CN106543320A - A kind of RAFT methods prepare the method and its product of high-efficiency coarse whiting ground dispersant and application - Google Patents
A kind of RAFT methods prepare the method and its product of high-efficiency coarse whiting ground dispersant and application Download PDFInfo
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- CN106543320A CN106543320A CN201510600908.0A CN201510600908A CN106543320A CN 106543320 A CN106543320 A CN 106543320A CN 201510600908 A CN201510600908 A CN 201510600908A CN 106543320 A CN106543320 A CN 106543320A
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Abstract
A first aspect of the present invention, there is provided a kind of method that RAFT methods prepare high-efficiency coarse whiting ground dispersant, comprises the steps:(1) a certain amount of solvent is added in reaction vessel, and adds reactant：Vinyl carboxylic acid monomer, polythio ester chain-transferring agent, initiator, and nitrogen bubble certain hour is used, seal afterwards；(2) it is heated to uniform temperature reaction certain hour；(3) reaction is distilled off solvent after terminating；(4) add a small amount of water dilution, the pH of one or more base reagent regulation system is added to 5～8, and the regulation polymer solution solid content that adds water is to mass percent 24%～26%, you can obtain high-efficiency coarse whiting ground dispersant.Present invention also offers a kind of high-efficiency coarse whiting ground dispersant prepared according to said method, and application of the dispersant in the wet grinding production of ultrafine heavy calcium.
Description
Technical field
The present invention relates to a kind of preparation method of coarse whiting ground dispersant, more particularly to a kind of RAFT methods preparation height
The application of the method for effect coarse whiting ground dispersant and the product prepared according to the method and the product.
Background technology
Dispersant is had been widely used in the middle of the wet grinding production of ultrafine heavy calcium, can significantly reduce triple superphosphate slurry
The stability of slurry is instead glued, is increased in the grinding viscosity of material, reduction after grinding, for reduction wears away and raising product product
Matter suffers from important function.
Most coarse whiting ground dispersants are all polycarboxylic acids sodium water solutions in the market, and reaction initiator is mostly
Inorganic sodium salt, in N-process it is mostly be using sodium hydrate aqueous solution neutralizing, so as in the above process
Introduce substantial amounts of free counterion sodium ion.Research shows that dispersant mechanism is mainly due to dispersant
The Coulomb repulsion effect and steric effect of calcium carbonate surface formation are attached to, the introducing of free counterion can have
Effect reduces electrostatic repulsion so as to reduce the performance of dispersant.
If calcium hydroxide or magnesium hydroxide are introduced in N-process, due to the polycarboxylic acids salinity in calcium, magnesium
In prose style free from parallelism system, calcium, magnesium ion degree of freedom it is low, and have the extraordinary compatibility with Calcium Carbonate grinding system,
Therefore free counterion effect can be reduced, so as to improve the dispersive property of dispersant.
The topmost synthetic method of traditional dispersant is traditional solution free radical polymerization.But the polymerization institute
The molecular weight distribution of synthesis is very wide, and poor to molecular weight control.According to the literature, dispersant
Molecular weight and its distribution are had a very big impact for its dispersion effect.J.Loiseau[Macromolecules 2003,
36,3066-3077] result of study shows, is close to the monodispersed sodium polyacrylate of molecular weight and gathers than polydisperse
Sodium acrylate has more preferable peptizaiton, and the former can be adsorbed onto the surface of calcium carbonate particle with irreversible whole
On, so as to realize disperseing Calcium Carbonate well；And the latter can only partially selectively be adsorbed onto calcium carbonate particle table
Face, the utilization ratio of dispersant substantially reduce, or even precipitation occurs.Therefore, synthesize a kind of molecular weight distribution
For raising, its grinding and dispersion effect tool to Calcium Carbonate is of great significance very narrow sodium polyacrylate.
Reversible-addition-fracture chain tra nsfer (RAFT) polymerization is a kind of excellent activity-control polymerization, should
Method can effectively synthesize the polymer of target molecular weight, can be accurately obtained by the regulation to reaction condition
The polymer of target molecular weight and while can ensure that very narrow molecular weight distribution；With the original for being equally living polymerization
Sub- transfer radical polymerization method is compared, and RAFT methods have the advantage that：System is drawn without introducing halogenated hydrocarbons
It is light trigger to send out agent；Do not need the halogenide of transition metal as catalyst, without introducing impurity mantoquita, keep away
Subsequent treatment is exempted from；Without introducing part, post processing is simple；Reaction condition is gentleer.Therefore, inventor Jing
Cross analysis and test, decision adopts RAFT methods to prepare a kind of high-efficiency coarse whiting ground dispersant.
The content of the invention
In order to overcome above-mentioned problems of the prior art, a first aspect of the present invention, there is provided a kind of
The method that RAFT methods (reversible-addition-fracture chain transfer polymerization method) prepare high-efficiency coarse whiting ground dispersant, its
It is characterised by, comprises the following steps：
(1) a certain amount of solvent is added in reaction vessel, and adds reactant：Vinyl carboxylic acid monomer, many sulfur
For ester chain-transferring agent, initiator, and nitrogen bubble certain hour is used, sealed afterwards；
(2) it is heated to uniform temperature reaction certain hour；
(3) reaction is distilled off solvent after terminating；
(4) add a small amount of water dilution, the pH of one or more base reagent regulation system is added to 5～8, and added water
Polymer solution solid content is adjusted to 24%～26%, you can obtain high-efficiency coarse whiting ground dispersant.
Preferably, the mass fraction of each reactant is as follows：
30～100 parts of vinyl carboxylic acid monomer
0.2～5 part of polythio ester chain-transferring agent
0.01～2 part of initiator
Also, the consumption of solvent causes the concentration of vinyl carboxylic acid monomer to remain 1～8mol/L.
It is further preferred that in the step (1), the nitrogen bubble certain hour is 15-30 minutes；
In the step (2), the uniform temperature is 60～80 degrees Celsius, and the certain hour is 8 to 16 hours；
In the step (3), the distillation is vacuum distillation.
It is further preferred that in the step (4), the base reagent is selected from：Calcium hydroxide solid, hydrogen-oxygen
Change magnesium solid, sodium hydroxide solution, also, its addition is according to following mass fraction：
Sodium hydroxide solution 10-100 parts
0～100 part of calcium hydroxide
0～100 part of magnesium hydroxide.
It is further preferred that the vinyl carboxylic acid monomer is acrylic acid or methacrylic acid.
It is further preferred that the polythio ester chain-transferring agent is selected from dithiobenzoic acid cyano group isopropyl ester, 4-
Cyano group -4- dithio benzoyloxy valeric acids, 2- (dodecyl dihydrogen thiocarbonate. ester group) -2 Methylpropionic acid,
One kind in 2- (dodecyl trithiocarbonate) -2- isopropylformic acid .s, 4- cyano group -4- lauryl trithio carbonic esters or
Person is various.
It is further preferred that the initiator is different selected from azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo two
One or more in butyl valeric acid, dibenzoyl peroxide, cyclohexanone peroxide, tert-butyl hydroperoxide.
It is further preferred that the solvent selected from tetrahydrofuran, benzene, toluene, DMF,
One or more in ethylbenzene, dimethylbenzene, 1,4- dioxane.
In addition, above all of mass fraction is 100% calculating according to raw material effective content and indicates, it is real
Actually active content conversion of the border used in amounts according to raw material.
A second aspect of the present invention, there is provided one kind has used high-efficiency coarse whiting ground obtained in any of the above-described kind of method
Dispersant.
A kind of a third aspect of the present invention, there is provided wet method of above-mentioned high-efficiency coarse whiting ground dispersant in ultrafine heavy calcium
Application in grinding production.
Certainly, the dispersant with high efficiency for being obtained according to said method, can be not only used for coarse whiting ground, it can also be used to light
Calcium disperses.The calcium carbonate superfine powder of gained can be used for papermaking, coating, plastics, rubber, fluid sealant, medicine, food
The field such as product and cosmetics.
Method synthetic molecular weight that the present invention is polymerized using reversible-addition-fracture chain tra nsfer (RAFT) is controllable,
The narrower polyvinyl carboxylic acid of molecular weight distribution, then base reagent is introduced in N-process, so as to obtain polyethylene
Yl carboxylic acid salt high-efficiency coarse whiting ground dispersant.
Heretofore described method compared with prior art, with advantages below and beneficial effect：
(1) the method advantage compared with the radical polymerization of the traditional dispersant of synthesis is that molecular weight is controllable, molecule
Amount narrow distribution, does not introduce free counterion in elicitation procedure；
(2) the method is compared with being equally the atom transfer radical polymerization method of living polymerization, system without
Introduce halogenated hydrocarbons；The halogenide of transition metal is not needed as catalyst, without introducing impurity mantoquita, it is to avoid
Subsequent treatment；Without introducing part, post processing is simple；Calcium hydroxide/magnesium hydroxide used in N-process,
Effectively reduce impact of the free counterion to calcium carbonate dispersion system.
Comprehensive above advantage, it is known that, the dispersant obtained using the method also has excellent performance.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following enforcement
Mode.
A first aspect of the present invention, there is provided a kind of method that RAFT methods prepare high-efficiency coarse whiting ground dispersant,
Characterized in that, comprising the following steps：
(1) a certain amount of solvent is added in reaction vessel, and adds reactant：Vinyl carboxylic acid monomer, many sulfur
For ester chain-transferring agent, initiator, and nitrogen bubble certain hour is used, sealed afterwards；
(2) it is heated to uniform temperature reaction certain hour；
(3) reaction is distilled off solvent after terminating；
(4) add a small amount of water dilution, the pH of one or more base reagent regulation system is added to 5～8, and added water
Polymer solution solid content is adjusted to 24%～26%, you can obtain high-efficiency coarse whiting ground dispersant.
In a preferred embodiment, the mass fraction of each reactant is as follows：
30～100 parts of vinyl carboxylic acid monomer
0.2～5 part of polythio ester chain-transferring agent
0.01～2 part of initiator
Also, the consumption of solvent causes the concentration of vinyl carboxylic acid monomer to remain 1～8mol/L.
In a further preferred embodiment, in the step (1), the nitrogen bubble certain hour
For 15-30 minutes；In the step (2), the uniform temperature is 60～80 degrees Celsius, a timing
Between be 8 to 16 hours；In the step (3), the distillation is vacuum distillation.
In a further preferred embodiment, in the step (4), the base reagent is selected from：Hydrogen-oxygen
Change calcium solid, magnesium hydroxide solid, sodium hydroxide solution, also, its addition is according to following mass fraction：
Sodium hydroxide solution 10-100 parts
0～100 part of calcium hydroxide
0～100 part of magnesium hydroxide.
In an embodiment still more preferably, the vinyl carboxylic acid monomer is acrylic acid or methyl-prop
Olefin(e) acid.
In an embodiment still more preferably, the polythio ester chain-transferring agent is selected from dithiobenzoic acid
Cyano group isopropyl ester, 4- cyano group -4- dithio benzoyloxy valeric acids, 2- (dodecyl dihydrogen thiocarbonate. ester group)
- 2 Methylpropionic acid, 2- (dodecyl trithiocarbonate) -2- isopropylformic acid .s, 4- cyano group -4- lauryl trithio carbon
One or more in acid esters.
In an embodiment still more preferably, the initiator is different selected from azodiisobutyronitrile, azo two
In heptonitrile, azo diisobutyl valeric acid, dibenzoyl peroxide, cyclohexanone peroxide, tert-butyl hydroperoxide
One or more.
In an embodiment still more preferably, the solvent is selected from tetrahydrofuran, benzene, toluene, N, N-
One or more in dimethylformamide, ethylbenzene, dimethylbenzene, 1,4- dioxane.
A second aspect of the present invention, there is provided one kind has used high-efficiency coarse whiting ground obtained in any of the above-described kind of method
Dispersant.
A kind of a third aspect of the present invention, there is provided wet method of above-mentioned high-efficiency coarse whiting ground dispersant in ultrafine heavy calcium
Application in grinding production.
The preparation of the polyacrylate of 1 low-molecular-weight narrow ditribution of embodiment
Dithioesters chain-transferring agent 4- cyano group -4- dithio benzoyloxy valeric acids are added in reaction vessel
9.12g, initiator azodiisobutyronitrile 2.05g, solvent toluene 312.0g and monomeric acrylic 180g.Body
System is sealed after 20 minutes with nitrogen bubble, is reacted 12 hours under the conditions of being warming up to 70 DEG C afterwards.Reaction terminates
Afterwards by resulting solution vacuum distillation, after removing solvent plus the dilution of a small amount of water, add 45g calcium hydroxide and
15g magnesium hydroxide.It is 6.78 to add sodium hydroxide solution (32%) and adjust pH value of solution, and the tune that adds water
Section polymer solution solid content is 24%, obtains final dispersant sample.Gained dispersant weight average molecular weight be
6418, molecular weight distributing index is 1.17.
The preparation of the poly-methyl acrylate of 2 low-molecular-weight narrow ditribution of embodiment
Dithioesters chain-transferring agent dithiobenzoic acid cyano group isopropyl ester 9.82g is added in quartz reaction container,
Initiator azodiisobutyronitrile 2.43g, solvents tetrahydrofurane 231.21g and monomer methacrylic acid 129.00g.
System is sealed with after nitrogen bubble 20 minutes, is reacted 8 hours under the conditions of being warming up to 80 DEG C afterwards.Reaction terminates
Afterwards by resulting solution vacuum distillation, after removing solvent plus the dilution of a small amount of water, add 39g calcium hydroxide and
30g magnesium hydroxide.It is 6.69 to add sodium hydroxide solution (32%) and adjust pH value of solution, and the tune that adds water
Section polymer solution solid content is 25%, obtains final dispersant sample.Gained dispersant weight average molecular weight be
4910, molecular weight distributing index is 1.23.
The preparation of poly- (sodium acrylate-co- methacrylates) of 3 low-molecular-weight narrow ditribution of embodiment
Trithio ester chain-transferring agent 2- (dodecyl dihydrogen thiocarbonate. ester group) -2- is added in quartz reaction container
Methylpropanoic acid 10.31g, initiator 2,2'-Azobis(2,4-dimethylvaleronitrile) 3.12g, solvent Isosorbide-5-Nitrae-dioxane 322.24g and list
Body methacrylic acid 107.20g and acrylic acid 90.23g.System is sealed with after nitrogen bubble 20 minutes, afterwards
React 16 hours under the conditions of being warming up to 65 DEG C.React by resulting solution vacuum distillation after terminating, after removing solvent
Plus a small amount of water dilution, add 30g calcium hydroxide and 35g magnesium hydroxide.Add sodium hydroxide solution
(32%) it is 6.81 to adjust pH value of solution, and the regulation polymer solution solid content that adds water is 26%, is obtained most
Whole dispersant sample.Gained dispersant weight average molecular weight is 5610, and molecular weight distributing index is 1.24.
Grinding effect is detected
Dispersant and control sample obtained in embodiment 1～3 (are disclosed by United States Patent (USP) 20020019329A1
The dispersant for preparing of method, weight average molecular weight 5591, and molecular weight distributing index is 1.43) in 98 grades of triple superphosphate
Carry out in grinding using (dispersant solid content is 24%～26%).
The water of amount of calculation is added in 15 liters of grinding pots, stirring is opened, the dispersant of amount of calculation, stirring is added
Add the ground calcium carbonate powder of amount of calculation, grinding to discharge after 2 hours after uniform, carry out viscosity and particle size data
The ratio of detection, wherein dispersant dosage and ground slurry other each components is consistent.It is quiet after particle diameter and dispersion
Only 1 hour viscosity data is as follows：
Table 1
Data result from table 1 was can be seen that using prepared by the embodiment 1～3 of the method for the invention dividing
The grinding effect of powder to be substantially better than the grinding effect of control sample dispersant.
Above the specific embodiment of the present invention has been described in detail, but, which is intended only as example, this
It is bright to be not restricted to particular embodiments described above.To those skilled in the art, it is any to the present invention
The equivalent modifications for carrying out and replacement are also all among scope of the invention.Therefore, in the essence without departing from the present invention
The impartial conversion made under god and scope and modification, should all cover within the scope of the invention.
Claims (10)
1. a kind of method that RAFT methods prepare high-efficiency coarse whiting ground dispersant, it is characterised in that comprise the steps:
(1) solvent is added in reaction vessel, and adds reactant：Vinyl carboxylic acid monomer, polythio ester chain turn
Agent, initiator are moved, and uses nitrogen bubble, sealed afterwards；
(2) it is heated to uniform temperature reaction certain hour；
(3) reaction is distilled off solvent after terminating；
(4) add a small amount of water dilution, the pH of one or more base reagent regulation system is added to 5～8, and added water
Polymer solution solid content is adjusted to 24%～26%, you can obtain high-efficiency coarse whiting ground dispersant.
2. method according to claim 1, it is characterised in that the mass fraction of each reactant is as follows：
30～100 parts of vinyl carboxylic acid monomer
0.2～5 part of polythio ester chain-transferring agent
0.01～2 part of initiator
Also, the consumption of solvent causes the concentration of vinyl carboxylic acid monomer to remain 1～8mol/L.
3. method according to claim 2, it is characterised in that in the step (1), the nitrogen bubble
Duration is 15-30 minutes；In the step (2), the uniform temperature is 60～80 degrees Celsius,
The certain hour is 8 to 16 hours；In the step (3), the distillation is vacuum distillation.
4. method according to claim 2, it is characterised in that in the step (4), the base reagent choosing
From：Calcium hydroxide solid, magnesium hydroxide solid, sodium hydroxide solution, also, its addition is according to following matter
Amount number：
Sodium hydroxide solution 10-100 parts
0～100 part of calcium hydroxide
0～100 part of magnesium hydroxide.
5. the method according to any one of claim 1-4, it is characterised in that the vinyl carboxylic acid monomer is
Acrylic acid or methacrylic acid.
6. the method according to any one of claim 1-4, it is characterised in that the polythio ester chain-transferring agent
Selected from dithiobenzoic acid cyano group isopropyl ester, 4- cyano group -4- dithio benzoyloxy valeric acids, 2- (dodecyls
Dihydrogen thiocarbonate. ester group) -2 Methylpropionic acid, 2- (dodecyl trithiocarbonate) -2- isopropylformic acid .s, 4- cyano group
One or more in -4- lauryl trithio carbonic esters.
7. the method according to any one of claim 1-4, it is characterised in that the initiator is selected from azo two
Isopropyl cyanide, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo diisobutyl valeric acid, dibenzoyl peroxide, cyclohexanone peroxide,
One or more in tert-butyl hydroperoxide.
8. the method according to any one of claim 1-4, it is characterised in that the solvent selected from tetrahydrofuran,
One or more in benzene, toluene, N,N-dimethylformamide, ethylbenzene, dimethylbenzene, 1,4- dioxane.
9. the high-efficiency coarse whiting ground dispersant that prepared by the method according to any one of claim 1～8.
10. high-efficiency coarse whiting ground dispersant according to claim 9 is in the wet grinding production of ultrafine heavy calcium
Using.
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Cited By (2)
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| CN111440259A (en) * | 2020-04-23 | 2020-07-24 | 济宁明升新材料有限公司 | Multi-branch type dispersing agent and preparation method thereof |
| CN113929606A (en) * | 2021-09-23 | 2022-01-14 | 武汉海翎化学工业有限公司 | Trithioester chain transfer agent, low-molecular-weight sodium polyacrylate obtained by using same, application and preparation |
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| CN111440259A (en) * | 2020-04-23 | 2020-07-24 | 济宁明升新材料有限公司 | Multi-branch type dispersing agent and preparation method thereof |
| CN113929606A (en) * | 2021-09-23 | 2022-01-14 | 武汉海翎化学工业有限公司 | Trithioester chain transfer agent, low-molecular-weight sodium polyacrylate obtained by using same, application and preparation |
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