CN106031855A - Preparation and applications of carboxylate binary copolymer dispersing agents - Google Patents
Preparation and applications of carboxylate binary copolymer dispersing agents Download PDFInfo
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- CN106031855A CN106031855A CN201510120245.2A CN201510120245A CN106031855A CN 106031855 A CN106031855 A CN 106031855A CN 201510120245 A CN201510120245 A CN 201510120245A CN 106031855 A CN106031855 A CN 106031855A
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Abstract
The invention relates to a class of carboxylate binary copolymer dispersing agents and a preparation process thereof. According to the polymer, the monomer ratio is the mass ratio, and the polymer comprises 15-30 parts of alpha-methyl styrene, and 20-60 parts of an acrylic acid homologue. According to the present invention, the compound has the following advantages that the binary copolymer dispersing agent has good water solubility and good universality to the dispersing system; the alpha position of the vinyl has one methyl, such that the steric hindrance can be provided so as to provide the good dispersing effect; the dispersing agent has the ideal polymerization degree and the carboxyl group, such that the dispersed substance can be stably dispersed through the steric hindrance effect and the electrostatic repulsion so as to reduce the viscosity of the system; and the preparation process of the compound has advantages of simpleness, short production period, easily available bulk drug, low cost, no environmental pollution, industrial scale, continuous production, and the like.
Description
Technical field
The present invention is preparation technology and the application thereof of a kind of carboxylate bipolymer dispersant, belongs to the synthetic technology of new copolymer dispersant, and this polymer is applied in the industries such as pigment, coating, dyestuff, water-coal-slurry, pesticide.
Background technology
In the industries such as pigment, dyestuff, water-coal-slurry, pesticide, dispersant to by dispersed substance play dispersion and stable effect suffer from important application.Compared with dispersal agent molecule dispersant little with tradition, traditional little dispersal agent molecule is insecure in solid particles surface absorption, easily causes reassembling or precipitating from disperse medium surface dissociation.Carboxylate polymer's dispersant can make stable system by sterically hindered effect and electrostatic repulsion effect, has more preferable dispersion effect than little dispersal agent molecule；Compared with traditional lignosulfonates, naphthalenesulfonate formaldehyde condensation compound dispersant, carboxylate polymer's dispersant is insensitive to ionic strength, pH value and the temperature etc. of dispersion, can significantly reduce the viscosity of system and improve the stability of dispersion.Higher owing to preparing the polymerization activity of monomer used by this analog copolymer, the control of polymer molecular weight becomes key technology prepared by this type of dispersant.The method controlling polymer molecular weight size in the art also has: patent CN1085570 uses slaine as molecular weight regulator；Patent EP1304314 uses sulfhydryl compound to control polymer molecular weight as chain-transferring agent；Patent literary composition US4301226 polyreaction in water-isopropyl alcohol mixed solvent reaches to control the purpose etc. of polymer molecular weight.The shortcoming of these methods is: introduces impurity substances in product, affects properties of product, adds the difficulty of post processing, and production cost is expensive.
Summary of the invention
Carboxylate bipolymer dispersant, is made up of than material following masses:
α-methyl styrene
15～30 parts
Acrylic homolog
20～60 parts
Acrylic homolog includes: maleic anhydride, acrylic acid, methacrylic acid.
As a example by acrylic homolog is dry for maleic acid, the synthetic route of described carboxylate bipolymer dispersant is as follows:
The concrete operation step of the present invention is as follows:
A) in there-necked flask, add the aqueous solution of a certain amount of distilled water and chain-transferring agent, be heated to 60～90 DEG C, then drip α-methyl styrene, acrylic homolog and initiator solution, drip complete in 3～4 hours, insulation reaction 3～6 hours；Being cooled to room temperature, with the carboxylic acid in alkali and in system, dosis neutralisata is the 70～120% of carboxyl molal quantity.
Described chain-transferring agent is sodium sulfite and isopropanol, and consumption is 0.1～15 % of monomer gross mass.
Described initiator is the one in Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide, and consumption is 1～15 % of monomer gross mass.
Described alkali is one or both in sodium hydroxide, potassium hydroxide, ammonia spirit, triethylamine, triethanolamine, and dosis neutralisata is 70～120 % of carboxyl molal quantity.
The present invention is characterized by: with α-methyl styrene, acrylic homolog as primary raw material, with chain-transferring agent, initiator, alkali as auxiliary material, reacts under the conditions of 60～90 DEG C, then cools down, neutralizes with alkali, prepares destination scatter agent solution；The solid content of dispersant solution is 30～40 %.
The application technology effect of the present invention: carboxylate bipolymer dispersant of the present invention has preferable dispersion effect to inorganic particles such as titanium dioxide, calcium carbonate, aluminium oxidies；In terms of the formulations of pesticide, 25% MTI-446 SC, 25% pyrazoles ether bacterium fat SC, 600g/L imidacloprid SC there is good dispersive property simultaneously；Additionally can be applicable to disperse the aspects such as pigment, dyestuff, water-coal-slurry, have good dispersion effect equally.
Compared with prior art, beneficial effects of the present invention and novelty are as follows:
1, carboxylate bipolymer dispersant structure of the present invention is novel, belongs to novel dispersant；
2, acrylic homolog contains the hydroxy-acid group of functionalization, and the pH value of dispersion is had good adaptability；
3, carboxylate bipolymer dispersant of the present invention has the preferable degree of polymerization and carboxyl, phenyl ring functional group, is made by dispersed substance stably dispersing by space steric effect and Coulomb repulsion；
The present invention has prominent substantial technical characterstic and has significant technological progress；So the present invention is creative.
Through extensively consulting domestic and international public publication and patent documentation, there are no technical data identical with technical solution of the present invention, the present invention has novelty.The present invention has a wide range of applications in formulations of pesticide field, and the present invention has practicality.
The invention have the advantage that copolymer dispersant preparation technology is simple, processing ease, with short production cycle, with low cost, non-environmental-pollution, be suitable to industrial scale and produce.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail and completely:
Embodiment 1:
1) preparation of dispersant:
By 1000 parts of distilled waters, 10 parts of chain-transferring agents, the composition of chain-transferring agent is the sodium sulfite of 1:1.2 and isopropanol water solution joins in four mouthfuls of reaction flasks, heats while stirring；When the temperature of solution rises to 60 DEG C in reaction bulb, add 200 parts of α-methyl styrene, 500 parts of acrylic homolog and 30 parts of initiator solutions and add in 3 hours, then 60 DEG C of insulation reaction 2 hours；Insulation reaction is down to room temperature after terminating while stirring, and with the carboxylic acid in sodium hydroxide solution and in system, dosis neutralisata is 50 % of carboxyl molal quantity, prepares destination scatter agent solution.
2) dispersibility of inorganic mineral is measured by the dispersant of preparation:
In 100 ml tool plug graduated cylinders, add dispersant and 50 ml distilled water solutions prepared by 0.4 g step (1), after dispersant dissolves, add 1.00 g treat scattered solid particle, then add aqueous solution to 100
Ml, turns upside down in 1 min 30 times, first overturns 180 °, and returning is 1 time in situ.Graduated cylinder is vertically disposed in 25 DEG C of constant temperature water baths, static friction, it is to avoid sunlight direct irradiation, 30
During min, extract upper strata 90 ml suspension out with suction pipe, complete in 15 s.The quality that remaining 10 ml suspensions are transferred to weighed is m1Desiccation culture ware in, and rinse graduated cylinder with distilled water solution, it is ensured that the precipitum in graduated cylinder is transferred completely in culture dish, and culture dish is put into 80 DEG C of drying in baking oven, and weigh m2 , calculate the mass M of insoluble matter, M=m2- m1, its suspensibility according to the following formula:
Wherein: M is 100
Dispersant and the quality (g) of solid particle contained by 10 ml suspensions bottom ml tool plug graduated cylinder, 1.400 is contained dispersant and the gross mass (g) of solid particle in 100 ml tool plug graduated cylinders；
By aforesaid operations step, recording prepared dispersant to the suspensibility of calcium carbonate suspension is 99.20 %, and prepared dispersant is 99.5 % to the suspensibility of aluminium sesquioxide suspension.
3) dispersibility of pesticide is measured by described dispersant:
Pesticide suspension concentrate (SC) is prepared with above-mentioned dispersant, weigh 1.0 g this pesticide SC in beaker, add 50 ml distilled water solutions, place 30 s, stir 30 s with Glass rod to be allowed to be uniformly dispersed, then with distilled water solution, this suspension is transferred in 100 ml tool plug graduated cylinders, adds distilled water solution to 100
At ml.Covering stopper, turned upside down 30 times by tool plug graduated cylinder in 1 min, graduated cylinder turns upside down 180 °, and to return be in situ 1 time.Graduated cylinder is vertically disposed in 30 DEG C of super thermostatted water solution bath, static friction, it is to avoid sunlight direct irradiation, after standing 30 min, with suction pipe removal upper strata 90 ml suspension, this process makes tip at several millimeters under liquid level, to guarantee not shake or stir the precipitum bottom graduated cylinder.The quality that remaining 10 ml suspensions are transferred to weighed is m1 Culture dish in, and rinse graduated cylinder with distilled water solution, it is ensured that the precipitum bottom graduated cylinder is transferred completely in culture dish, and culture dish is put into 80 DEG C of drying in baking oven, and weigh m2, calculate the mass M=(m of insoluble matter2-m1), then it is calculated as follows suspensibility:
Wherein, 1.0 is the quality of aqueous suspension agent (SC) added；Effective content is the percentage composition of SC Pesticides；M is the quality of precipitum bottom tool plug graduated cylinder；
By aforesaid operations step, recording above-mentioned dispersant to the suspensibility of 43% Tebuconazole aqueous suspension agent is 98.6%.
Embodiment 2:
By 1000 parts of distilled waters and 80 parts of chain-transferring agents, the composition of chain-transferring agent is the sodium sulfite of 1:1.1 and isopropanol water solution joins in four mouthfuls of reaction flasks, heats while stirring；When the temperature of solution rises to 70 DEG C in reaction bulb, add 200 parts of α-methyl styrene, 400 parts of acrylic homolog and 60 parts of initiator solutions and add in 5 hours, then insulation reaction 3 hours；Insulation reaction is down to room temperature after terminating while stirring, and with the carboxylic acid in sodium hydroxide solution and in system, dosis neutralisata is the 75% of carboxyl molal quantity, prepares destination scatter agent solution；
Operating procedure as described in embodiment 1, recording above-mentioned dispersant to the suspensibility of calcium carbonate suspension is 96.24
%, the suspensibility to aluminium sesquioxide suspension is 96.49 %, and the suspensibility to 43% Tebuconazole aqueous suspension agent is 97.12%.
Embodiment 3:
By 1000 parts of distilled waters and 20 parts of chain-transferring agents, the composition of chain-transferring agent is the sodium sulfite of 1:0.8 and isopropanol water solution joins in four mouthfuls of reaction flasks, heats while stirring；When the temperature of solution rises to 80 DEG C in reaction bulb, add 150 parts of α-methyl styrene, 500 parts of acrylic homolog and 60 parts of initiator solutions and add in 2 hours, then insulation reaction 5 hours；Insulation reaction is down to room temperature after terminating while stirring, and with the carboxylic acid in sodium hydroxide solution and in system, dosis neutralisata is the 90% of carboxyl molal quantity, prepares destination scatter agent solution；
Operating procedure as described in embodiment 1, recording above-mentioned dispersant to the suspensibility of calcium carbonate suspension is 98.26
%, the suspensibility to aluminium sesquioxide suspension is 97.38 %, and the suspensibility to 43% Tebuconazole aqueous suspension agent is 97.34%.
Embodiment 4:
By 1000 parts of distilled waters and 40 parts of chain-transferring agents, the composition of chain-transferring agent is sodium sulfite and the isopropanol water solution of 1:1, joins in four mouthfuls of reaction flasks, heats while stirring；When the temperature of solution rises to 70 DEG C in reaction bulb, add 90 parts of α-methyl styrene, 410 parts of acrylic homolog and 30 parts of initiator solutions and add in 2 hours, then insulation reaction 3 hours；Insulation reaction is down to room temperature after terminating while stirring, and with the carboxylic acid in sodium hydroxide solution and in system, dosis neutralisata is 110 % of carboxyl molal quantity, prepares destination scatter agent solution；
Operating procedure as described in embodiment 1, recording above-mentioned dispersant to the suspensibility of calcium carbonate suspension is 99.69
%, the suspensibility to aluminium sesquioxide suspension is 98.64 %, and the suspensibility to 43% Tebuconazole aqueous suspension agent is 98.53%.
Embodiment 5:
By 1000 parts of distilled waters and 40 parts of chain-transferring agents, the composition of chain-transferring agent is sodium sulfite and the isopropanol water solution of 1:1, joins in four mouthfuls of reaction flasks, heats while stirring；When the temperature of solution rises to 90 DEG C in reaction bulb, add 300 parts of α-methyl styrene, 300 parts of acrylic homolog and 40 parts of initiator solutions and add in 3 hours, then insulation reaction 4 hours；Insulation reaction is down to room temperature after terminating while stirring, and with the carboxylic acid in sodium hydroxide solution and in system, dosis neutralisata is 90 % of carboxyl molal quantity, prepares destination scatter agent solution；
Operating procedure as described in embodiment 1, recording above-mentioned dispersant to the suspensibility of calcium carbonate suspension is 98.63
%, the suspensibility to aluminium sesquioxide suspension is 98.58 %, and the suspensibility to 43% Tebuconazole aqueous suspension agent is 96.27%.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have change and change.All within the spirit and principles in the present invention, any amendment of being made, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. carboxylate bipolymer dispersant, is made up of than material following masses:
α-methyl styrene
15～30 parts
Acrylic homolog
20～60 parts.
2. according to claim 1, acrylic homolog includes: maleic anhydride, acrylic acid, methacrylic acid.
3. the preparation technology of carboxylate bipolymer dispersant, step is as follows:
In there-necked flask, add the aqueous solution of a certain amount of distilled water and chain-transferring agent, be heated to 60～90 DEG C, then drip α-methyl styrene, acrylic homolog and initiator solution, drip complete in 3～4 hours, insulation reaction 3～6 hours；Being cooled to room temperature, with the carboxylic acid in alkali and in system, dosis neutralisata is the 70～120% of carboxyl molal quantity.
The preparation technology of carboxylate bipolymer dispersant the most according to claim 3, it is characterised in that: described initiator is the one in Ammonium persulfate., potassium peroxydisulfate, hydrogen peroxide, and consumption is the 1～15% of monomer gross mass.
The preparation technology of carboxylate bipolymer dispersant the most according to claim 3, it is characterised in that: described chain-transferring agent is sodium sulfite and isopropanol, and consumption is the 0.1～15% of monomer gross mass.
The preparation technology of carboxylate bipolymer dispersant the most according to claim 3, it is characterized in that: described alkali is one or both in sodium hydroxide, potassium hydroxide, ammonia spirit, triethylamine, triethanolamine, dosis neutralisata is the 70～120% of carboxyl molal quantity.
7. the application of bipolymer dispersant described in claim 1, can be applicable to disperse the aspects such as pigment, dyestuff, water-coal-slurry, has good dispersion effect；It is characterized in that: described dispersant has good dispersion effect to water-coal-slurry suspension, the inorganic particles such as titanium dioxide, calcium carbonate, aluminium oxide are had preferable dispersion effect；In terms of the formulations of pesticide, 25% MTI-446 SC, 25% pyrazoles ether bacterium fat SC, 600g/L imidacloprid SC have good dispersive property simultaneously.
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| CN201510120245.2A CN106031855A (en) | 2015-03-19 | 2015-03-19 | Preparation and applications of carboxylate binary copolymer dispersing agents |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758391A (en) * | 2016-12-22 | 2017-05-31 | 绍兴海成化工有限公司 | Multifunctional dyeing auxiliary agent and the dyeing using the multifunctional dyeing auxiliary agent |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230209A (en) * | 2007-12-24 | 2008-07-30 | 上海东升新材料有限公司 | Dispersant for wet grinding of heavy calcium carbonate and preparation method thereof |
| CN101323651A (en) * | 2008-07-24 | 2008-12-17 | 上海东升新材料有限公司 | Acrylic acid series polymer dispersants, preparation and use thereof |
| US20090163635A1 (en) * | 2007-12-19 | 2009-06-25 | Eastman Chemical Company | Aqueous dispersions of adhesion promoters |
| CN103172788A (en) * | 2013-03-26 | 2013-06-26 | 段海宝 | Preparation method of dispersing agent |
-
2015
- 2015-03-19 CN CN201510120245.2A patent/CN106031855A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090163635A1 (en) * | 2007-12-19 | 2009-06-25 | Eastman Chemical Company | Aqueous dispersions of adhesion promoters |
| CN101230209A (en) * | 2007-12-24 | 2008-07-30 | 上海东升新材料有限公司 | Dispersant for wet grinding of heavy calcium carbonate and preparation method thereof |
| CN101323651A (en) * | 2008-07-24 | 2008-12-17 | 上海东升新材料有限公司 | Acrylic acid series polymer dispersants, preparation and use thereof |
| CN103172788A (en) * | 2013-03-26 | 2013-06-26 | 段海宝 | Preparation method of dispersing agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758391A (en) * | 2016-12-22 | 2017-05-31 | 绍兴海成化工有限公司 | Multifunctional dyeing auxiliary agent and the dyeing using the multifunctional dyeing auxiliary agent |
| CN106758391B (en) * | 2016-12-22 | 2018-02-13 | 绍兴海成化工有限公司 | Multifunctional dyeing auxiliary agent and the dyeing using the multifunctional dyeing auxiliary agent |
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Application publication date: 20161019 |