CN107722161B - Polymer diluent for clay grinding and preparation method thereof - Google Patents

Polymer diluent for clay grinding and preparation method thereof Download PDF

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Publication number
CN107722161B
CN107722161B CN201710879314.7A CN201710879314A CN107722161B CN 107722161 B CN107722161 B CN 107722161B CN 201710879314 A CN201710879314 A CN 201710879314A CN 107722161 B CN107722161 B CN 107722161B
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grinding
argil
mass
polymer diluent
reaction solution
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CN107722161A (en
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张磊
戴永强
苏瑜
贾康乐
钟本镔
高敏
麦裕良
廖兵
熊文杰
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Institute of Chemical Engineering of Guangdong Academy of Sciences
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Guangdong Research Institute Of Petrochemical And Fine Chemical Engineering
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04Acids; Metal salts or ammonium salts thereof
    • C08F220/06Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/6261Milling
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/38Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Polymerisation Methods In General (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paper (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a polymer diluent for argil grinding and a preparation method thereof, wherein the preparation method of the polymer diluent for argil grinding comprises the following steps: uniformly mixing an acrylic monomer, a chain transfer agent and water, adding an alkali solution until the pH value of a reaction solution is 7-8, vacuumizing, adding an initiator, carrying out polymerization reaction, cooling the reaction solution, and adding the alkali solution until the pH value of the reaction solution is 8-9 to obtain the polymer diluent for grinding the argil. The polymer diluent for grinding the argil has the advantages of small addition amount, good viscosity reducing effect, excellent water reducing effect, low cost, good stability, simple production process, atom economy, no need of post-treatment and environmental protection, and can obviously improve the dispersibility and grinding efficiency of the argil.

Description

Polymer diluent for clay grinding and preparation method thereof
Technical Field
The invention relates to a polymer diluent for clay grinding and a preparation method thereof, belonging to the field of ceramic ball-milling aids.
Background
The ceramic products have a long history and become an indispensable part of people's daily life, and along with the development of society, people have higher and higher requirements on the ceramic products. When ceramics are manufactured, the pottery clay needs to be ground to a certain particle size range, and the high-quality requirement of pottery clay products can be met. In the pottery clay grinding process, water needs to be added for dilution, after the pottery clay grinding is finished, more than 90% of water in the pottery clay needs to be removed for entering the next process, and if the addition amount of the water in the pottery clay grinding process is too large, the energy consumption is obviously increased during water removal. Therefore, during the clay grinding process, a diluent is required to be added to reduce the viscosity of the system, and further reduce the addition amount of water.
At present, the diluents for clay grinding can be mainly classified into the following types: inorganic salts, organic micromolecules and composite water reducing agent. Inorganic salts are developed more mature, but the molecular structure and molecular weight of the inorganic salts are uncontrollable, the addition amount is large when the inorganic salts are used, and the water reducing effect is poor; the water reducing effect of the organic micromolecules is good, but the cost is high and the stability is poor; the composite water reducing agent has low cost and good adaptability, but has limited water reducing efficiency, and cannot meet the requirements of high water reducing rate and high stability of modern ceramic production.
Therefore, there is a need to develop a diluent for clay grinding with small addition amount, excellent water reducing effect, low cost and good stability.
Disclosure of Invention
The invention aims to provide a polymer diluent for clay grinding and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a preparation method of a polymer diluent for argil grinding comprises the following steps: the method comprises the following steps: uniformly mixing an acrylic monomer, a chain transfer agent and water, adding an alkali solution until the pH value of a reaction solution is 7-8, vacuumizing, adding an initiator, carrying out polymerization reaction, cooling the reaction solution, and adding the alkali solution until the pH value of the reaction solution is 8-9 to obtain the polymer diluent for grinding the argil.
The acrylic monomer is at least one of acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid, and the mass of the acrylic monomer accounts for 30-45% of the total mass of the acrylic monomer and water.
The chain transfer agent is S, S ' -di (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate, and the mass of the chain transfer agent accounts for 1-4% of the total mass of the acrylic monomer and the water.
The initiator is ammonium persulfate, and the mass of the initiator accounts for 0.3-2.0% of the total mass of the acrylic monomer and the water.
The polymerization reaction is carried out at 60-75 ℃, and the reaction time is 4-6 h.
And dropwise adding the initiator into the reaction solution in the form of aqueous solution for 0.6-2 h.
The alkali solution is a sodium hydroxide solution with the mass fraction of 40-60%.
The invention has the beneficial effects that: the polymer diluent for grinding the argil has the advantages of small addition amount, good viscosity reducing effect, excellent water reducing effect, low cost, good stability, simple production process, atom economy, no need of post-treatment and environmental protection, and can obviously improve the dispersibility and grinding efficiency of the argil.
Detailed Description
A preparation method of a polymer diluent for argil grinding comprises the following steps: uniformly mixing an acrylic monomer, a chain transfer agent and water, adding an alkali solution until the pH value of a reaction solution is 7-8, vacuumizing, adding an initiator, carrying out polymerization reaction, cooling the reaction solution, and adding the alkali solution until the pH value of the reaction solution is 8-9 to obtain the polymer diluent for grinding the argil.
Preferably, the acrylic monomer is at least one of acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid, and the mass of the acrylic monomer accounts for 30-45% of the total mass of the acrylic monomer and water.
More preferably, the acrylic monomer is acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid according to a mass ratio of (55-65): (10-15): (10-20): (10-20) in the presence of a catalyst.
Preferably, the chain transfer agent is S, S ' -di (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate, and the mass of the chain transfer agent accounts for 1-4% of the total mass of the acrylic monomer and the water.
Preferably, the initiator is ammonium persulfate, and the mass of the initiator accounts for 0.3-2.0% of the total mass of the acrylic monomer and the water.
Preferably, the polymerization reaction is carried out at 60-75 ℃, and the reaction time is 4-6 h.
Preferably, the initiator is dripped into the reaction liquid in the form of aqueous solution, and the dripping is completed within 0.6-2 h.
Preferably, the alkali solution is a sodium hydroxide solution with the mass fraction of 40-60%.
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a polymer diluent for argil grinding is prepared by the following steps:
stirring and uniformly mixing 35g of acrylic monomers (acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid in a mass ratio of 60:10:10:20), 1.0g S, S ' -bis (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate and 65mL of deionized water, adding a 50% by mass sodium hydroxide solution until the pH value of the reaction solution is 7, vacuumizing, heating to 70 ℃, slowly dropwise adding an ammonium persulfate aqueous solution (containing 0.3g of ammonium persulfate), finishing dropwise adding for 0.7h, reacting for 5h at a constant temperature of 70 ℃, cooling the reaction solution to room temperature, adding a 50% by mass sodium hydroxide solution until the pH value of the reaction solution is 8, and obtaining the polymer diluent for argil grinding.
And (3) performance testing:
through testing, the weight average molecular weight of the polymer diluent for clay grinding is 24700, and the PDI is 1.29; the polymer diluent for grinding the argil is added into the slurry, wherein the mass of the macromolecular diluent is 0.2 percent of the mass of the argil, the viscosity of a slurry system is 360mPa & s, the flowing time is 54s, the argil blank does not have a sedimentation phenomenon after standing overnight, the stability is good, and the breaking strength of the obtained argil blank is improved by 210 percent compared with that of the argil blank without the polymer diluent.
Example 2:
a polymer diluent for argil grinding is prepared by the following steps:
the preparation method comprises the following steps of uniformly stirring and mixing 38g of acrylic monomers (acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid in a mass ratio of 55:15:20:10), 2.1g S, S ' -bis (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate and 62mL of deionized water, adding a 50% by mass sodium hydroxide solution until the pH value of the reaction solution is 7, vacuumizing, heating to 65 ℃, slowly dropwise adding an ammonium persulfate aqueous solution (containing 1.2g of ammonium persulfate), finishing dropwise adding for 1h, reacting at a constant temperature of 65 ℃ for 4h, cooling the reaction solution to room temperature, adding a 50% by mass sodium hydroxide solution until the pH value of the reaction solution is 8, and obtaining the polymer diluent for argil grinding.
And (3) performance testing:
through testing, the weight average molecular weight of the polymer diluent for clay grinding is 17100, and the PDI is 1.21; the polymer diluent for grinding the argil is added into the slurry, wherein the mass of the macromolecular diluent is 0.2 percent of the mass of the argil, the viscosity of a slurry system is 340mPa & s, the flowing time is 50s, the argil blank does not have a sedimentation phenomenon after standing overnight, the stability is good, and the breaking strength of the obtained argil blank is improved by 240 percent compared with that of the argil blank without the polymer diluent.
Example 3:
a polymer diluent for argil grinding is prepared by the following steps:
stirring and uniformly mixing 40g of acrylic monomers (acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid in a mass ratio of 65:15:10:10), 4.0g S, S ' -bis (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate and 60mL of deionized water, adding a 50 mass percent sodium hydroxide solution until the pH value of the reaction solution is 8, vacuumizing, heating to 60 ℃, slowly dropwise adding an ammonium persulfate aqueous solution (containing 2.0g of ammonium persulfate), finishing dropwise adding for 1.5h, reacting for 6h at a constant temperature of 60 ℃, cooling the reaction solution to room temperature, adding a 40 mass percent sodium hydroxide solution until the pH value of the reaction solution is 9, and obtaining the polymer diluent for argil grinding.
And (3) performance testing:
through tests, the weight average molecular weight of the polymer diluent for clay grinding is 21100, and the PDI is 1.32; the polymer diluent for grinding the argil is added into the slurry, wherein the mass of the macromolecular diluent is 0.2 percent of the mass of the argil, the viscosity of a slurry system is 300mPa & s, the flowing time is 49s, the argil blank does not have a sedimentation phenomenon after standing overnight, the stability is good, and the breaking strength of the obtained argil blank is improved by 260 percent compared with that of the argil diluent which is not added.
Example 4:
a polymer diluent for argil grinding is prepared by the following steps:
stirring and uniformly mixing 35g of acrylic monomers (acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid in a mass ratio of 60:10:15:15), 2.6g S, S ' -bis (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate and 65mL of deionized water, adding a 50 mass percent sodium hydroxide solution until the pH value of the reaction solution is 7, vacuumizing, heating to 65 ℃, slowly dropwise adding an ammonium persulfate aqueous solution (containing 1.4g of ammonium persulfate), finishing dropwise adding for 1.2h, reacting for 6h at a constant temperature of 65 ℃, cooling the reaction solution to room temperature, adding a 55 mass percent sodium hydroxide solution until the pH value of the reaction solution is 9, and obtaining the polymer diluent for argil grinding.
And (3) performance testing:
through testing, the weight average molecular weight of the polymer diluent for clay grinding is 15400, and the PDI is 1.19; the polymer diluent for grinding the argil is added into the slurry, wherein the mass of the macromolecular diluent is 0.2 percent of the mass of the argil, the viscosity of a slurry system is 375mPa & s, the flowing time is 60s, the argil blank does not have a sedimentation phenomenon after standing overnight, the stability is good, and the breaking strength of the obtained argil blank is improved by 160 percent compared with that of the argil blank without the polymer diluent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A preparation method of a polymer diluent for clay grinding is characterized by comprising the following steps: the method comprises the following steps: uniformly mixing an acrylic monomer, a chain transfer agent and water, adding an alkali solution until the pH value of a reaction solution is 7-8, vacuumizing, adding an initiator, carrying out polymerization reaction, cooling the reaction solution, and adding the alkali solution until the pH value of the reaction solution is 8-9 to obtain a polymer diluent for grinding the argil; the acrylic monomer is acrylic acid, sodium allylsulfonate, maleic anhydride and 2-acrylamide-2-methylpropanesulfonic acid according to the mass ratio (55-65): (10-15): (10-20): (10-20) in the presence of a catalyst.
2. The method of claim 1, wherein: the chain transfer agent is S, S ' -di (alpha, alpha ' -methyl-alpha ' -acetic acid) trithiocarbonate, and the mass of the chain transfer agent accounts for 1-4% of the total mass of the acrylic monomer and the water.
3. The method of claim 1, wherein: the initiator is ammonium persulfate, and the mass of the initiator accounts for 0.3-2.0% of the total mass of the acrylic monomer and the water.
4. The method of claim 1, wherein: the polymerization reaction is carried out at 60-75 ℃, and the reaction time is 4-6 h.
5. The method of claim 1, wherein: and dropwise adding the initiator into the reaction solution in the form of aqueous solution for 0.6-2 h.
6. The method of claim 1, wherein: the alkali solution is a sodium hydroxide solution with the mass fraction of 40-60%.
7. A polymer diluent for clay grinding, which is prepared by the method according to any one of claims 1 to 6.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675504A (en) * 2012-05-09 2012-09-19 中科院广州化学有限公司 Efficient water reducing agent for low-thixotropy ceramic slurry and preparation method thereof
CN102898575A (en) * 2012-06-08 2013-01-30 深圳市国大长兴科技有限公司 Ceramic slurry high-solid content promoter and preparation method thereof
CN103275264A (en) * 2013-05-08 2013-09-04 中科院广州化学有限公司 Water reducing agent capable of reducing viscosity of slurry as well as preparation method and application thereof
CN103304244A (en) * 2012-12-20 2013-09-18 中科院广州化学有限公司 High-polymer water reducing agent for ceramic concentrated suspension as well as preparation method and application of high-polymer water reducing agent

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102675504A (en) * 2012-05-09 2012-09-19 中科院广州化学有限公司 Efficient water reducing agent for low-thixotropy ceramic slurry and preparation method thereof
CN102898575A (en) * 2012-06-08 2013-01-30 深圳市国大长兴科技有限公司 Ceramic slurry high-solid content promoter and preparation method thereof
CN103304244A (en) * 2012-12-20 2013-09-18 中科院广州化学有限公司 High-polymer water reducing agent for ceramic concentrated suspension as well as preparation method and application of high-polymer water reducing agent
CN103275264A (en) * 2013-05-08 2013-09-04 中科院广州化学有限公司 Water reducing agent capable of reducing viscosity of slurry as well as preparation method and application thereof

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Address after: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318

Patentee after: Institute of chemical engineering, Guangdong Academy of Sciences

Address before: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318

Patentee before: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING