CN106749907A - A kind of block polymer dispersant of ATRP technologies synthesis - Google Patents
A kind of block polymer dispersant of ATRP technologies synthesis Download PDFInfo
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- CN106749907A CN106749907A CN201611053233.3A CN201611053233A CN106749907A CN 106749907 A CN106749907 A CN 106749907A CN 201611053233 A CN201611053233 A CN 201611053233A CN 106749907 A CN106749907 A CN 106749907A
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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
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
- C08F293/005—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule using free radical "living" or "controlled" polymerisation, e.g. using a complexing agent
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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
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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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
- C08F2438/00—Living radical polymerisation
- C08F2438/01—Atom Transfer Radical Polymerization [ATRP] or reverse ATRP
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The present invention relates to a kind of block polymer dispersant of ATRP technologies synthesis, obtained block polymer dispersant adjustable molecular weight, narrow molecular weight distribution, due to being easy in pulp particle adsorption containing anchoring group sulfonic group and amino and play peptizaiton, and discharge the hydrone of aquation Cation adsorption in slurry, so as to reduce the viscosity of slurry, and thixotroping is less likely to occur；The present invention also provides a kind of preparation method of the block polymer dispersant of ATRP technologies synthesis, with process is simple, reaction condition is gentle, one-step method is obtained a kind of aqueous block polymer dispersant of narrow molecular weight distribution, can be used for coating industry, printing industry, energy electronic industry, ceramic industry, color stuffing industry, commodity industry.
Description
Technical field
The present invention relates to a kind of preparation method of dispersant, and in particular to a kind of ATRP ATRP skills
The block polymer dispersant of art synthesis, belongs to macromolecule dispersing agent synthesis technical field.
Background technology
Dispersant as important source material in water-based system such as coating, ink, ceramic glaze and blank, pesticidal preparations, its
The quality of quality determines in coating that can colouring agent dispersed in system and keep stabilization, determines bending for coating completely
Gloss, covering power of clothes value and film etc., determine viscosity, flowing and the thixotropic property of Glaze Slip, also determine agricultural chemicals system
Can agent Pesticides particle be dispersed in water uniform high-efficiency, not reduce drug effect.
Macromolecule dispersing agent structure influences larger to dispersion effect.Usually, in water-based system be applicable hyper-dispersant by
Chain segment and hydrophilic segment two parts are constituted, and to reach good dispersion effect, hydrophilic segment molecular weight general control is 1000
~3000 or so, hydrophilic chain is long, and hyper-dispersant molecule easily comes off from surface of pigments, and hydrophilic chain is easily twined with hydrophilic interchain
Tie and cause flocculation；The molecular weight general control of chain segment is 2000~5000 or so, and chain segment is long, often because cannot be complete
It is adsorbed in particle surface and cyclization or is combined with adjacent particles surface, causes interparticle " bridge formation " flocculation.Additionally, macromolecule point
The suitable proportion of hydrophilic segment is 20%~40% in powder molecule segment, if hydrophilic segment ratio is too high, dispersant is molten
Agentization is too strong, and the adhesion between particle and dispersant is relative to be weakened, and dispersant is easy to fall off；If otherwise the ratio mistake of hydrophilic segment
Low, dispersant cannot be completely dissolved in water, poor compatibility, and dispersion effect declines.
Ceramic dispersants are also ceramic water reducing agent, as a part for macromolecule dispersing agent, in glaze field, blank field
Have a wide range of applications.Because polymer ceramic dispersants hydrophobic group, the position of hydrophilic group, size and quantity are adjustable, molecule knot
Structure can be in pectination, highly branched chain etc., therefore disperse particles surface is covered polymer ceramic dispersants and encapsulating effect is than nothing
Machine ceramic dispersants are much better than, dispersion is more stable, dispersion adaptability is more extensive, and polymer ceramic dispersants are
As up-and-coming class dispersant with high efficiency.
Mainly there are ICI, KvK, Dupont, BASF, BYK in external exploitation at present, the company of development macromolecule dispersing agent,
The companies such as Daniel, SunChemical.The domestic research to macromolecule dispersing agent is started late, and dispersant is few, synthesis side
Method is also immature, and the product performance of its exploitation cannot also fully meet use requirement, still need to a large amount of import external products.Cause
This, the macromolecule dispersing agent of exploitation and development function admirable is significant.
The research such as Yang Jianhong finds can when the addition metering of Sodium Polyacrylate is 0.6%~0.8% in potter's clay
The solidifying effect of preferably solution is obtained, this report haves the shortcomings that addition is bigger than normal.
China Patent No. CN201410316056.8 is related to a kind of Ceramic manufacturing polyalcohol water reducing agent and its synthetic method,
Characterized in that, first that macromolecular unsaturated monomer and unsaturated acids containing long polyether chains is common under radical initiator effect
It is poly-, another part unsaturated acids and radical initiator are subsequently adding, proceed polymerisation, neutrality is finally neutralized to, i.e.,
Can obtain polyalcohol water reducing agent of the invention.The polyalcohol water reducing agent water-reducing rate is high, dispersion and plasticizing capacity are strong, can be applied to pottery
The technical process such as powder processed, the injection forming of porcelain industry.
But from the point of view of existing patent with technical matters, ceramic industry dispersant has that dispersion efficiency is low, dispersant product
Can be unstable.
The content of the invention
To overcome the shortcoming and defect of prior art, the present invention to provide a kind of ATRP ATRP technologies and close
Into block polymer dispersant and preparation method thereof.
Described ATRP (ATRP polymerization method) be with simple organohalogen compounds as initiator, transition
Metal complex is halogen atom carrier, by redox reaction, reversible dynamic is set up between spike and dormancy kind and is put down
Weighing apparatus, it is achieved thereby that the control to polymerisation, by the block polymer dispersant that ATRP technologies synthesize can be used for coating industry,
Printing industry, energy electronic industry, ceramic industry, color stuffing industry, commodity industry.
A kind of block polymer dispersant of ATRP technologies synthesis of the invention, its preparation method is as follows：
A) under inert gas shielding, by 0.1~0.8 part of initiator, 0.2~1.6 part of catalyst, 0.1~1.0 part match somebody with somebody
Body, 0.05~0.1 part of surfactant, 100.0~500.0 parts of water, 20.0~40.0 parts of polymerized monomers are added to reaction unit
In, heated up stirring, and ATRP polymerization reaction 6h~24h is carried out at 40~95 DEG C, obtains a polymer solution；
B) excessive methyl alcohol is added in above-mentioned polymer solution, stirring is stopped after stirring, standing allows it to precipitate, mistake
Filter, washing to halogen-free ionic, vacuum drying are obtained a kind of narrower block polymer dispersant of molecular weight distribution.
Wherein, described initiator is 2- chlorine propionamide, 2- bromines propionamide, 2- bromopropenes acetoacetic ester, propylene bromide acid second
One or more in ester, 2- isobutyl ethyl bromides, 2- bromopropene acetoacetic esters；Further, it is preferable to be 2- chlorine propionyl
Amine or 2- bromines propionamide or the mixture of the two.
Described catalyst be cuprous bromide, stannous chloride, cuprous bromide, copper bromide in one or more；Enter
One step ground, preferably stannous chloride.
Described part be 2,2 '-bipyridyl, N, N, N ', N ', N "-PMDETA, N, N, N ', N ', N "-
Pentamethyl methyl acrylate base diethylene triamine, N, N, N ', N ', N ", N " and-hexamethyl n-butyl acrylate base trivinyl four
Amine, N, N, N ', N ', N ", N " and one or more in-hexamethyl methyl acrylate base triethylene tetraamine；Further,
Preferably 2,2 '-bipyridyl.
Described surfactant is neopelex, fatty glyceride, fatty acid sorbitan, polyvinyl alcohol
In one or more.
Described polymerized monomer is sodium p styrene sulfonate, the mixture of N- caprolactams, and its mass ratio is
0.2:1~0.8:1.
A kind of preparation side of the block polymer dispersant of ATRP ATRP technologies synthesis of the invention
Method, with process is simple, reaction condition is gentle, and one-step synthesis method is obtained a kind of aqueous block polymer of narrow molecular weight distribution
Dispersant.
A kind of block polymer dispersant of ATRP ATRP technologies synthesis of the invention, action principle
It is as follows：Glaze slip particle diameter in grinding is smaller (10 microns), due to the macromolecule using the synthesis of conventional free radical polymerization technique
Dispersant molecule amount wider distribution, the glaze slurry viscosity after grinding is bigger than normal and thixotroping is serious.The dispersant point prepared using the present invention
Son measures adjustable, narrow molecular weight distribution, and due to being easy in frit particles adsorption simultaneously containing anchoring group sulfonic group and amino
Peptizaiton is played, and the hydrone of aquation Cation adsorption in glaze slip is discharged, reduce the viscosity of glaze slip, and be not easy
Generation thixotroping.
A kind of block polymer dispersant of ATRP ATRP technologies synthesis of the invention, application method
For：The dispersant of the invention that glaze slip total amount 0.1%~0.3% will be accounted for is added to be ground into glaze slip and requires particle diameter, or will
The dispersant of the invention for accounting for glaze slip total amount 0.1%~0.3% is added to stirring in high viscosity glaze slip, then enters this glaze slip
Common process glazing, is calcined the Ceramic glaze effect for obtaining better than the glazing effect for adding conventional dispersant.
Specific embodiment
The block polymer dispersant that a kind of ATRP technologies of the invention synthesize is done further with reference to embodiment
Description.It is understood that specific embodiment described herein is used only for explaining related invention, rather than to the limit of the invention
It is fixed.
Embodiment 1
A kind of block polymer dispersant of ATRP technologies synthesis, its preparation technology is as follows：
A) under the conditions of inert atmosphere protection, by 0.2 part of 2- chlorine propionamide, 0.1 part of cuprous bromide, 0.3 part of stannous chloride,
0.2 part 2,2 '-bipyridyl, 0.05 part of fatty glyceride, 300 parts of water, 6 parts of sodium p styrene sulfonates, 20 parts of N- vinyl oneself
Lactams is added in reaction unit, and heat up stirring, and ATRP polymerization reaction 14h is carried out at 70~75 DEG C, obtains reactant solution.
B) excessive methyl alcohol being added in a polymer solution, stirring being stopped after stirring, standing allows it to precipitate, filtering,
Washing to halogen-free ionic, vacuum drying is obtained a kind of narrower block polymer dispersant of molecular weight distribution.
0.1 part of above-mentioned diblock copolymer dispersant is added into 100 parts of ground glaze slips stirring, glaze slip is applying -4
Flowing time has 59s to be reduced to 36s in cup；Above-mentioned glaze slip enters common process glazing, is calcined the Ceramic glaze effect for obtaining excellent
In the glazing effect for adding conventional dispersant.
Embodiment 2
A kind of block polymer dispersant of ATRP technologies synthesis, its preparation technology is as follows：
A) under the conditions of inert atmosphere protection, by 0.4 part of 2- bromine propionamide, 0.4 part of 2- chlorine propionamide, 1.3 parts of protobromides
Copper, 0.4 part 2,2 '-bipyridyl, 0.05 part of neopelex, 400 parts of water, 10 parts of sodium p styrene sulfonates, 20 parts of N-
Caprolactam is added in reaction unit, and heat up stirring, and ATRP polymerization reaction 12h is carried out at 80~85 DEG C, is obtained instead
Answer thing solution.
B) excessive methyl alcohol being added in a polymer solution, stirring being stopped after stirring, standing allows it to precipitate, filtering,
Washing to halogen-free ionic, vacuum drying is obtained a kind of narrower block polymer dispersant of molecular weight distribution.
0.2 part of above-mentioned two pincers section copolymer dispersant is added into 100 parts of ground glaze slips stirring, glaze slip is applying -4
Flowing time has 59s to be reduced to 30s in cup；Above-mentioned glaze slip enters common process glazing, is calcined the Ceramic glaze effect for obtaining excellent
In the glazing effect for adding conventional dispersant.
Embodiment 3
A kind of block polymer dispersant of ATRP technologies synthesis, its preparation technology is as follows：
A) under the conditions of inert atmosphere protection, at a certain temperature by 0.3 part of initiator, 1.0 parts of catalyst, 0.1 part of N,
N, N ', N ', N "-PMDETA, 0.1 part of polyvinyl alcohol, 200 parts of water, 6 parts of sodium p styrene sulfonates, 15 parts of N-
Caprolactam is added in reaction unit, and heat up stirring, and ATRP polymerization reaction 24h is carried out at 80~85 DEG C, is obtained instead
Answer thing solution.
B) excessive methyl alcohol being added in a polymer solution, stirring being stopped after stirring, standing allows it to precipitate, filtering,
Washing to halogen-free ionic, vacuum drying is obtained a kind of narrower block polymer dispersant of molecular weight distribution.
0.2 part of above-mentioned two pincers section copolymer dispersant is added into 100 parts of ground glaze slips stirring, glaze slip is applying -4
Flowing time has 59s to be reduced to 32s in cup；Above-mentioned glaze slip enters common process glazing, is calcined the Ceramic glaze effect for obtaining excellent
In the glazing effect for adding conventional dispersant.
Above description is only the preferred embodiment and the explanation to institute's application technology principle of the application.People in the art
Member is it should be appreciated that involved invention scope in the application, however it is not limited to the technology of the particular combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where the inventive concept is not departed from, is carried out by above-mentioned technical characteristic or its equivalent feature
Other technical schemes for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (9)
1. the block polymer dispersant that a kind of ATRP technologies synthesize, it is characterised in that：Described block polymer dispersant, its
Preparation method is as follows：
A) under inert gas shielding, by 0.1~0.8 part of initiator, 0.2~1.6 part of catalyst, 0.1~1.0 part of part,
0.05~0.1 part of surfactant, 100.0~500.0 parts of water, 20.0~40.0 parts of polymerized monomers are added in reaction unit,
Heated up stirring, and ATRP polymerization reaction 6h~24h is carried out at 40~95 DEG C, obtains a polymer solution；
B) excessive methyl alcohol is added in above-mentioned polymer solution, stirring is stopped after stirring, standing allows it to precipitate, filtering,
Washing to halogen-free ionic, vacuum drying is obtained a kind of narrower block polymer dispersant of molecular weight distribution.
2. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described draws
Hair agent is 2- chlorine propionamide, 2- bromines propionamide, 2- bromopropenes acetoacetic ester, propylene bromide acetoacetic ester, 2- isobutyl ethyl bromides, 2-
One or more in bromopropene acetoacetic ester.
3. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described draws
Hair agent is 2- chlorine propionamide or 2- bromines propionamide or the mixture of the two.
4. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described urges
Agent be cuprous bromide, stannous chloride, cuprous bromide, copper bromide in one or more.
5. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described urges
Agent is stannous chloride.
6. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described
Part is 2,2 '-bipyridyl, N, N, N ', N ', N "-PMDETA, N, N, N ', N ', N "-pentamethyl acrylic acid first
Ester group diethylene triamine, N, N, N ', N ', N ", N "-hexamethyl n-butyl acrylate base triethylene tetraamine, N, N, N ', N ',
One or more in N ", N "-hexamethyl methyl acrylate base triethylene tetraamine.
7. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described
Part is 2,2 '-bipyridyl.
8. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described table
Face activating agent be neopelex, fatty glyceride, fatty acid sorbitan, polyvinyl alcohol in one or two with
On.
9. the block polymer dispersant that a kind of ATRP technologies as claimed in claim 1 synthesize, it is characterised in that：Described is poly-
The mixture that monomer is sodium p styrene sulfonate and N- caprolactams is closed, its mass ratio is 0.2:1~0.8:1.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537401A (en) * | 2017-08-20 | 2018-01-05 | 湖南七纬科技有限公司 | A kind of sulfonate type block copolymer dispersant and preparation method thereof |
| CN108659166A (en) * | 2018-06-19 | 2018-10-16 | 湖南辰砾新材料有限公司 | A kind of combed block copolymer ceramic water reducing agent of ATRP technologies |
| CN109369060A (en) * | 2018-09-28 | 2019-02-22 | 合众（佛山）化工有限公司 | A kind of combed block copolymer ceramic water reducing agent of ATRP technology |
| CN109942754A (en) * | 2019-03-05 | 2019-06-28 | 北京工业大学 | The method that atom transfer radical polymerization prepares retardation setting type super plasticizer |
| CN113336894A (en) * | 2021-07-05 | 2021-09-03 | 扬州市立达树脂有限公司 | High molecular dispersant and preparation method thereof |
| CN114213563A (en) * | 2022-01-12 | 2022-03-22 | 山东理工大学 | Efficient and controllable preparation method of sodium poly (p-styrene) sulfonate |
| CN114369212A (en) * | 2021-12-10 | 2022-04-19 | 复旦大学 | High molecular dispersant for pigment and its multi-step synthesis process and application |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537401A (en) * | 2017-08-20 | 2018-01-05 | 湖南七纬科技有限公司 | A kind of sulfonate type block copolymer dispersant and preparation method thereof |
| CN108659166A (en) * | 2018-06-19 | 2018-10-16 | 湖南辰砾新材料有限公司 | A kind of combed block copolymer ceramic water reducing agent of ATRP technologies |
| CN109369060A (en) * | 2018-09-28 | 2019-02-22 | 合众（佛山）化工有限公司 | A kind of combed block copolymer ceramic water reducing agent of ATRP technology |
| CN109942754A (en) * | 2019-03-05 | 2019-06-28 | 北京工业大学 | The method that atom transfer radical polymerization prepares retardation setting type super plasticizer |
| CN109942754B (en) * | 2019-03-05 | 2021-06-25 | 北京工业大学 | Method for preparing delayed coagulation type superplasticizer by atom transfer radical polymerization |
| CN113336894A (en) * | 2021-07-05 | 2021-09-03 | 扬州市立达树脂有限公司 | High molecular dispersant and preparation method thereof |
| CN114369212A (en) * | 2021-12-10 | 2022-04-19 | 复旦大学 | High molecular dispersant for pigment and its multi-step synthesis process and application |
| CN114213563A (en) * | 2022-01-12 | 2022-03-22 | 山东理工大学 | Efficient and controllable preparation method of sodium poly (p-styrene) sulfonate |
| CN114213563B (en) * | 2022-01-12 | 2023-09-01 | 山东理工大学 | Method for preparing sodium poly (p-styrenesulfonate) in high-efficiency controllable manner |
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Application publication date: 20170531 |