CN106496431A - A kind of modified high oil-absorbing resin and preparation method thereof - Google Patents
A kind of modified high oil-absorbing resin and preparation method thereof Download PDFInfo
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- CN106496431A CN106496431A CN201610914279.3A CN201610914279A CN106496431A CN 106496431 A CN106496431 A CN 106496431A CN 201610914279 A CN201610914279 A CN 201610914279A CN 106496431 A CN106496431 A CN 106496431A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/04—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to rubbers
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Abstract
The present invention relates to a kind of modified high oil-absorbing resin and preparation method thereof, belongs to oil-absorbing resin technical field.The modified high oil-absorbing resin of the present invention includes water phase and oil phase.The present invention is prepared for oil-absorbing resin using process for suspension polymerization.In formulation selection, with ethyleneglycol dimethyacrylate and divinylbenzene as combining cross-linking agent；Dibenzoyl peroxide (BPO) is initiator；Polymerized monomer selects, in addition to traditional oil-absorbing resin synthesis component methyl methacrylate, octadecyl acrylate, dodecyl acrylate is adopted, also to add lipophile preferably butadiene rubber to increase the oil absorption of oil-absorbing resin in polymerization system；Meanwhile, add 200#Gasoline is the porous that porogen increases resin, accelerates the swelling rate of resin；Under this process recipe conditions prepare high oil-absorbing resin toluene, the adsorbance of dimethylbenzene up to 25 35g/g and 20 25g/g, with preferable application prospect.
Description
Technical field
A kind of a kind of the present invention relates to oil-absorbing resin and preparation method thereof, it is more particularly related to modified high suction
Oleoresin and preparation method thereof, belongs to oil-absorbing resin technical field.
Background technology
With the continuous development of social economy, the problem of environmental pollution come with global industry is increasingly people institute
Concern.The living environment that threaten marine environment and urbanite that wherein oil pollution is serious.Especially offshore oil is opened
That adopted and transport is increasingly frequent, and marine oil spill accident happens occasionally.And oils enters ocean, to natural environment, aquaculture, shallow
Water seashore, harbour industry etc. can all cause harm difficult to the appraisal.The eighties, marine pollution scientific research expert group (GESAMP)
Marine pollution is investigated and has been assessed, it is found that oil is the one side of marine pollution most serious.Therefore, develop dynamical
Oil suction product has important actual application value.High oil-absorbing resin is low crosslinking degree polymer obtained in oleophylic monomer, has
Three-dimensional cross-linked network structure, inside have certain micropore, and this material being capable of effective process sea and land oil spilling and oily waste water
Water, reduces the harm to environment.
The oil absorption of existing oil-absorbing resin and swelling rate are undesirable.
Content of the invention
Present invention seek to address that the undesirable problem of the oil absorption of oil-absorbing resin of the prior art and swelling rate, carries
For a kind of modified high oil-absorbing resin, the oil absorption of the oil-absorbing resin and swelling rate are preferable.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of modified high oil-absorbing resin, it is characterised in that：Including following raw materials by weight：
Oil phase：
Butadiene rubber 15-20 parts
Methyl methacrylate 30-40 parts
Octadecyl acrylate 10-15 parts
Dodecyl acrylate 15-20 parts
Divinylbenzene 0.2-0.5 part
Methacrylate diethylene glycol ester 0.5-1.0 parts
200# gasoline 50-60 parts
Dibenzoyl peroxide (BPO) 3-5 parts；
Water phase：
10% polyvinyl alcohol（PVA1788）Aqueous 8-10 part
Gelatin 5-10 parts
NaCl 15-20 parts
CaCO38-10 parts
0.1% methylene blue aqueous 5-8 part
Deionized water 800-1000 parts.
A kind of preparation method of modified high oil-absorbing resin, it is characterised in that：Comprise the following steps that：
Water phase is prepared in A, the there-necked flask according to water phase formula in 2500ml with stirring, condensing tube and charge door, standby；
B, methyl methacrylate, octadecyl acrylate, dodecyl acrylate, divinyl is accurately weighed according to oil phase recipe requirements
, in 1500ml beakers, stirring, mixing are for base benzene, methacrylate diethylene glycol ester, 200# gasoline, dibenzoyl peroxide
Even, standby；
C, the butadiene rubber that addition is cut into pieces in advance toward in oil phase, are sufficiently mixed until butadiene rubber is completely dissolved；
D, the aqueous phase system temperature for preparing in advance is risen to 40-50 DEG C, start stirring until water phase each component be sufficiently mixed molten
Solution；The oil mixture that step B is prepared is poured in water phase there-necked flask；
E, the speed for keeping stirring in reactor, make oil phase form uniform bead and are dispersed in the water phase for preparing in advance；When
After oil phase dispersion bead particle diameter meets the requirements, temperature of reaction system is risen to 75-78 DEG C, until scattered oil droplet does not rupture determining
Type；
F, polymerization reaction system temperature is raised to 85-90 DEG C, is incubated 2-3 hour；Polymerization reaction system is warming up to 90-95
DEG C, it is incubated 3-4 hour；Reaction system is cooled to room temperature, resin bead is leached；
G, drip washing being carried out using ethanol to resin, removing porogen 200# gasoline and other impurity in resin, vacuum drying is
Obtain modified high oil-absorbing resin.
In step E, the speed for keeping stirring in reactor is 100-150 rev/min to the present invention.
The Advantageous Effects that the present invention brings：
The present invention is prepared for oil-absorbing resin using process for suspension polymerization.In formulation selection, with ethyleneglycol dimethyacrylate
It is combination cross-linking agent with divinylbenzene；Dibenzoyl peroxide (BPO) is initiator；Polymerized monomer is selected except using tradition suction
Outside oleoresin synthesis component methyl methacrylate, octadecyl acrylate, dodecyl acrylate, also add in polymerization system
Lipophile preferably butadiene rubber is increasing the oil absorption of oil-absorbing resin；Meanwhile, add 200#Gasoline is that porogen increases resin
Porous, accelerate the swelling rate of resin；The high oil-absorbing resin toluene for preparing under this process recipe conditions, dimethylbenzene
Adsorbance up to 25-35g/g and 20-25g/g, with preferable application prospect.
Specific embodiment
Embodiment 1
A kind of modified high oil-absorbing resin, including following raw materials by weight：
Oil phase：
15 parts of butadiene rubber
30 parts of methyl methacrylate
10 parts of octadecyl acrylate
15 parts of dodecyl acrylate
0.2 part of divinylbenzene
0.5 part of methacrylate diethylene glycol ester
50 parts of 200# gasoline
3 parts of dibenzoyl peroxide (BPO)；
Water phase：
10% polyvinyl alcohol（PVA1788）8 parts of aqueous
5 parts of gelatin
15 parts of NaCl
CaCO38 parts
0.1% 5 parts of methylene blue aqueous
800 parts of deionized water.
Embodiment 2
A kind of modified high oil-absorbing resin, including following raw materials by weight：
Oil phase：
20 parts of butadiene rubber
40 parts of methyl methacrylate
15 parts of octadecyl acrylate
20 parts of dodecyl acrylate
0.5 part of divinylbenzene
1.0 parts of methacrylate diethylene glycol ester
60 parts of 200# gasoline
5 parts of dibenzoyl peroxide (BPO)；
Water phase：
10% polyvinyl alcohol（PVA1788）10 parts of aqueous
10 parts of gelatin
20 parts of NaCl
CaCO310 parts
0.1% 8 parts of methylene blue aqueous
1000 parts of deionized water.
Embodiment 3
A kind of modified high oil-absorbing resin, including following raw materials by weight：
Oil phase：
17.5 parts of butadiene rubber
35 parts of methyl methacrylate
12.5 parts of octadecyl acrylate
17.5 parts of dodecyl acrylate
0.35 part of divinylbenzene
0.7 part of methacrylate diethylene glycol ester
55 parts of 200# gasoline
4 parts of dibenzoyl peroxide (BPO)；
Water phase：
10% polyvinyl alcohol（PVA1788）9 parts of aqueous
7.5 parts of gelatin
17 parts of NaCl
CaCO389 parts
0.1% 6.5 parts of methylene blue aqueous
900 parts of deionized water.
Embodiment 4
A kind of preparation method of modified high oil-absorbing resin, comprises the following steps that：
Water phase is prepared in A, the there-necked flask according to water phase formula in 2500ml with stirring, condensing tube and charge door, standby；
B, methyl methacrylate, octadecyl acrylate, dodecyl acrylate, divinyl is accurately weighed according to oil phase recipe requirements
, in 1500ml beakers, stirring, mixing are for base benzene, methacrylate diethylene glycol ester, 200# gasoline, dibenzoyl peroxide
Even, standby；
C, the butadiene rubber that addition is cut into pieces in advance toward in oil phase, are sufficiently mixed until butadiene rubber is completely dissolved；
D, the aqueous phase system temperature for preparing in advance is risen to 40 DEG C, stirring is started until water phase each component is sufficiently mixed dissolving；
The oil mixture that step B is prepared is poured in water phase there-necked flask；
E, the speed for keeping stirring in reactor, make oil phase form uniform bead and are dispersed in the water phase for preparing in advance；When
After oil phase dispersion bead particle diameter meets the requirements, temperature of reaction system is risen to 75 DEG C, until scattered oil droplet does not rupture sizing；
F, polymerization reaction system temperature is raised to 85 DEG C, is incubated 2 hours；Polymerization reaction system is warming up to 90 DEG C, 3 are incubated
Hour；Reaction system is cooled to room temperature, resin bead is leached；
G, drip washing being carried out using ethanol to resin, removing porogen 200# gasoline and other impurity in resin, vacuum drying is
Obtain modified high oil-absorbing resin.
Preferably, in step E, the speed for keeping stirring in reactor is 100 revs/min.
Embodiment 5
A kind of preparation method of modified high oil-absorbing resin, comprises the following steps that：
Water phase is prepared in A, the there-necked flask according to water phase formula in 2500ml with stirring, condensing tube and charge door, standby；
B, methyl methacrylate, octadecyl acrylate, dodecyl acrylate, divinyl is accurately weighed according to oil phase recipe requirements
, in 1500ml beakers, stirring, mixing are for base benzene, methacrylate diethylene glycol ester, 200# gasoline, dibenzoyl peroxide
Even, standby；
C, the butadiene rubber that addition is cut into pieces in advance toward in oil phase, are sufficiently mixed until butadiene rubber is completely dissolved；
D, the aqueous phase system temperature for preparing in advance is risen to 50 DEG C, stirring is started until water phase each component is sufficiently mixed dissolving；
The oil mixture that step B is prepared is poured in water phase there-necked flask；
E, the speed for keeping stirring in reactor, make oil phase form uniform bead and are dispersed in the water phase for preparing in advance；When
After oil phase dispersion bead particle diameter meets the requirements, temperature of reaction system is risen to 78 DEG C, until scattered oil droplet does not rupture sizing；
F, polymerization reaction system temperature is raised to 90 DEG C, is incubated 3 hours；Polymerization reaction system is warming up to 95 DEG C, 4 are incubated
Hour；Reaction system is cooled to room temperature, resin bead is leached；
G, drip washing being carried out using ethanol to resin, removing porogen 200# gasoline and other impurity in resin, vacuum drying is
Obtain modified high oil-absorbing resin.
Preferably, in step E, the speed for keeping stirring in reactor is 150 revs/min.
Embodiment 6
A kind of preparation method of modified high oil-absorbing resin, comprises the following steps that：
Water phase is prepared in A, the there-necked flask according to water phase formula in 2500ml with stirring, condensing tube and charge door, standby；
B, methyl methacrylate, octadecyl acrylate, dodecyl acrylate, divinyl is accurately weighed according to oil phase recipe requirements
, in 1500ml beakers, stirring, mixing are for base benzene, methacrylate diethylene glycol ester, 200# gasoline, dibenzoyl peroxide
Even, standby；
C, the butadiene rubber that addition is cut into pieces in advance toward in oil phase, are sufficiently mixed until butadiene rubber is completely dissolved；
D, the aqueous phase system temperature for preparing in advance is risen to 45 DEG C, stirring is started until water phase each component is sufficiently mixed dissolving；
The oil mixture that step B is prepared is poured in water phase there-necked flask；
E, the speed for keeping stirring in reactor, make oil phase form uniform bead and are dispersed in the water phase for preparing in advance；When
After oil phase dispersion bead particle diameter meets the requirements, temperature of reaction system is risen to 76.5 DEG C, until scattered oil droplet does not rupture sizing；
F, polymerization reaction system temperature is raised to 87.5 DEG C, is incubated 2.5 hours；Polymerization reaction system is warming up to 92.5 DEG C,
3.5 hours of insulation；Reaction system is cooled to room temperature, resin bead is leached；
G, drip washing being carried out using ethanol to resin, removing porogen 200# gasoline and other impurity in resin, vacuum drying is
Obtain modified high oil-absorbing resin.
Preferably, in step E, the speed for keeping stirring in reactor is 125 revs/min.
Claims (3)
1. a kind of modified high oil-absorbing resin, it is characterised in that：Including following raw materials by weight：
Oil phase：
Butadiene rubber 15-20 parts
Methyl methacrylate 30-40 parts
Octadecyl acrylate 10-15 parts
Dodecyl acrylate 15-20 parts
Divinylbenzene 0.2-0.5 part
Methacrylate diethylene glycol ester 0.5-1.0 parts
200# gasoline 50-60 parts
Dibenzoyl peroxide 3-5 parts；
Water phase：
10% polyvinyl alcohol aqueous 8-10 part
Gelatin 5-10 parts
NaCl 15-20 parts
CaCO38-10 parts
0.1% methylene blue aqueous 5-8 part
Deionized water 800-1000 parts.
2. the preparation method of a kind of modified high oil-absorbing resin according to claim 1, it is characterised in that：Including following technique
Step：
Water phase is prepared in A, the there-necked flask according to water phase formula in 2500ml with stirring, condensing tube and charge door, standby；
B, methyl methacrylate, octadecyl acrylate, dodecyl acrylate, divinyl is accurately weighed according to oil phase recipe requirements
, in 1500ml beakers, stirring, mixing are for base benzene, methacrylate diethylene glycol ester, 200# gasoline, dibenzoyl peroxide
Even, standby；
C, the butadiene rubber that addition is cut into pieces in advance toward in oil phase, are sufficiently mixed until butadiene rubber is completely dissolved；
D, the aqueous phase system temperature for preparing in advance is risen to 40-50 DEG C, start stirring until water phase each component be sufficiently mixed molten
Solution；The oil mixture that step B is prepared is poured in water phase there-necked flask；
E, the speed for keeping stirring in reactor, make oil phase form uniform bead and are dispersed in the water phase for preparing in advance；When
After oil phase dispersion bead particle diameter meets the requirements, temperature of reaction system is risen to 75-78 DEG C, until scattered oil droplet does not rupture determining
Type；
F, polymerization reaction system temperature is raised to 85-90 DEG C, is incubated 2-3 hour；Polymerization reaction system is warming up to 90-95
DEG C, it is incubated 3-4 hour；Reaction system is cooled to room temperature, resin bead is leached；
G, drip washing being carried out using ethanol to resin, removing porogen 200# gasoline and other impurity in resin, vacuum drying is
Obtain modified high oil-absorbing resin.
3. the preparation method of a kind of modified high oil-absorbing resin according to claim 2, it is characterised in that：In step E, institute
It is 100-150 rev/min to state and keep the speed stirred in reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610914279.3A CN106496431A (en) | 2016-10-20 | 2016-10-20 | A kind of modified high oil-absorbing resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610914279.3A CN106496431A (en) | 2016-10-20 | 2016-10-20 | A kind of modified high oil-absorbing resin and preparation method thereof |
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| CN106496431A true CN106496431A (en) | 2017-03-15 |
Family
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141417A (en) * | 2017-06-27 | 2017-09-08 | 白才蓉 | A kind of oiliness sewage treatment high oil-absorbing resin and preparation method thereof |
| CN109453749A (en) * | 2018-09-14 | 2019-03-12 | 江苏省金峰石油机械制造有限公司 | A kind of fast absorbing oil device for emergency processing oil accident |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333286A (en) * | 2013-07-23 | 2013-10-02 | 中蓝晨光化工研究设计院有限公司 | Oil-absorbing resin and preparation method |
| CN103360539A (en) * | 2013-07-25 | 2013-10-23 | 南京市荣达树脂有限公司 | Preparation method of high-oil-absorbency resin |
| CN105254818A (en) * | 2015-10-23 | 2016-01-20 | 蓝星（成都）新材料有限公司 | High-oil-absorption resin and preparation method thereof |
-
2016
- 2016-10-20 CN CN201610914279.3A patent/CN106496431A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333286A (en) * | 2013-07-23 | 2013-10-02 | 中蓝晨光化工研究设计院有限公司 | Oil-absorbing resin and preparation method |
| CN103360539A (en) * | 2013-07-25 | 2013-10-23 | 南京市荣达树脂有限公司 | Preparation method of high-oil-absorbency resin |
| CN105254818A (en) * | 2015-10-23 | 2016-01-20 | 蓝星（成都）新材料有限公司 | High-oil-absorption resin and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141417A (en) * | 2017-06-27 | 2017-09-08 | 白才蓉 | A kind of oiliness sewage treatment high oil-absorbing resin and preparation method thereof |
| CN109453749A (en) * | 2018-09-14 | 2019-03-12 | 江苏省金峰石油机械制造有限公司 | A kind of fast absorbing oil device for emergency processing oil accident |
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Application publication date: 20170315 |