CN106995513B - A kind of short-chain branch system oil-absorbing resin and preparation method thereof - Google Patents
A kind of short-chain branch system oil-absorbing resin and preparation method thereof Download PDFInfo
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- CN106995513B CN106995513B CN201710350547.8A CN201710350547A CN106995513B CN 106995513 B CN106995513 B CN 106995513B CN 201710350547 A CN201710350547 A CN 201710350547A CN 106995513 B CN106995513 B CN 106995513B
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of short-chain branch system oil-absorbing resins and preparation method thereof, it is calculated by mass parts, the resin is by 1 ~ 5 part of 5 ~ 10 parts of methyl methacrylate, 15 ~ 20 parts of butyl acrylate, 2 ~ 5 parts of styrene, 0.1 ~ 0.3 part of benzoyl peroxide, 0.1 ~ 0.5 part of polyvinyl alcohol, 0.1 ~ 0.5 part of divinylbenzene, coupling agent KH570 copolymerization, the resin that the present invention is synthesized by above-mentioned technique, with good oil absorbency, very big guarantor's oil cut rate, the thermal stability of resin are improved.
Description
Technical field
The present invention relates to a kind of short-chain branch system oil-absorbing resins and preparation method thereof, belong to macromolecule synthesising technology field.
Background technique
Short-chain branch system oil-absorbing resin belongs to synthetic resin, have swelling rate it is fast, oil-retaining is strong, preferable cold resistance and
The advantages that non-aging, can be used as aromatic, rubber oiliness modifying agent, it can also be used to water process.Make in the higher condition of temperature
Used time, the molecule segment in resin are easy to stretch because of solvation, show biggish oil absorbency until resin is unlimited
Swelling, the destruction of molecular structure.This is resin to improve its thermal stability, need to usually carry out having connect the modified introducing of branch just to resin
Property group such as phenyl ring, phenol, biphenyl, naphthalene etc..However the introducing of rigid radical, the flexibility of material is destroyed, in same temperature condition
Under, in oil suction, molecule segment is difficult to trail resin, and the power of the elastic recovery force of molecule segment and solvation generation is very
Reach balance fastly, the oil absorbency of resin reduces.Therefore, a kind of oil-absorbing resin is synthesized, in the case where not changing oil absorbency, is improved
Its thermal stability, is of great significance.
Summary of the invention
The object of the present invention is to provide a kind of short-chain branch system oil-absorbing resins and preparation method thereof, carry out to synthon
Reasonable proportion carries out preparing oil-absorbing resin, is not changing Resin oil adsorption through outstanding temperature programming technique, the continuous technique that is added dropwise
While, the thermal stability of resin is improved, with overcome the deficiencies in the prior art.
Technical solution of the present invention
A kind of short-chain branch system oil-absorbing resin is calculated by mass parts, and the resin is by 5 ~ 10 parts of methyl methacrylate, acrylic acid fourth
15 ~ 20 parts of ester, 2 ~ 5 parts of styrene, 0.1 ~ 0.3 part of benzoyl peroxide, 0.1 ~ 0.5 part of polyvinyl alcohol, divinylbenzene 0.1 ~ 0.5
1 ~ 5 part of part, coupling agent KH570 copolymerization.
Polyvinyl alcohol, will be dissolved in deionized water, metering system by a kind of preparation method of short-chain branch system oil-absorbing resin
Sour methyl esters, butyl acrylate, styrene are mixed to form monomer, then benzoyl peroxide, divinylbenzene are dissolved in monomer,
Finally mixed solution is added drop-wise in solubilized Polyvinyl alcohol solution and is polymerize.
In a kind of preparation method of short-chain branch system oil-absorbing resin above-mentioned, temperature programming is successively used in above-mentioned preparation method
It is prepared by technique, the continuous technique that is added dropwise.
In a kind of preparation method of short-chain branch system oil-absorbing resin above-mentioned, the temperature programming technique is by final mixing
Good mixed liquor is filled using heating water bath in 70 DEG C ~ 75 DEG C pre- hot mixing 30min, 75 DEG C ~ 80 DEG C prepolymerization 60min, 80 ~ 85
Divide polymerization 90min, 85 DEG C ~ 90 DEG C, 60min solidified resin.
In a kind of preparation method of short-chain branch system oil-absorbing resin above-mentioned, the continuous dropwise addition technique is in prepolymerization rank
In the period of section, the continuous coupling agent KH570 that is added dropwise is until adding coupling agent KH570 to specified numerical value.
In a kind of preparation method of short-chain branch system oil-absorbing resin above-mentioned, the deionized water and monomer ratio use mass ratio
For 3:1.
Compared with prior art, the resin that the present invention is synthesized by above-mentioned technique has good oil absorbency, very greatly
Guarantor's oil cut rate, the thermal stability of resin improved.
Detailed description of the invention
Attached drawing 1 is the infrared spectrogram for being not added with KH570 and adding KH570 resin；
Wherein 701cm-1,760cm-1 are the monosubstituted characteristic peak of benzene, and 820cm-1 corresponds to Si-C stretching vibration, 1087cm-
1 is SI-O stretching vibration peak, and 1164cm-1 is C-O stretching vibration peak, and the C-H that 2956cm-1 and 1460cm-1 correspond to CH3 is not right
Claim stretching vibration, 2873cm-1 and 1380cm-1 correspond to the C-H symmetrical stretching vibration of CH3,1460cm-1 and 2930cm-1 correspondence-
The C-H absorption peak of CH2-, 1727cm-1 are C=O stretching vibration peaks.Comparative analysis is it is found that add the infrared light of resin after kh570
Spectrogram, more two absorption peaks, illustrate monomer and kh570 copolymerization resin at 820cm-1 and 1164cm-1.
Attached drawing 2 is the resin for being not added with KH570, and decomposition starting temperature is 373.3 DEG C, and decomposition rate is fast, at 397.7 DEG C points
Solution rate reaches maximum, and decomposition curve is single, only one decomposes platform, without mutually separating, illustrates that monomer is copolymerized into single tree
Rouge；
Attached drawing 3 is 383.9 DEG C of KH570 resin decomposition starting temperature of addition, and decomposition rate is low, in 406.9 DEG C of decomposition rates
Reach maximum, decomposition rate is lower than the resin for being not added with KH570, and decomposition curve is single, only one decomposes platform, without phase point
From coupling agent and monomer form good copolymerization.
Specific embodiment
With reference to the accompanying drawing to further detailed description of the invention, but not as any limitation of the invention.
The present invention is made by grouping experiment, and specific experiment is as follows:
The present invention is made by grouping experiment, and specific experiment is as follows:
Embodiment 1), in parts by weight, the resin is by 5 ~ 10 parts of methyl methacrylate, butyl acrylate 15 ~ 20
Part, 2 ~ 5 parts of styrene, 0.1 ~ 0.3 part of benzoyl peroxide, 0.1 ~ 0.5 part of polyvinyl alcohol, 0.1 ~ 0.5 part of divinylbenzene suspension
Polymerization is made.The resin is not the continuous KH570 that is added dropwise and polymerize, and decomposition rate is very fast, and decomposition temperature is lower, as shown in Figure 2.
Embodiment 2), in parts by weight, the resin is by 5 ~ 10 parts of methyl methacrylate, butyl acrylate 15 ~ 20
Part, 2 ~ 5 parts of styrene, 0.1 ~ 0.3 part of benzoyl peroxide, 0.1 ~ 0.5 part of polyvinyl alcohol, 0.1 ~ 0.5 part of divinylbenzene, coupling
1 ~ 5 part of suspension polymerisation of agent KH570 is made, and coupling agent KH570 is added during the reaction with the continuous technique that is added dropwise.It decomposes speed
Rate is lower, and decomposition temperature is higher, as shown in figure 3, Resin oil adsorption variation is less, enhances guarantor's oil cut rate of oil product.
Through resin made of temperature programming technique of the present invention and continuous dropwise addition process polymerisation, oil absorbency changes not
Greatly, sustained release equation k value is smaller, and guarantor's oil cut rate is higher, and thermal decomposition temperature is promoted, and decomposition rate reduces.
In conclusion the basic principles, main features and advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Effect object defines.
Claims (4)
1. a kind of short-chain branch system oil-absorbing resin, it is characterised in that: calculated by mass parts, the resin is by methyl methacrylate 5~10
Part, 15~20 parts of butyl acrylate, 2~5 parts of styrene, 0.1~0.3 part of benzoyl peroxide, 0.1~0.5 part of polyvinyl alcohol,
1~5 part of 0.1~0.5 part of divinylbenzene, coupling agent KH570 copolymerization.
2. the preparation method of a kind of short-chain branch system oil-absorbing resin according to claim 1, it is characterised in that: polyvinyl alcohol is molten
For solution in deionized water, methyl methacrylate, butyl acrylate, styrene are mixed to form monomer, then by benzoyl peroxide,
Divinylbenzene is dissolved in monomer, and finally mixed solution is added drop-wise in solubilized Polyvinyl alcohol solution and is polymerize；Above-mentioned system
It is successively prepared using temperature programming technique, the continuous technique that is added dropwise in Preparation Method；The continuous dropwise addition technique is in pre-polymerization
In the period in conjunction stage, the continuous coupling agent KH570 that is added dropwise is until adding coupling agent KH570 to specified numerical value.
3. a kind of preparation method of short-chain branch system oil-absorbing resin according to claim 2, it is characterised in that: the program
Heating process is the mixed liquor that will finally mix, using heating water bath, in 70 DEG C~75 DEG C pre- hot mixing 30min, 75 DEG C~
80 DEG C of prepolymerizations 60min, 80~85 DEG C of sufficiently polymerization 90min, 85 DEG C~90 DEG C, 60min solidified resin.
4. a kind of preparation method of short-chain branch system oil-absorbing resin according to claim 2, it is characterised in that: the deionized water
Use mass ratio for 3:1 with monomer ratio.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710350547.8A CN106995513B (en) | 2017-05-18 | 2017-05-18 | A kind of short-chain branch system oil-absorbing resin and preparation method thereof |
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| CN201710350547.8A CN106995513B (en) | 2017-05-18 | 2017-05-18 | A kind of short-chain branch system oil-absorbing resin and preparation method thereof |
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| CN106995513A CN106995513A (en) | 2017-08-01 |
| CN106995513B true CN106995513B (en) | 2019-05-07 |
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| CN201710350547.8A Expired - Fee Related CN106995513B (en) | 2017-05-18 | 2017-05-18 | A kind of short-chain branch system oil-absorbing resin and preparation method thereof |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107286285A (en) * | 2017-08-07 | 2017-10-24 | 江苏优纳优盛新材料有限公司 | A kind of polymer oil absorption material and preparation method thereof |
| CN107663316B (en) * | 2017-09-21 | 2020-05-12 | 贵州理工学院 | Preparation method of oil-absorbing expansion rubber |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215355A (en) * | 2008-01-09 | 2008-07-09 | 苏州大学 | High oil absorption resin and synthetic method thereof |
| CN101314624A (en) * | 2008-05-21 | 2008-12-03 | 安徽省电力公司合肥供电公司 | High oil suction resin and uses thereof |
| CN101880353A (en) * | 2010-07-03 | 2010-11-10 | 鲁东大学 | Preparation method of short-chain high-oil-absorption resin |
| CN102924657A (en) * | 2012-11-02 | 2013-02-13 | 厦门大学 | Oil absorption material containing silicon polymer and preparation methods thereof |
| CN103936919A (en) * | 2014-04-14 | 2014-07-23 | 中国石油大学(华东) | Method for preparing high-oil-absorbency resin with good mechanical properties |
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- 2017-05-18 CN CN201710350547.8A patent/CN106995513B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215355A (en) * | 2008-01-09 | 2008-07-09 | 苏州大学 | High oil absorption resin and synthetic method thereof |
| CN101314624A (en) * | 2008-05-21 | 2008-12-03 | 安徽省电力公司合肥供电公司 | High oil suction resin and uses thereof |
| CN101880353A (en) * | 2010-07-03 | 2010-11-10 | 鲁东大学 | Preparation method of short-chain high-oil-absorption resin |
| CN102924657A (en) * | 2012-11-02 | 2013-02-13 | 厦门大学 | Oil absorption material containing silicon polymer and preparation methods thereof |
| CN103936919A (en) * | 2014-04-14 | 2014-07-23 | 中国石油大学(华东) | Method for preparing high-oil-absorbency resin with good mechanical properties |
Non-Patent Citations (1)
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| 苯乙烯-甲基丙烯酸酯三元共聚高吸油树脂的合成与性能研究;王志辉等;《化工新型材料》;20090430;第37卷(第4期);第73-75页 |
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