acid number and viscosity, MA≤0.6%, acid number >=85KOHmg/g, viscosity >=3500 centistokes(cst), entirely
Amination is turned after portion is qualified.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: institute
Stating polyamines polyene is diethylenetriamine, triethylene tetramine, TEPA or five hexamine.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: amine
When changing reaction, reaction temperature is 120 DEG C-130 DEG C.
The synthetic method of macromolecule boronation polyisobutylene succinamide the most according to claim 1, is characterized in that: institute
Stating base oil is 150SN base oil.
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| CN111690081A (en) * | 2020-06-23 | 2020-09-22 | 新乡市瑞丰新材料股份有限公司 | Preparation method of boronized high-molecular-weight ashless dispersant |
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