CN101274242B - Method for preparing polymer ceramic dispersants - Google Patents
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- CN101274242B CN101274242B CN2008100172587A CN200810017258A CN101274242B CN 101274242 B CN101274242 B CN 101274242B CN 2008100172587 A CN2008100172587 A CN 2008100172587A CN 200810017258 A CN200810017258 A CN 200810017258A CN 101274242 B CN101274242 B CN 101274242B
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Abstract
The invention discloses a preparation method of a polymer ceramic dispersant, which is characterized in that polyethylene glycol and maleic anhydride are uniformly mixed and polymerized to obtain a semi-esterification product; the semi-esterification product, vinyl monomer and water are uniformly mixed to carry out free radical polymerization under the inducement of initiating agent so as to obtain the polymer ceramic dispersant. The product prepared by adopting the invention has excellent dispersion dilution effect and grinding-aid effect on the ceramic slurry, improves the billet strength and the billet yield, thus reducing the production cost; meanwhile, the indexes such as the density and the folding resistance strength, etc. of the ceramic product are greatly reinforced. Furthermore, the product can be also used for the dispersion of dye and coating, etc.
Description
Technical field
The present invention relates to a kind of preparation method of macromolecule dispersing agent, relate in particular to a kind of preparation method of polymer ceramic dispersants.
Background technology
The development that becomes more meticulous along with ceramics, new moulding process emerges in an endless stream, annotate film moulding, colloidal vibration moulding, LOW TEMPERATURES moulding, directly solidify and annotate film moulding, infiltration solidification moulding etc. as the moulding of centrifugal notes film, gel, and numerous moulding process all requires to prepare the ceramic size of low-viscosity, high dispersive, high stability, high solid loading.Solution mainly is to use dispersant in processing procedure, improves the rheological characteristic of slip, improves the uniformity of its microstructure and improves its intensity.
At present, ceramic dispersants is divided into inorganic dispersant, organic dispersing agent and macromolecule dispersing agent three classes.Inorganic dispersant mainly is an inorganic electrolyte, as sodium chloride, sodium metasilicate, sodium metasilicate, calgon, sodium carbonate, sodium phosphate trimer (STPP) etc., mainly is applicable to aluminium oxide and zirconia slurry.Organic dispersing agent mainly is organic bath class dispersant and surfactant-dispersed agent, as natrium citricum, sodium humate, sodium ethylene diamine tetracetate (EDTA), odium stearate, sodium alkyl sulfonate, AEO etc.Little dispersal agent molecule is owing to be subjected to the influence of factors such as molecular structure, relative molecular mass, and its dispersion effect is often very limited, and large usage quantity.And macromolecule dispersing agent is because hydrophilic group, hydrophobic group position and adjustable size, and molecular structure can be pectination, can present highly branched chainization again, to the disperse particles surface coverage and to seal effect better than the former.Its dispersion is easier in addition tends towards stability, flows, and macromolecule dispersing agent will become a rising class ceramic dispersants, and it synthesizes and application study causes extensive attention.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polymer ceramic dispersants, it has good dispersion diluting effect and grinding aid effect to ceramic slurry; Improved blank strength and billet yield, thereby reduced production costs; Make ceramic density simultaneously, indexs such as rupture strength strengthen greatly but also can be used for the dispersion of pigment, coating etc.
For achieving the above object, the technical solution used in the present invention is: polyethylene glycol and maleic anhydride are pressed 1: the mixed in molar ratio of 0.1-1.2 is even, makes solution A; Add acid solution in solution A, the mass ratio of solution A and acid solution is 100: 0.5-10, be warming up to 30-90 ℃ then, and reacted 0.5-4 hour, make esterification products B; With product B, functional monomer and vinyl monomer by 1: the mass ratio of 1-10: 0.1-1.5 mixes, and makes monomer solution C, and wherein, functional monomer is the monomer of 1. being represented by general formula; Described vinyl monomer is acrylic ester monomer of 2. being represented by general formula or the styrene monomer of 3. being represented by general formula:
1. R in the formula
1Be hydrogen atom or alkyl, M
1Be hydrogen atom or carboxyl; M
2For hydrogen atom or carboxylic side chain or contain sulfonic side chain or the organic amine group;
2. the R in the formula
2Be hydrogen atom or methyl, M
3Be alkyl;
3. the R in the formula
3Be hydrogen atom or methyl; With solution C, molecular weight regulator and water by 1: the mass ratio of 0-0.5: 1-10 mixes, and makes monomer mixture solution D; With water and water soluble starter by 1: the mass ratio of 0.002-1 mixes, and obtains initiator solution E; At 40-90 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.05-20, the dropping time is 0.1-4 hour, after dropwising, adjust the temperature to 50-95 ℃, reacted 1-6 hour, make aqueous copolymers solution F; With alkaline solution the pH value of solution F is adjusted to 7-13, sub-ceramic dispersants promptly secures satisfactory grades.
It is PEG200, PEG400, PEG600, PEG800, the PEG1000 of 200-8000 that polyethylene glycol of the present invention adopts molecular weight; Acid solution is a kind of in sulfuric acid, formic acid, acetate, the oxalic acid; Functional monomer is acrylic or methacrylic acid; Described vinyl monomer is a kind of in methyl acrylate, methyl methacrylate, ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, Hexyl 2-propenoate, hexyl methacrylate, octadecyl acrylate, octadecyl methacrylate, styrene, the methyl styrene; Molecular weight regulator is lauryl mercaptan, ethyl mercaptan, triethanolamine or isopropyl alcohol; Water soluble starter is ammonium persulfate, potassium peroxydisulfate, ammonium persulfate-sodium sulfite or ammonium persulfate-sodium bisulfite, potassium peroxydisulfate-sodium sulfite or potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-sodium thiosulfate or potassium peroxydisulfate-sodium thiosulfate; Alkaline solution is a kind of in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, trimethylamine, triethylamine or the triethanolamine.
The present invention adopts anchoring group to replace the lipophilic group of traditional dispersant, and be polymer chain, and select the group of opposed polarity according to the surface nature of oversubscription loose powder body, with the firm absorption of assurance dispersant on solid particles surface, and this absorption is generally Irreversible Adsorption, is difficult to desorption, replace hydrophilic radical with solvent chain, main chain and side chain adjustable length have been introduced new polymerization single polymerization monomer, and the product that makes has good dispersion effect and humidification; Use the monomer of maleic anhydride one polyethylene glycol half ester product as polymerisation, both can in product, introduce an amount of relative molecular mass as requested as side chain, can regulate the side chain relative molecular mass according to application conditions again, guarantee that dispersant forms the protective layer of adequate thickness in solid particles surface, this has just widened the application of product greatly, has improved the application performance of product; Change tradition and produce the means of the binary copolymerization of macromolecule dispersing agent, add a small amount of hydrophobic monomer, as polymer hydrophile-lipophile balance group, to strengthen the dispersive property of end product as the 3rd monomer.
Embodiment 1: polyethylene glycol (PEG200) and maleic anhydride is even by 1: 0.8 mixed in molar ratio, make solution A; Add bright sulfur acid in solution A, solution A is 100: 3 with the mass ratio of acid, is warming up to 30 ℃ then, reacts 4 hours, makes esterification products B; Product B, functional monomer acrylic acid and the vinyl monomer methyl acrylate mass ratio by 1: 1: 1.5 is mixed, make monomer solution C; Solution C and the water mass ratio by 1: 8 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate mass ratio by 1: 0.002 is mixed, obtain initiator solution E; At 80 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 10, the dropping time is 2 hours, after dropwising, adjusts the temperature to 50 ℃, reacted 6 hours, and made aqueous copolymers solution F; With alkaline solution ammoniacal liquor the pH value of solution F is adjusted to 8, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 2: polyethylene glycol (PEG400) and maleic anhydride is even by 1: 0.5 mixed in molar ratio, make solution A; Add pure formic acid in solution A, solution A is 100: 5 with the mass ratio of acid, is warming up to 40 ℃ then, reacts 3.5 hours, makes esterification products B; Product B, functional monomer methacrylic acid and the vinyl monomer methyl methacrylate mass ratio by 1: 3: 1.2 is mixed, make monomer solution C; Solution C, molecular weight regulator ethyl mercaptan and the water mass ratio by 1: 0.04: 5 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate mass ratio by 1: 0.005 is mixed, obtain initiator solution E; At 50 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 5, the dropping time is 1 hour, after dropwising, adjusts the temperature to 55 ℃, reacted 5.5 hours, and made aqueous copolymers solution F; With alkaline solution NaOH the pH value of solution F is adjusted to 12, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 3: polyethylene glycol (PEG600) and maleic anhydride are evenly made solution A by 1: 1.0 mixed in molar ratio; Add pure acetate in solution A, solution A is 100: 8 with the mass ratio of acid, is warming up to 50 ℃ then, reacts 3 hours, makes esterification products B; Product B, functional monomer itaconic acid and the vinyl monomer ethyl acrylate mass ratio by 1: 8: 0.8 is mixed, make monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.01: 3 is mixed, make monomer mixture solution D; Water and water soluble starter ammonium persulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.009 is mixed, obtain initiator solution E; At 70 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.5, the dropping time is 4 hours, after dropwising, adjusts the temperature to 60 ℃, reacted 5 hours, and made aqueous copolymers solution F; With alkaline solution potassium hydroxide the pH value of solution F is adjusted to 7, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 4: polyethylene glycol (PEG800) and maleic anhydride is even by 1: 0.9 mixed in molar ratio, make solution A; Add pure oxalic acid in solution A, solution A is 100: 1 with the mass ratio of acid, is warming up to 60 ℃ then, reacts 2.5 hours, makes esterification products B; Product B, functional monomer hydroxy-ethyl acrylate and the vinyl monomer EMA mass ratio by 1: 5: 0.3 is mixed, make monomer solution C; Solution C, molecular weight regulator isopropyl alcohol and the water mass ratio by 1: 0.2: 1 is mixed, make monomer mixture solution D; Water and water soluble starter potassium peroxydisulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.5 is mixed, obtain initiator solution E; At 40 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.05, the dropping time is 4 hours, after dropwising, adjust the temperature to 65 ℃, reacted 4.5 hours, make aqueous copolymers solution F; With alkaline solution sodium carbonate the pH value of solution F is adjusted to 13, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 5: polyethylene glycol (PEG1000) and maleic anhydride is even by 1: 0.6 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid and oxalic acid, solution A is 100: 0.8 with the mass ratio of acid, is warming up to 70 ℃ then, reacts 2 hours, makes esterification products B; Product B, functional monomer hydroxyethyl methacrylate and the vinyl monomer butyl acrylate mass ratio by 1: 4: 0.1 is mixed, make monomer solution C; Solution C, molecular weight regulator lauryl mercaptan and the water mass ratio by 1: 0.3: 10 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate-sodium thiosulfate mass ratio by 1: 0.8 is mixed, obtain initiator solution E; At 60 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 20, the dropping time is 0.1 hour, after dropwising, adjusts the temperature to 70 ℃, reacted 4 hours, and made aqueous copolymers solution F; With the alkaline solution sodium acid carbonate pH value of solution F is adjusted to 10, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 6: polyethylene glycol (PEG200) and maleic anhydride is even by 1: 1.1 mixed in molar ratio, make solution A; The mixture that in solution A, adds pure formic acid and acetate, solution A is 100: 10 with the mass ratio of acid, is warming up to 80 ℃ then, reacts 1.5 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer hydroxypropyl acrylate and hydroxy propyl methacrylate and vinyl monomer butyl methacrylate and Hexyl 2-propenoate by 1: 4: 4: 0.2: 0.8 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator ethyl mercaptan and the water mass ratio by 1: 0.5: 2 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate-sodium thiosulfate mass ratio by 1: 0.2 is mixed, obtain initiator solution E; At 90 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 1, the dropping time is 3.5 hours, after dropwising, adjust the temperature to 75 ℃, reacted 3.5 hours, make aqueous copolymers solution F; With the alkaline solution trimethylamine pH value of solution F is adjusted to 9, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 7: polyethylene glycol (PEG400) and maleic anhydride is even by 1: 0.1 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, acetate and oxalic acid, solution A is 100: 7 with the mass ratio of acid, is warming up to 90 ℃ then, reacts 0.5 hour, makes esterification products B; With the mixture of product B, functional monomer methallyl sulfonic acid and allyl sulphonic acid and vinyl monomer hexyl methacrylate and octadecyl acrylate by 1: 2: 7: 0.3: 0.2 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.1: 9 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate mass ratio by 1: 1 is mixed, obtain initiator solution E; At 45 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 15, the dropping time is 0.5 hour, after dropwising, adjusts the temperature to 80 ℃, reacted 3 hours, and made aqueous copolymers solution F; With the alkaline solution triethylamine pH value of solution F is adjusted to 11, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 8: polyethylene glycol (PEG600) and maleic anhydride is even by 1: 1.2 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, formic acid and oxalic acid, solution A is 100: 2 with the mass ratio of acid, is warming up to 45 ℃ then, reacts 3.8 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer allyl benzene sulfonic acid and methacrylic acid and vinyl monomer octadecyl methacrylate, styrene and methyl styrene by 1: 3: 7: 0.2: 0.4: 0.7 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator isopropyl alcohol and the water mass ratio by 1: 0.4: 7 is mixed, make monomer mixture solution D; Water and water soluble starter ammonium persulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.1 is mixed, obtain initiator solution E; At 65 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 8, the dropping time is 2 hours, after dropwising, adjusts the temperature to 85 ℃, reacted 2.5 hours, and made aqueous copolymers solution F; With the alkaline solution triethanolamine pH value of solution F is adjusted to 12, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 9: polyethylene glycol (PEG800) and maleic anhydride is even by 1: 0.3 mixed in molar ratio, make solution A; The mixture that in solution A, adds pure formic acid, acetate and oxalic acid, solution A is 100: 0.5 with the mass ratio of acid, is warming up to 65 ℃ then, reacts 2.7 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer itaconic acid and hydroxy-ethyl acrylate and vinyl monomer methyl methacrylate and ethyl acrylate by 1: 5: 2: 0.8: 0.4 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator lauryl mercaptan and the water mass ratio by 1: 0.05: 4 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate-sodium thiosulfate mass ratio by 1: 0.7 is mixed, obtain initiator solution E; At 85 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 13, the dropping time is 1.5 hours, after dropwising, adjusts the temperature to 90 ℃, reacted 2 hours, and made aqueous copolymers solution F; Mixture with alkaline solution ammoniacal liquor and NaOH) the pH value with solution F is adjusted to 10.5, and sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 10: polyethylene glycol (PEG1000) and maleic anhydride is even by 1: 0.7 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, acetate and oxalic acid, solution A is 100: 7 with the mass ratio of acid, is warming up to 85 ℃ then, reacts 1 hour, makes esterification products B; With the mixture of the mixture of product B, functional monomer hydroxy-ethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl acrylate and vinyl monomer butyl acrylate and butyl methacrylate by 1: 2: 3: 4: 0.2: 0.6 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.09: 6 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate mass ratio by 1: 0.4 is mixed, obtain initiator solution E; At 55 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 3, the dropping time is 3 hours, after dropwising, adjusts the temperature to 95 ℃, reacted 1 hour, and made aqueous copolymers solution F; With the mixture of alkaline solution potassium hydroxide and sodium carbonate, the pH value of solution F is adjusted to 8.5, sub-ceramic dispersants promptly secures satisfactory grades.
The present invention can form double electrical layers at particle surface, and simultaneously electrostatic stabilization own, the stable triple mechanism of macromolecule steric stabilization and room can make colloid-stabilised or make particle insoluble in solvent continue to keep the state of high degree of dispersion.It both can add in slip, again can be in glaze slip adapted, have good dispersiveness and grinding aid effect, make slip under the situation of low moisture content, have suitable viscosity, good flowability, be convenient to operation, can reach energy-saving and cost-reducing purpose.Improved blank strength and billet yield, thereby reduced production costs; Make ceramic density simultaneously, indexs such as rupture strength strengthen greatly.This invention product also can be used for fields such as papermaking, mud conditioning, pigment dispersion and coating dispersion.
Claims (8)
1. the preparation method of a polymer ceramic dispersants is characterized in that:
1) polyethylene glycol and maleic anhydride are pressed 1: the mixed in molar ratio of 0.1-1.2 is even, makes solution A;
2) add acid solution in solution A, the mass ratio of solution A and acid solution is 100: 0.5-10, be warming up to 30-90 ℃ then, and reacted 0.5-4 hour, make esterification products B;
3) with product B, functional monomer and vinyl monomer by 1: the mass ratio of 1-10: 0.1-1.5 mixes, and makes monomer solution C, and wherein, functional monomer is the monomer of 1. being represented by general formula; Described vinyl monomer is acrylic ester monomer of 2. being represented by general formula or the styrene monomer of 3. being represented by general formula:
1. R in the formula
1Be hydrogen atom or alkyl, M
1Be hydrogen atom or carboxyl; M
2For hydrogen atom or carboxylic side chain or contain sulfonic side chain or the organic amine group;
2. the R in the formula
2Be hydrogen atom or methyl, M
3Be alkyl;
3. the R in the formula
3Be hydrogen atom or methyl;
4) with solution C, molecular weight regulator and water by 1: the mass ratio of 0-0.5: 1-10 mixes, and makes monomer mixture solution D;
5) with water and water soluble starter by 1: the mass ratio of 0.002-1 mixes, and obtains initiator solution E;
6) at 40-90 ℃, in monomer mixture solution D, drip initiator solution E, wherein the mass ratio of the water soluble starter among monomer mixture solution D and the initiator solution E is 100: 0.05-20, the dropping time is 0.1-4 hour, after dropwising, adjust the temperature to 50-95 ℃, reacted 1-6 hour, make aqueous copolymers solution F;
7) with alkaline solution the pH value of solution F is adjusted to 7-13, sub-ceramic dispersants promptly secures satisfactory grades.
2. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: it is PEG200, PEG400, PEG600, PEG800, the PEG1000 of 200-8000 that described polyethylene glycol adopts molecular weight.
3. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: described acid solution is a kind of in sulfuric acid, formic acid, acetate, the oxalic acid.
4. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said functional monomer is acrylic or methacrylic acid.
5. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: said vinyl monomer is a kind of in methyl acrylate, methyl methacrylate, ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, Hexyl 2-propenoate, hexyl methacrylate, octadecyl acrylate, octadecyl methacrylate, styrene, the methyl styrene.
6. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said molecular weight regulator is lauryl mercaptan, ethyl mercaptan, triethanolamine or isopropyl alcohol.
7. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said water soluble starter is ammonium persulfate, potassium peroxydisulfate, ammonium persulfate-sodium sulfite or ammonium persulfate-sodium bisulfite, potassium peroxydisulfate-sodium sulfite or potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-sodium thiosulfate or potassium peroxydisulfate-sodium thiosulfate.
8. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: said alkaline solution is a kind of in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, trimethylamine, triethylamine or the triethanolamine.
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| CN101274242A (en) | 2008-10-01 |
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