CN106750400A - The preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel - Google Patents
The preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel Download PDFInfo
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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Abstract
The present invention relates to a kind of preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel.The method is to make comonomer with MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacrylic acid oxygen ethyl trimellitic anhydride ester, sorbic acid, PEGDMA-400 makees crosslinking agent, and potassium peroxydisulfate sodium hydrogensulfite makees initiator and carry out copolymerization in deionized water to obtain organic amphiprotic copolymerized macromolecule first network gel;The first network gel is swelling in the aqueous solution that caffeic acid, inositol, methacrylic acid oxygen propyl group trimellitic anhydride ester, the bromo DOPCP of dimethacrylate two and deionized water are prepared, monomer, crosslinking agent in the aqueous solution are copolymerized conjunction, esterification through the effect of potassium peroxydisulfate, pyridoxine hydrochloride, finally obtain organic amphiprotic copolymerized macromolecule interpenetrating networks gel.
Description
Technical field
The present invention relates to a kind of preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel.
Background technology
Gel is a kind of special dispersion, and high-polymer molecular or colloidal solid interconnect, and to form three dimensions netted
Structure, can absorb substantial amounts of water-swellable and water insoluble, and definite shape can be kept in water, have solid and liquid duality concurrently
Matter.Macroscopically see, high-molecular gel has certain shape, applying certain external force can deform, can recover original after removal external force
Shape, the viscoplasticity with solid;Seen on microcosmic, high-molecular gel has three-dimensional net structure water insoluble, three-dimensional network point
Son can stretch in water, with liquid property.With soft, water content it is high and have the viscoelastic gel of rubber environmental protection, weaving,
All many-sides such as building materials, petrochemical industry, food, agricultural gardening, daily cosmetics have and are widely applied.
Organism including humans is all high-molecular gel composition, mostly with electrical, such as protein, amino acid.
Copolymerization Amphiphatic high polymer interpenetrating networks gel can obtain Protean specific performance, particularly height and contains with the change of copolymerization component
The similitude of the electrical and organization of human body in water and molecule, good biocompatibility, environmental stimulus response is cured in biology
The fields such as medicine controlled releasing, bio-sensing, the organizational project in medicine field have obtained some applications.
The problem that the preparation method of current organic amphiprotic copolymerized macromolecule interpenetrating networks gel is primarily present is monomer propylene
The toxic articles of acid amides category " carcinogenic, aberration inducing, mutagenesis ", crosslinking agent N, N methylene diacrylamine toxicity is larger, and gel is deposited
In unfavorable toxic effect;The interpenetrating networks gel stability that single crosslinking agent is formed is relatively low.Exploitation uses nontoxic or low toxicity
Monomer, crosslinking agent carry out combined polymerization to reduce gel toxicity, forming multiple interpenetrating networks using compounding crosslinking agent improves gel
The preparation method of the organic amphiprotic copolymerized macromolecule interpenetrating networks gel of stability has larger practical value.
The content of the invention
For the problem that the preparation method of current organic amphiprotic copolymerized macromolecule interpenetrating networks gel is present, mesh of the invention
Be to provide it is a kind of use nontoxic or low-toxicity monomer, the crosslinking agent to carry out combined polymerization to reduce gel toxicity, use and compound crosslinking agent
The preparation method that multiple interpenetrating networks improve the organic amphiprotic copolymerized macromolecule interpenetrating networks gel of gel stability is formed, it is special
It is that in closed reactor component A and deionized water stirring can added to prepare the aqueous solution to levy, and the weight concentration for controlling component A is
28%~62%;After the completion of prepared by solution, relative degree of vacuum is evacuated to for -0.02MPa~-0.08MPa, be passed through nitrogen and recover anti-
After answering device to normal pressure, add the aqueous solution prepared by B component and deionized water under agitation, the weight concentration of B component for 20%~
40%;After the aqueous solution charging of B component terminates, 35 DEG C~50 DEG C are warming up to, add matched somebody with somebody by component C and deionized water under agitation
The aqueous solution of system, the weight concentration of component C is 5%~15%;Control ph is 4~10, in 35 DEG C~50 DEG C constant temperature, continues to stir
Reaction 2h~3.5h, obtains organic amphiprotic copolymerized macromolecule first network gel;Then cooled down, in the case where nitrogen is passed through, will
The aqueous solution that first network gel input is prepared equipped with D components and deionized water can be swelling in closed reactor, D components
Weight concentration is 1.8%~11%, by weight, first network gel:Weight ratio=1 of D component deionized water solutions:(95~
155), swelling 2h~6h;Add the aqueous solution prepared by component E and deionized water and continue swelling, the weight concentration of component E is
10%~20%, swelling 16 h~24 h;After the completion of swelling, 75 DEG C~95 DEG C are warming up to, control ph is 3~7,75 DEG C~95
DEG C constant temperature, reacts 4h~6h, obtains organic amphiprotic copolymerized macromolecule interpenetrating networks gel.The component A is by methacryloxypropyl
Ethyl-trimethyl salmiac, methacrylic acid oxygen ethyl trimellitic anhydride ester, sorbic acid composition, by the gauge of material, methyl-prop
Alkene acyloxyethyl trimethyl ammonium chloride:Methacrylic acid oxygen ethyl trimellitic anhydride ester:The ratio between amount of material of sorbic acid=(0.5
~1.2):(0.3~1.6):(0.4~1.1);B component is PEGDMA-400, number-average molecular weight is 2000~
20000, its charged material weight is the 2.5%~11% of component A gross weight;Component C is made up of potassium peroxydisulfate-sodium hydrogensulfite, its throwing
Material gross weight is the 0.3%~1.8% of component A gross weight, by weight, potassium peroxydisulfate:Weight ratio=1 of sodium hydrogensulfite:
(0.2~1.1);D components are by caffeic acid, inositol, methacrylic acid oxygen propyl group trimellitic anhydride ester and dimethacrylate
Two bromo DOPCPs are constituted, by the gauge of material, caffeic acid:Inositol:Methacrylic acid oxygen propyl group trimellitic anhydride
The ratio between amount of material of ester=(0.5~2.0):(0.08~0.32):(0.4~1.1), by weight, dimethacrylate dibromo
It is total caffeic acid, inositol, methacrylic acid oxygen propyl group trimellitic anhydride three kinds of monomers of ester for DOPCP charged material weight
The 1.8%~5.5% of weight;Component E is made up of potassium peroxydisulfate, pyridoxine hydrochloride, and potassium peroxydisulfate charged material weight is D component gross weights
The 0.1%~1.2% of amount, the pyridoxine hydrochloride gross weight that feeds intake is the 0.8%~5.6% of D component weights.
What technical method of the invention was realized in:Methylacryoyloxyethyl front three can be being prepared in closed reactor
Ammonium chloride CH2=C(CH3)COO(CH2)2N(CH3)3Cl, methacrylic acid oxygen ethyl trimellitic anhydride ester CH2=C(CH3)COO
(CH2)2OOCC6H3C2O3, sorbic acid CH3The aqueous solution of CH=CHCH=CHCOOH comonomers;After vacuumizing deoxidation, nitrogen is passed through
Protection, adds the aqueous solution of crosslinking agent PEGDMA-400;After intensification, redox initiator over cure is added
Sour potassium-sodium hydrogensulfite K2S2O8-NaHSO3The aqueous solution, through trigger, combined polymerization chain propagation reaction, crosslinking agent dimethyl allene
Acid polyethylene glycol ester participates in copolyreaction and line style copolymerization macromolecular crosslinks reaction and forms cross-linked network structure, through chain termination
Reaction, obtains organic amphiprotic copolymerized macromolecule first network gel.Logical nitrogen protection, organic amphiprotic copolymerized macromolecule first network
Gel is at caffeic acid (HO)2C6H3CH=CHCOOH, inositol (CH)6(OH)6, methacrylic acid oxygen propyl group trimellitic anhydride ester
CH2=C(CH3)COO(CH2)3OOCC6H3C2O3, the bromo DOPCP CH of dimethacrylate two2=C(CH3)COOCH2C
(CH2Br)2CH2OOC(CH3)C=CH2The aqueous solution effect under it is swelling, add initiator potassium persulfate K2S2O8, catalyst pyrrole trembles
Alcohol hydrochloride (CH3)(HOCH2)2(HO)C5Continue swelling in the presence of the HNHCl aqueous solution, in swelling process, in the aqueous solution
Monomer, crosslinking agent, initiator, catalyst enter into organic amphiprotic copolymerized macromolecule first network gel inside and are uniformly distributed;
Line style copolymerization macromolecular, the bromo DOPCP of crosslinking agent dimethacrylate two are formed through initiation, combined polymerization chain propagation reaction
Participate in copolyreaction and line style copolymerization macromolecular crosslinks reaction, form cross-linked network structure, pyridoxine hydrochloride catalysis band
There is esterification in the molecule of the molecule of carboxylic group and hydroxyl group, due to inositol with six OH groups will and band
The molecule of carboxylic group reacts to form cross-linked network structure;Further reaction, finally due to the chain of radical copolymerization macromolecular
Terminate the completion with esterification, form organic amphiprotic copolymerized macromolecule interpenetrating networks gel.
Relative to art methods, outstanding advantages of the present invention are monomer methacryloxypropyl second used in technology of preparing
Base trimethyl ammonium chloride, methacrylic acid oxygen ethyl trimellitic anhydride ester, methacrylic acid oxygen propyl group trimellitic anhydride ester and friendship
The bromo DOPCP low toxicity of connection agent dimethacrylate two, monomer sorbic acid, caffeic acid and crosslinking agent dimethacrylate gather
Glycol ester, inositol are nontoxic, reduce gel toxicity;There is the interpenetrating networks gel of preparation radical crosslinking and esterification to hand over
Connection network structure, improves the stability of interpenetrating networks gel;Preparation method is simple, reaction condition is gentle, be suitable for production, has
Good environmental benefit and economic benefit.
Specific embodiment
Embodiment 1:124.5g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, the 110.5g methacrylic acid inclined benzene of oxygen ethyl
Three acid anhydride esters, 56.1g sorbic acids and 679.1ml deionized waters are added to volume and can stir mixing in closed reactor for 1.5L
Uniformly, the weight concentration of the aqueous solution is 30%;Relative degree of vacuum -0.03MPa is evacuated to, nitrogen is then passed to and is recovered reaction
To normal pressure, the number-average molecular weight for adding 8.7g is that 3000 PEGDMA-400 and 32.9ml deionized waters are matched somebody with somebody to device
The aqueous solution of system, the weight concentration of the aqueous solution is 21%;37 DEG C are then heated to, 1.12g potassium peroxydisulfates, 0.34g sulfurous is added
The aqueous solution that sour hydrogen sodium and 25ml deionized waters are prepared, the weight concentration of the aqueous solution is 5.5%, in 37 DEG C of constant temperature, control ph
It is 4.5, continues stirring reaction 2.3h, obtains organic amphiprotic copolymerized macromolecule first network gel;Then cooled down, be passed through
Under nitrogen, organic amphiprotic copolymerized macromolecule first network gel 138.6g input volumes can be swelling in closed reactor for 20L's,
In the reactor equipped with 108.1g caffeic acids, 18.6g inositol, 143.1g methacrylic acid oxygen propyl group trimellitic anhydrides ester,
The aqueous solution that the bromo DOPCP of 5.44g dimethacrylates two and 13586.8ml deionized waters are prepared, the weight of the aqueous solution
Amount concentration is 2%, the weight of first network gel(138.6g):The weight of the aqueous solution(13864.1g)=1:100, swelling 3h;
The aqueous solution for adding the preparation of 0.55g potassium peroxydisulfates, 2.77g pyridoxine hydrochlorides and 28.4ml deionized waters continues swelling, should
The weight concentration of the aqueous solution is 10.5%, swelling 17h;77 DEG C are warming up to after the completion of swelling, control ph is 3.4, in 77 DEG C of constant temperature
Reaction 4.3h, obtains organic amphiprotic copolymerized macromolecule interpenetrating networks gel.The gel is water insoluble, can be swelling in water, gel
Swelling ratio(ESR)=5257%(Deionized water), gel swelling rate(ESR)=5172%(The NaCl aqueous solution of weight concentration 1%).
Embodiment 2:228.3g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, the 414.4g methacrylic acid inclined benzene of oxygen ethyl
Three acid anhydride esters, 112.1g sorbic acids and 503.2ml deionized waters are added to volume for 1.5L can stir mixing in closed reactor
Uniformly, the weight concentration of the aqueous solution is 60%;Relative degree of vacuum -0.07MPa is evacuated to, nitrogen is then passed to and is recovered reaction
To normal pressure, the number-average molecular weight for adding 75.5g is 19000 PEGDMA-400 and 118.1ml deionizations to device
The aqueous solution that water is prepared, the weight concentration of the aqueous solution is 39%;48 DEG C are then heated to, 5.66g potassium peroxydisulfates, 5.66g is added
The aqueous solution that sodium hydrogensulfite and 66.8ml deionized waters are prepared, the weight concentration of the aqueous solution is 14.5%, in 48 DEG C of constant temperature,
Control ph is 9.3, continues stirring reaction 3.2h, obtains organic amphiprotic copolymerized macromolecule first network gel;Then carry out cold
But, in the case where nitrogen is passed through, organic amphiprotic copolymerized macromolecule first network gel 46.9g inputs 10L can be swelling in closed reactor,
In the reactor equipped with 324.3g caffeic acids, 55.9g inositol, 290.3g methacrylic acid oxygen propyl group trimellitic anhydrides ester,
The aqueous solution that the bromo DOPCP of 33.5g dimethacrylates two and 6335.3ml deionized waters are prepared, the weight of the aqueous solution
Amount concentration is 10%, the weight of first network gel(46.9g):The weight of the aqueous solution(7039.2g)=1:150, swelling 5.5h;
The aqueous solution for adding the preparation of 1.41g potassium peroxydisulfates, 7.04g pyridoxine hydrochlorides and 34.9ml deionized waters continues swelling, should
The weight concentration of the aqueous solution is 19.5%, swelling 23h;93 DEG C are warming up to after the completion of swelling, control ph is 6.5, in 93 DEG C of constant temperature
Reaction 5.6h, obtains organic amphiprotic copolymerized macromolecule interpenetrating networks gel.The gel is water insoluble, can be swelling in water, gel
Swelling ratio(ESR)=5173%(Deionized water), gel swelling rate(ESR)=5091%(The NaCl aqueous solution of weight concentration 1%).
Claims (1)
1. a kind of preparation method of organic amphiprotic copolymerized macromolecule interpenetrating networks gel, it is characterized in that can in closed reactor plus
Enter component A and deionized water stirring prepares the aqueous solution, it is 28%~62% to control the weight concentration of component A, after the completion of prepared by solution,
Relative degree of vacuum is evacuated to for -0.02MPa~-0.08MPa, after being passed through nitrogen recovery reactor to normal pressure, is added under agitation
Enter the aqueous solution prepared by B component and deionized water, the weight concentration of B component is 20%~40%, the aqueous solution charging knot of B component
Shu Hou, is warming up to 35 DEG C~50 DEG C, and the aqueous solution prepared by component C and deionized water is added under agitation, and the weight of component C is dense
It is 5%~15% to spend, and control ph is 4~10, in 35 DEG C~50 DEG C constant temperature, continues stirring reaction 2h~3.5h, obtains organic two
Property copolymerized macromolecule first network gel, then cooled down, in the case where nitrogen is passed through, by the first network gel input be equipped with D
The aqueous solution that component and deionized water are prepared can be swelling in closed reactor, the weight concentration of D components is 1.8%~11%, is pressed
Weight meter, first network gel:Weight ratio=1 of D component deionized water solutions:(95~155), swelling time is 2h~6h, then
The aqueous solution prepared by component E and deionized water is added to continue swelling, the weight concentration of component E is 10%~20%, swelling time
Be 16 h~24 h, it is swelling after the completion of, control ph is 3~7, in 75 DEG C~95 DEG C constant temperature, reacts 4h~6h, obtains organic two
Property copolymerized macromolecule interpenetrating networks gel;The component A is by MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacrylic acid oxygen
Ethyl trimellitic anhydride ester, sorbic acid composition, by the gauge of material, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride:Methyl-prop
Olefin(e) acid oxygen ethyl trimellitic anhydride ester:The ratio between amount of material of sorbic acid=(0.5~1.2):(0.3~1.6):(0.4~1.1),
B component is PEGDMA-400, and number-average molecular weight is 2000~20000, and its charged material weight is component A gross weight
2.5%~11%, component C is made up of potassium peroxydisulfate-sodium hydrogensulfite, its gross weight that feeds intake be component A gross weight 0.3%~
1.8%, by weight, potassium peroxydisulfate:Weight ratio=1 of sodium hydrogensulfite:(0.2~1.1), D components are by caffeic acid, hexamethylene six
Alcohol, methacrylic acid oxygen propyl group trimellitic anhydride ester and the bromo DOPCP of dimethacrylate two composition, by the amount of material
Meter, caffeic acid:Inositol:The ratio between amount of material of methacrylic acid oxygen propyl group trimellitic anhydride ester=(0.5~2.0):
(0.08~0.32):(0.4~1.1), by weight, the bromo DOPCP charged material weight of dimethacrylate two is coffee
Acid, inositol, three kinds the 1.8%~5.5% of total monomer weight of methacrylic acid oxygen propyl group trimellitic anhydride ester, component E is by mistake
Potassium sulfate, pyridoxine hydrochloride composition, potassium peroxydisulfate charged material weight is the 0.1%~1.2% of D component weights, pyridoxine hydrochloric acid
The salt gross weight that feeds intake is the 0.8%~5.6% of D component weights.
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CN105289316A (en) * | 2015-09-28 | 2016-02-03 | 浙江大学 | Preparation method of composite separating film filled by interpenetrating polymer network hydrogel |
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Title |
---|
李友森 主编: "《轻化工业助剂实用手册 造纸、食品、印染工业卷》", 31 July 2002, 化学工业出版社 * |
薛巍 等主编: "《生物医用水凝胶》", 31 December 2012, 暨南大学出版社 * |
金关泰 主编: "《高分子化学的理论和应用进展》", 31 March 1995, 中国石化出版社 * |
韩长日 等主编: "《精细有机化工产品生产技术手册(下卷)》", 30 June 2010, 中国石化出版社 * |
魏佳: "具有半互穿网络结构的两性吸水树脂的合成及性能研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》 * |
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