CN104058751A - Polymer water reducing agent used for ceramic machining and synthetic method thereof - Google Patents
Polymer water reducing agent used for ceramic machining and synthetic method thereof Download PDFInfo
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Abstract
The invention relates to a polymer water reducing agent used for ceramic machining and a synthetic method of the polymer water reducing agent used for ceramic machining. The method is characterized in that firstly, macromolecule unsaturated monomers containing polyether long chains are copolymerized under the action of radical initiators to form intermediate state polymers, then the other part of unsaturated acid and radical imitators are added, copolymerization is performed continuously, and finally neutralizing is performed to obtain the polymer water reducing agent. The polymer water reducing agent is high in water-reducing rate and dispersing and plasticizing capacity and can be applied to the technological processes of powder making, slip casting and others in the ceramic industry and dispersing pigment and fillings in coating and ink.
Description
Technical field
The invention belongs to ceramic processing aid field, be specifically related to a kind of pottery processing polyalcohol water reducing agent and synthetic method thereof.
Background technology
Pottery is a resource industry, and China will consume the non-renewable mineral wealth such as a large amount of clays, gypsum every year, causes many tonerde storages significantly to reduce, and some areas are approach exhaustion.And pottery is also the industry that high energy gamma source consumes, energy consumption accounts for 1/3rd of Production of Ceramics cost, will consume a large amount of electric energy and combustion gas every year.Therefore, reducing energy consumption, improving resource utilization is ceramic industry problem demanding prompt solution.
Water reducer, as applying maximum additives in the ceramic course of processing, can not only reduce costs, and can also further improve ceramic product performance.If do not add water reducer, free water easily enters in clay particle, makes the Distance Shortened between particle, need to add a lot of water and just can make base, glaze have mobility.After adding water reducer, at surface of clay, form hydrophobic structure and double electrical layers, intergranular like this repulsive force increases, free water increases, thereby improves the mobility of slip.Under the condition of equal amount of water, add the mobility of the slip of water reducer to improve, uniformity coefficient, the settlement prevention of particle can be improved, and setting time can be shortened, improve intensity, thereby make Production of Ceramics person obtain higher economic value added and social benefit.
Along with developing rapidly of ceramic industry, traditional ceramic additive oneself can not adaption demand.Countries in the world are all at active research and the new and effective ceramic water reducing agent of application.Polyalcohol water reducing agent adds in ceramic size, not only can significantly improve slip mobility and stability, can also reduce water ratio, and then reduces the production cost that pottery is manufactured.Along with the development of ceramics, the production of high quality pottery more and more be unable to do without polyalcohol water reducing agent.Compared with developed countries, the overall study level of China's ceramic water reducing agent is not high, and existing polycarboxylate sodium and organic sulfonate all can not meet the needs in market.
For overcoming the above problems, the invention provides a kind of pottery processing polyalcohol water reducing agent and synthetic method thereof.
Summary of the invention
The object of the invention is to provide a kind of high performance pottery processing polyalcohol water reducing agent and synthetic method thereof.
To achieve these goals, technical solution of the present invention is, the polyalcohol water reducing agent of preparing by radical polymerization, and its chemical structural formula is expressed as:
A is: Na, or K, or NH
4;
K, L, M, N is for repeating link units number: 20≤K≤60,2≤L≤10,5≤M≤20,30≤N≤300.
Above-mentioned polyalcohol water reducing agent and synthetic method thereof, it comprises the following steps:
1) radical polymerization, minute low temperature causes technique and high temperature causes two kinds of techniques.
(1) low temperature causes technique, in reactor, add macromole unsaturated monomer and appropriate amount of deionized water containing polyethers long-chain, be warming up to 30～50 ℃ of stirring and dissolving, add superoxol 1, slowly drip unsaturated carboxylic acid 1, xitix 1 and the chain-transfer agent aqueous solution simultaneously, control and in approximately 3 hours, drip unsaturated carboxylic acid, within 3.5 hours, add xitix 1 aqueous solution, continue reaction 1 hour, obtain a kind of intermediate state polymkeric substance.Again in reactor, add superoxol 2, drip unsaturated carboxylic acid 2 and xitix 2 aqueous solution simultaneously slowly, control and in approximately 2 hours, drip unsaturated carboxylic acid and within 2,2.5 hours, add xitix 2 aqueous solution, continue reaction 1-2 hour copolymerization product.
Its reaction raw materials proportioning is:
Containing the macromole unsaturated monomer of polyethers long-chain and the mol ratio of unsaturated acid 1, be 1:3～1:6;
Hydrogen peroxide 1 is 0.1～1.0% of the macromole unsaturated monomer quality containing polyethers long-chain;
Xitix 1 is 0.1～0.5% of the macromole unsaturated monomer quality containing polyethers long-chain;
Chain-transfer agent 1 is 0.2～1.0% of the macromole unsaturated monomer quality containing polyethers long-chain;
Containing the macromole unsaturated monomer of polyethers long-chain and the mol ratio of unsaturated acid 2, be 1:15～1:60;
Hydrogen peroxide 2 is 0.3～3.0% of the macromole unsaturated monomer quality containing polyethers long-chain;
Xitix 2 is 0.3～2.0% of the macromole unsaturated monomer quality containing polyethers long-chain.
(2) high temperature causes technique, in reactor, add macromole unsaturated monomer, chain-transfer agent and appropriate amount of deionized water containing polyethers long-chain, be warming up to 70～90 ℃ of stirring and dissolving, slowly drip respectively unsaturated carboxylic acid 1 and ammonium persulphate 1 aqueous solution, control and in approximately 3 hours, drip unsaturated carboxylic acid, within 3.5 hours, add ammonium persulphate 1 aqueous solution, continue reaction 1 hour, obtain a kind of intermediate state polymkeric substance.Again to slowly dripping respectively unsaturated carboxylic acid 2 and ammonium persulphate 2 aqueous solution in reactor, controlling, in approximately 2 hours, drip unsaturated carboxylic acid and within 2,2.5 hours, add ammonium persulphate 2 aqueous solution, continue reaction 1 hour copolymerization product.
Its reaction raw materials proportioning is:
Containing the macromole unsaturated monomer of polyethers long-chain and the mol ratio of unsaturated acid 1, be 1:3～1:6;
Ammonium persulphate 1 is 0.5～2.0% of the macromole unsaturated monomer quality containing polyethers long-chain;
Chain-transfer agent 1 is 0.2～1.0% of the macromole unsaturated monomer quality containing polyethers long-chain;
Containing the macromole unsaturated monomer of polyethers long-chain and the mol ratio of unsaturated acid 2, be 1:15～1:60;
Ammonium persulphate 2 is 1.0～3.0% of macromole unsaturated monomer quality.
2) neutralizing treatment
After gained copolymerization product is cooling, slowly add basic solution, as ammoniacal liquor or sodium hydroxide or potassium hydroxide solution are neutralized to pH value 7 left and right, obtain poly carboxylic acid fluidizer.
The described macromole unsaturated monomer containing polyethers long-chain is allyl alcohol polyethenoxy ether or propyl alcohol polyoxyethylene polyoxypropylene copolyether or prenol Soxylat A 25-7 or prenol polyoxyethylene polyoxypropylene copolyether; ;
Described unsaturated carboxylic acid is acrylic or methacrylic acid;
Described chain-transfer agent is Virahol or Thiovanic acid or thiohydracrylic acid or lauryl mercaptan.
The invention has the advantages that:
Polyalcohol water reducing agent of the present invention has the advantages that water-reducing rate is high, plasticizing capacity is strong, adaptability is good, can be applicable to the technological process such as abrasive dust, slurrying, idiosome moulding of ceramic industry, and the dispersion of pigment and filler in coating, ink.In ceramic abrasive dust, can promote powder to disperse, improve abrasive dust efficiency, conserve energy; In ceramic powder slurrying, can greatly reduce the dispersion of water consumption, promotion powder, the mobility of raising slurry, can greatly save the dry required energy of slurry simultaneously; Intensity and the ratio of briquetting that when idiosome moulding, can reduce water consumption, raising idiosome, increase ceramic density; In coating, ink, can promote the dispersion of pigment and filler and prevent coagulation.
Embodiment
In conjunction with example, further illustrate content of the present invention, but the present invention is not only confined to following instance.
Example 1:
The allyl alcohol polyethenoxy ether 145kg that is 2000 by molecular weight, water 120kg add reactor, are heated to 30 ℃ and stirring, after allyl alcohol polyethenoxy ether is dissolved completely, add hydrogen peroxide (mass concentration 35%) 1.2kg.
In No. 1 header tank, add vinylformic acid 18kg and deionized water 20kg, in No. 2 header tanks, add xitix 0.2kg, Virahol 1.0kg and deionized water 38kg, then solution in two header tanks is slowly added to reactor simultaneously, control that liquid in No. 1 header tank adds for approximately 3 hours, liquid adds for approximately 3.5 hours in No. 2 header tanks.In No. 3 header tanks, add vinylformic acid 80kg, to No. 4 header tanks, add xitix 0.5kg and deionized water 80kg.After in No. 2 header tanks, liquid adds, continue constant temperature stirring reaction 1.0 hours, obtain a kind of intermediate state polymkeric substance.Then in reactor, add 1.5kg hydrogen peroxide (mass concentration 35%), open No. 3 and No. 4 header tank valves, slowly in reactor, add vinylformic acid and aqueous ascorbic acid, control that liquid in No. 3 header tanks adds for approximately 2 hours, liquid approximately 2.5 hours in No. 4 header tanks, add rear continuation isothermal reaction 2.0 hours, after cooling, add ammonia neutralization and obtain 1# polyalcohol water reducing agent, its chemical structural formula is as follows:
1# poly carboxylic acid fluidizer is applied to alumina slurry preparation, the alumina slurry of addition 0.2%, water content 20%, with rotational viscosimeter normal temperature, measuring viscosity is 200cP, with coating-4 viscosity meter, is determined as 30s, flowing property is good, and static 24 hours of slurry is without demixing phenomenon.
Example 2:
The allyl alcohol polyethenoxy polyoxypropylene copolyether 150kg, the water 120kg that by molecular weight, are 2400 add reactor, are heated to 30 ℃ and stirring, after allyl alcohol polyethenoxy ether is dissolved completely, add hydrogen peroxide (mass concentration 35%) 1.0kg.
In No. 1 header tank, add vinylformic acid 15kg and deionized water 20kg, in No. 2 header tanks, add xitix 0.2kg, Virahol 1.0kg and deionized water 38kg, then solution in two header tanks is slowly added to reactor simultaneously, control that liquid in No. 1 header tank adds for approximately 3 hours, liquid adds for approximately 3.5 hours in No. 2 header tanks.In No. 3 header tanks, add vinylformic acid 100kg, to No. 4 header tanks, add xitix 0.4kg and deionized water 100kg.After in No. 2 header tanks, liquid adds, continue constant temperature stirring reaction 1.0 hours, obtain a kind of intermediate state polymkeric substance.Then in reactor, add 1.2kg hydrogen peroxide (mass concentration 35%), open No. 3 and No. 4 header tank valves, slowly in reactor, add vinylformic acid and aqueous ascorbic acid, control that liquid in No. 3 header tanks adds for approximately 2 hours, liquid approximately 2.5 hours in No. 4 header tanks, add rear continuation isothermal reaction 2.0 hours, after cooling, add ammonia neutralization and obtain 2# polyalcohol water reducing agent, its chemical structural formula is as follows:
2# poly carboxylic acid fluidizer is applied to alumina slurry preparation, the alumina slurry of addition 0.3%, water content 20%, with rotational viscosimeter normal temperature, measuring viscosity is 160cP, with coating-4 viscosity meter, is determined as 26s, flowing property is good, and static 24 hours of slurry is without demixing phenomenon.
Example 3:
The prenol polyoxyethylene polyoxypropylene copolyether 180kg, the water 120kg that by molecular weight, are 2400 add reactor, are heated to 30 ℃ and stirring, after allyl alcohol polyethenoxy ether is dissolved completely, add hydrogen peroxide (mass concentration 35%) 1.2kg.
In No. 1 header tank, add vinylformic acid 20kg and deionized water 20kg, in No. 2 header tanks, add xitix 0.2kg, Thiovanic acid 0.5kg and deionized water 38kg, then solution in two header tanks is slowly added to reactor simultaneously, control that liquid in No. 1 header tank adds for approximately 3 hours, liquid adds for approximately 3.5 hours in No. 2 header tanks.In No. 3 header tanks, add vinylformic acid 100kg, to No. 4 header tanks, add xitix 0.5kg and deionized water 100kg.After in No. 2 header tanks, liquid adds, continue constant temperature stirring reaction 1.0 hours, obtain a kind of intermediate state polymkeric substance.Then in reactor, add 1.5kg hydrogen peroxide (mass concentration 35%), open No. 3 and No. 4 header tank valves, slowly in reactor, add vinylformic acid and aqueous ascorbic acid, control that liquid in No. 3 header tanks adds for approximately 2 hours, liquid approximately 2.5 hours in No. 4 header tanks, add rear continuation isothermal reaction 2.0 hours, cooling back end hydrogenation sodium hydroxide solution neutralization obtains 3# polyalcohol water reducing agent, and its chemical structural formula is as follows:
3# poly carboxylic acid fluidizer is applied to alumina slurry preparation, the alumina slurry of addition 0.3%, water content 20%, with rotational viscosimeter normal temperature, measuring viscosity is 150cP, with coating-4 viscosity meter, is determined as 25s, flowing property is good, and static 24 hours of slurry is without demixing phenomenon.
Example 4:
The allyl alcohol polyethenoxy polyoxypropylene copolyether 120kg, water 120kg, the Virahol 1.5kg that by molecular weight, are 2400 add reactor, are heated to 80 ℃ and stirring, make allyl alcohol polyethenoxy ether completely molten.
In No. 1 header tank, add vinylformic acid 15kg and deionized water 20kg, in No. 2 header tanks, add ammonium persulphate 3.0kg and deionized water 38kg, then solution in two header tanks is slowly added to reactor simultaneously, control that liquid in No. 1 header tank adds for approximately 3 hours, liquid adds for approximately 3.5 hours in No. 2 header tanks.In No. 3 header tanks, add vinylformic acid 80kg, to No. 4 header tanks, add ammonium persulphate 2.0kg and deionized water 100kg.After in No. 2 header tanks, liquid adds, continue constant temperature stirring reaction 1.0 hours, obtain a kind of intermediate state polymkeric substance.Open No. 3 and No. 4 header tank valves, slowly in reactor, add vinylformic acid and ammonium persulfate aqueous solution, control that liquid in No. 3 header tanks adds for approximately 2 hours, liquid approximately 2.5 hours in No. 4 header tanks, add rear continuation isothermal reaction 1.0 hours, after cooling, add ammonia neutralization and obtain 4# polyalcohol water reducing agent, its chemical structural formula is as follows:
4# poly carboxylic acid fluidizer is applied to alumina slurry preparation, the alumina slurry of addition 0.3%, water content 20%, with rotational viscosimeter normal temperature, measuring viscosity is 220cP, with coating-4 viscosity meter, is determined as 38s, flowing property is good, and static 24 hours of slurry is without demixing phenomenon.
As known by the technical knowledge, the present invention can realize by other the embodiment that does not depart from its spirit or essential feature.Therefore, above-mentioned disclosed embodiment, with regard to each side, all just illustrates, and is not only.Change within the scope of the present invention all or within being equal to scope of the present invention is all included in the invention.
Claims (8)
1. a pottery processing polyalcohol water reducing agent, is characterized in that: its chemical structure of general formula is expressed as:
Wherein, X is:
, or;
R
1, R
2, R
3, R
4for H or CH
3;
A is: Na, or K, or NH
4;
K, L, M, N is for repeating link units number: 20≤K≤60,2≤L≤10,5≤M≤20,30≤N≤300.
2. pottery is processed the synthetic method with polyalcohol water reducing agent as claimed in claim 1, it is characterized in that, affiliated radical polymerization step is that low temperature causes technique, comprising:
(1) in reactor, add macromole unsaturated monomer and the appropriate amount of deionized water containing polyethers long-chain, be warming up to 30～50 ℃ of stirring and dissolving, add for the first time superoxol, slowly drip respectively unsaturated carboxylic acid, xitix and the chain-transfer agent aqueous solution simultaneously, control for the first time and in approximately 3 hours, drip unsaturated carboxylic acid, within 3.5 hours, add aqueous ascorbic acid, continue reaction 1 hour, obtain a kind of intermediate state polymkeric substance;
In reactor, add superoxol for the second time, slowly drip respectively unsaturated carboxylic acid and aqueous ascorbic acid simultaneously, control and in approximately 2 hours, drip unsaturated carboxylic acid, within 2.5 hours, add aqueous ascorbic acid, add rear continuation isothermal reaction 1-2 hour copolymerization product;
(2) neutralizing treatment step:
After described copolymerization product is cooling, slowly add basic solution to be neutralized to pH value 7 left and right, obtain polyalcohol water reducing agent.
3. the synthetic method of polyalcohol water reducing agent for pottery processing as claimed in claim 2, is characterized in that, the reaction raw materials proportioning that described low temperature causes in technique is respectively:
The hydrogen peroxide adding is for the first time 0.1～1.0% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The described macromole unsaturated monomer containing polyethers long-chain is 1:3～1:6 with the mol ratio of the unsaturated carboxylic acid adding for the first time;
The xitix adding is for the first time 0.1～0.5% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The chain-transfer agent adding is for the first time 0.2～1.0% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The described macromole unsaturated monomer containing polyethers long-chain is 1:15～1:60 with the mol ratio of the unsaturated acid adding for the second time; The hydrogen peroxide adding is for the second time 0.3～3.0% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The xitix adding is for the second time 0.3～2.0% of the described macromole unsaturated monomer quality containing polyethers long-chain.
4. pottery is processed the synthetic method with polyalcohol water reducing agent as claimed in claim 1, it is characterized in that, affiliated radical polymerization step is that high temperature causes technique, comprising:
(1) in reactor, add macromole unsaturated monomer, chain-transfer agent and the appropriate amount of deionized water containing polyethers long-chain, be warming up to 70～90 ℃ of stirring and dissolving, slowly drip respectively for the first time unsaturated carboxylic acid and ammonium persulfate aqueous solution; Control and in approximately 3 hours, drip unsaturated carboxylic acid, within 3.5 hours, add ammonium persulfate aqueous solution; Continue reaction 1 hour, obtain a kind of intermediate state polymkeric substance;
For the second time to slowly dripping respectively unsaturated carboxylic acid and ammonium persulfate aqueous solution in reactor, control and in approximately 2 hours, drip unsaturated carboxylic acid, within 2.5 hours, add ammonium persulfate aqueous solution, continue reaction 1 hour copolymerization product;
(2) neutralizing treatment step:
After described copolymerization product is cooling, slowly add basic solution to be neutralized to pH value 7 left and right, obtain polyalcohol water reducing agent.
5. the synthetic method of polyalcohol water reducing agent for pottery processing as claimed in claim 4, is characterized in that, described reaction raw materials proportioning is:
The chain-transfer agent adding is for the first time 0.2～1.0% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The described macromole unsaturated monomer containing polyethers long-chain is 1:3～1:6 with the mol ratio of the unsaturated acid adding for the first time;
The ammonium persulphate adding is for the first time 0.5～2.0% of the described macromole unsaturated monomer quality containing polyethers long-chain;
The described macromole unsaturated monomer containing polyethers long-chain is 1:15～1:60 with the mol ratio of the unsaturated acid adding for the second time;
The ammonium persulphate adding is for the second time 1.0～3.0% of the described macromole unsaturated monomer quality containing polyethers long-chain.
6. as described in any one in claim 2-5, pottery is processed the synthetic method with polyalcohol water reducing agent, it is characterized in that:
The described macromole unsaturated monomer containing polyethers long-chain is allyl alcohol polyethenoxy ether or propyl alcohol polyoxyethylene polyoxypropylene copolyether or prenol Soxylat A 25-7 or prenol polyoxyethylene polyoxypropylene copolyether;
Described unsaturated carboxylic acid is acrylic or methacrylic acid;
Described chain-transfer agent is Virahol or Thiovanic acid or thiohydracrylic acid or lauryl mercaptan.
7. as described in any one in claim 2-5, pottery is processed the synthetic method with polyalcohol water reducing agent, it is characterized in that, the basic solution in described neutralizing treatment step is ammoniacal liquor or sodium hydroxide or potassium hydroxide solution.
8. pottery is processed the synthetic method with polyalcohol water reducing agent as claimed in claim 6, it is characterized in that, the basic solution in described neutralizing treatment step is ammoniacal liquor or sodium hydroxide or potassium hydroxide solution.
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Cited By (4)
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| CN104910315A (en) * | 2015-07-14 | 2015-09-16 | 唐山市龙亿科技开发有限公司 | Method for preparing polycarboxylate-type ceramic dispersant by use of normal temperature method |
| CN106496442A (en) * | 2016-10-27 | 2017-03-15 | 湖南大学 | A kind of high-efficiency water-reducing agent of poly-carboxylic acid and preparation method thereof |
| CN109503776A (en) * | 2018-12-03 | 2019-03-22 | 广东科隆智谷新材料股份有限公司 | A kind of preparation method of polyocarboxy acid type ceramic dispersants |
| CN112851373A (en) * | 2021-02-01 | 2021-05-28 | 湖北工业大学 | High-dispersity ceramic water reducing agent and preparation method thereof |
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| CN103183788A (en) * | 2011-12-27 | 2013-07-03 | 山西黄腾化工有限公司 | Preparation method for polycarboxylic acid type concrete slump-retaining agent |
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| CN103183788A (en) * | 2011-12-27 | 2013-07-03 | 山西黄腾化工有限公司 | Preparation method for polycarboxylic acid type concrete slump-retaining agent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910315A (en) * | 2015-07-14 | 2015-09-16 | 唐山市龙亿科技开发有限公司 | Method for preparing polycarboxylate-type ceramic dispersant by use of normal temperature method |
| CN106496442A (en) * | 2016-10-27 | 2017-03-15 | 湖南大学 | A kind of high-efficiency water-reducing agent of poly-carboxylic acid and preparation method thereof |
| CN106496442B (en) * | 2016-10-27 | 2018-11-06 | 湖南大学 | A kind of high-efficiency water-reducing agent of poly-carboxylic acid and preparation method thereof |
| CN109503776A (en) * | 2018-12-03 | 2019-03-22 | 广东科隆智谷新材料股份有限公司 | A kind of preparation method of polyocarboxy acid type ceramic dispersants |
| CN112851373A (en) * | 2021-02-01 | 2021-05-28 | 湖北工业大学 | High-dispersity ceramic water reducing agent and preparation method thereof |
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