CN105061690A - Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid - Google Patents
Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid Download PDFInfo
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Abstract
The present invention relates to a preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid. The prepartion method specifically comprises the following steps: performing heat fusion on two unsaturated polyoxyethylene ether composite macromonomers with different molecular weights; then dropwise adding a mixed liquid of an unsaturated carboxylic micromonomer, an unsaturated amide micromonomer and a chain transfer agent under the reaction of an initiator; and preparing the water reducer through a free radical polymerization reaction, and after the reaction, using a neutralizing agent to adjust a pH value to 5-6 and then cooling and grinding the water reducer in a solid particulate shape. The preparation method provided by the present invention has advantages of being simple in process, high in conversion rate and environmental-friendly and free of pollution, and has the characteristics of high water reduction and low adulterate amount in concrete and dry-mixed mortar, and the transportation cost in long distance transportation is greatly lowered.
Description
Technical field
The present invention relates to the technical field of concrete admixture, be related specifically to a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer.
Background technology
The synthesis of tradition poly carboxylic acid series water reducer is formed by radical polymerization in aqueous, mother liquor product solid content is about 40%, this causes very large Cost Problems to long-distance transportation, can use after needing that liquid water reducer product is carried out spraying dry before using in dry-mix, but drying process with atomizing process energy consumption is high, in pyroprocess, the effective constituent of water reducer molecule reduces, and performance does not reach the water-reducing rate of liquid polycarboxylate water-reducer in actual applications.
Patent CN103012694A reports the preparation method of the pure solid high-performance polycarboxylate water-reducer of a kind of polyester type.This patent for reaction monomers, generates esterification polymeric monomer with (methyl) Acrylic Acid Monomer and polyethylene glycols under catalyst action, is being obtained by free radical bulk polymerization with unsaturated carboxylic acid monomer.Prepared by this invention two-step approach, complex process, and esterifying efficiency is large on late phase reaction impact, is difficult to form scale operation.
Patent CN102993387A reports a kind of method that a step directly synthesizes pure solid high-performance polycarboxylate water-reducer.This patent is carried out single stage method free radical bulk copolymerization with acrylic compounds and unsaturated Soxylat A 25-7 and is reacted the pure solid polycarboxylic acid water reducing agent be prepared from, this invention is without the need to heat drying or be separated the postprocessing working procedures such as solvent, but uses a kind of solid high-performance polycarboxylate water-reducer of unsaturated Soxylat A 25-7 synthesis of molecular weight still can not meet the requirement of high diminishing low-dosage.
The polycarboxylate water-reducer of pure solid not only will possess the high water-reducing property of conventional solution polycarboxylate water-reducer, and will realize work simplification, the production requirement of environmental protection.
Summary of the invention
The object of the invention is the preparation method providing a kind of high water reducing type solid high-performance polycarboxylate water-reducer in order to improve the deficiencies in the prior art, the high water reducing type solid high-performance polycarboxylate water-reducer adopting mass polymerization to synthesize under without any solvent environment, in order to improve the water-reducing rate of ready mixed concrete.
Technical scheme of the present invention is: a kind of preparation method of high water reducing type solid high-performance polycarboxylate water-reducer, concrete steps are as follows: unsaturated Soxylat A 25-7 combination polymeric monomer A and B of two kinds of different molecular weights is placed in still, after heating and melting, add initiator, start subsequently to drip unsaturated carboxylic acid class minor comonomer, the mixed solution of unsaturated acyl amine minor comonomer and chain-transfer agent, time for adding is 2 ~ 8h, at melt temperature insulation 1.5 ~ 3h after being added dropwise to complete, after being completed by free radical bulk polymerization, employing neutralizing agent adjustment pH is 5 ~ 6, after cooling through grinding be solid granular, the mass ratio of wherein said unsaturated Soxylat A 25-7 A, unsaturated Soxylat A 25-7 B, unsaturated carboxylic acid acids minor comonomer, unsaturated acyl amine minor comonomer, initiator, chain-transfer agent and neutralizing agent is 1:(0.08 ~ 0.25): (0.13 ~ 0.25): (0.01 ~ 0.02): (0.005 ~ 0.01): (0.01 ~ 0.015): (0.01 ~ 0.015).
Preferably above-mentioned unsaturated Soxylat A 25-7 polymeric monomer A is methyl allyl alcohol polyoxyethylene ether, isobutene alcohol Soxylat A 25-7 or isopentenol polyoxyethylene ether; Molecular weight is 2400 ~ 5000; Described unsaturated Soxylat A 25-7 polymeric monomer B is methoxy poly (ethylene glycol) monomethyl ether acrylate or methyl allyl alcohol polyoxyethylene ether; Molecular weight is 800 ~ 1400;
Preferably above-mentioned unsaturated carboxylic acid class minor comonomer is at least one in acrylic or methacrylic acid.
Preferably above-mentioned unsaturated acyl amine minor comonomer is at least one in acrylamide, n-methylolacrylamide or N-isopropylacrylamide.
Preferably above-mentioned initiator is at least one in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide or ammonium persulphate.
Preferably above-mentioned chain-transfer agent is at least one in Thiovanic acid, 2 mercaptopropionic acid or inferior sodium phosphate.
Preferably above-mentioned neutralizing agent is at least one in sodium hydroxide, calcium hydroxide, magnesium hydroxide or trolamine.
Preferred heating and melting temperature is 55 DEG C ~ 85 DEG C.
Beneficial effect:
1. the preparation method of a kind of high water reducing type high performance water reducing agent of polyocarboxy acid of the present invention adopts mass polymerization synthesis, the polycarboxylate water-reducer of preparation is pure solid phase prod, and transformation efficiency is high, and water-reducing rate is high, volume is low, stable storing, and greatly reduce transportation cost.
2. the present invention utilizes the copolymerization in without any solvent of the polyether macromonomer of different side chain lengths, space steric effect is defined three-dimensional arrangement, effectively improves the dissemination of water reducer in cement granules.
Embodiment
Below by embodiment, technical solution of the present invention is further described.
Embodiment 1
100g methyl allyl alcohol polyoxyethylene ether (molecular weight is 2400) and 25g methyl allyl alcohol polyoxyethylene ether (molecular weight is 1400) are placed in still, after being heated to 55 DEG C of meltings, add 0.5g Diisopropyl azodicarboxylate, start the mixed solution dripping 13g vinylformic acid, 1g acrylamide and 1g Thiovanic acid subsequently, time for adding is 2, after being added dropwise to complete 55 DEG C insulation 3h, add after react 1g sodium hydroxide adjust pH be 5.5, after cooling through grinding be solid granular.
Embodiment 2
100g isobutene alcohol Soxylat A 25-7 (molecular weight is 2900) and 20g methyl allyl alcohol polyoxyethylene ether (molecular weight is 1200) are placed in still, after being heated to 65 DEG C of meltings, add 0.6g 2,2'-Azobis(2,4-dimethylvaleronitrile), start the mixed solution dripping 15g vinylformic acid, 1.3g n-methylolacrylamide and 1.2g thiohydracrylic acid subsequently, time for adding is 3, at 65 DEG C of insulation 2h after being added dropwise to complete, add after having reacted 1.2g calcium hydroxide adjustment pH be 5, after cooling through grinding be solid granular.
Embodiment 3
400g isopentenol polyoxyethylene ether (molecular weight is 3500) and 60g methoxy poly (ethylene glycol) monomethyl ether acrylate (molecular weight is 800) are placed in still, after being heated to 60 DEG C of meltings, add 3.2g ammonium persulphate, start the mixed solution dripping 72g methacrylic acid, 6g N-isopropylacrylamide and 5.2g inferior sodium phosphate subsequently, time for adding is 5, at 60 DEG C of insulation 1.5h after being added dropwise to complete, add after having reacted 5.2g magnesium hydroxide adjustment pH be 5.3, after cooling through grinding be solid granular.
Embodiment 4
300g isobutene alcohol Soxylat A 25-7 (molecular weight is 5000) and 24g (0.08) methoxy poly (ethylene glycol) monomethyl ether acrylate (molecular weight is 1200) are placed in still, after being heated to 70 DEG C of meltings, add 2.1g Diisopropyl azodicarboxylate, start the mixed solution dripping 69g methacrylic acid, 5.4g acrylamide and 4.2g inferior sodium phosphate subsequently, time for adding is 6, at 70 DEG C of insulation 2h after being added dropwise to complete, add after having reacted 4.2g trolamine adjustment pH be 6, after cooling through grinding be solid granular.
Embodiment 5
360g methyl allyl alcohol polyoxyethylene ether (molecular weight is 2900) and 36g (0.1) methyl allyl alcohol polyoxyethylene ether (molecular weight is 1400) are placed in still, after being heated to 85 DEG C of meltings, add 3.6g benzoyl peroxide, start the mixed solution dripping 90g methacrylic acid, 7.2g n-methylolacrylamide and 5.4g2-thiohydracrylic acid subsequently, time for adding is 8, at 85 DEG C of insulation 1.5h after being added dropwise to complete, add after having reacted 5.4g calcium hydroxide adjustment pH be 5.5, after cooling through grinding be solid granular.
1. flowing degree of net paste of cement test
Test is with reference to GB8077-2000 " Methods for testing uniformity of concrete admixture ", and W/C=0.29, tests the paste flowing degree of each embodiment in reference cement under identical volume.Preferably liquid high-performance polycarboxylic acids water reducing agent (reference examples) is as a comparison sample to select existing commercially available performance.Test-results is in table 1
Table 1 pulp flowage results of property
As can be seen from Table 1, the high water reducing type solid polycarboxylic acid water reducing agent contrasting fluid height performance poly carboxylic acid series water reducer of the inventive method synthesis, has excellent clean slurry dispersing property when solid volume 0.15%.
2. testing concrete performance
Test with reference to GB8076-2008 " concrete admixture " to embodiment gained sample and commercially available performance preferably liquid high-performance polycarboxylic acids water reducing agent (reference examples) carry out concrete strength inspection.The solid volume of sample in cement is 0.28%, selects reference cement, and concrete mix is reference cement: sand: stone: water=360:812:1033:195.Test-results is in table 2
Table 2 concrete slump, divergence and ultimate compression strength
As can be seen from Table 2, high water reducing type solid poly carboxylic acid series water reducer prepared by the inventive method, shows excellent diminishing dispersing property compared with liquid high-performance polycarboxylic acids water reducing agent under low-dosage in concrete.
Claims (8)
1. the preparation method of one kind high water reducing type solid high-performance polycarboxylate water-reducer, its concrete steps are as follows: unsaturated Soxylat A 25-7 combination polymeric monomer A and B of two kinds of different molecular weights is placed in still, after heating and melting, add initiator, start the mixed solution dripping unsaturated carboxylic acid class minor comonomer, unsaturated acyl amine minor comonomer and chain-transfer agent subsequently, time for adding is 2 ~ 8h, under melt temperature, 1.5 ~ 3h is incubated after being added dropwise to complete, after being completed by free radical bulk polymerization employing neutralizing agent adjustment pH be 5 ~ 6, after cooling through grinding be solid granular; The mass ratio of wherein said unsaturated Soxylat A 25-7 A, unsaturated Soxylat A 25-7 B, unsaturated carboxylic acid acids minor comonomer, unsaturated acyl amine minor comonomer, initiator, chain-transfer agent and neutralizing agent is 1:(0.08 ~ 0.25): (0.13 ~ 0.25): (0.01 ~ 0.02): (0.005 ~ 0.01): (0.01 ~ 0.015): (0.01 ~ 0.015).
2. preparation method according to claim 1, is characterized in that described unsaturated Soxylat A 25-7 polymeric monomer A is methyl allyl alcohol polyoxyethylene ether, isobutene alcohol Soxylat A 25-7 or isopentenol polyoxyethylene ether; Molecular weight is 2400 ~ 5000; Described unsaturated Soxylat A 25-7 polymeric monomer B is methoxy poly (ethylene glycol) monomethyl ether acrylate or methyl allyl alcohol polyoxyethylene ether; Molecular weight is 800 ~ 1400.
3. preparation method according to claim 1, is characterized in that described unsaturated carboxylic acid class minor comonomer is at least one in acrylic or methacrylic acid.
4. preparation method according to claim 1, is characterized in that described unsaturated acyl amine minor comonomer is at least one in acrylamide, n-methylolacrylamide or N-isopropylacrylamide.
5. preparation method according to claim 1, is characterized in that described initiator is at least one in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), benzoyl peroxide or ammonium persulphate.
6. preparation method according to claim 1, is characterized in that described chain-transfer agent is at least one in Thiovanic acid, 2 mercaptopropionic acid or inferior sodium phosphate.
7. preparation method according to claim 1, is characterized in that described neutralizing agent is at least one in sodium hydroxide, calcium hydroxide, magnesium hydroxide or trolamine.
8. preparation method according to claim 1, is characterized in that the temperature of heating and melting is 55 DEG C ~ 85 DEG C.
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| CN105669919A (en) * | 2016-01-14 | 2016-06-15 | 厦门路桥翔通建材科技有限公司 | Polycarboxylate superplasticizer with high water retention and preparation method thereof |
| CN105754034A (en) * | 2016-03-09 | 2016-07-13 | 合众（佛山）化工有限公司 | N-Methylolacrylamide modified polycarboxylate ceramic water reducer and normal-temperature preparation method and application thereof |
| CN106543382A (en) * | 2016-12-07 | 2017-03-29 | 湖北工业大学 | A kind of solid lamellar polycarboxylate water-reducer and its polymerization process for preparing |
| CN106749970A (en) * | 2016-12-07 | 2017-05-31 | 湖北工业大学 | A kind of solid sheet polycarboxylic acid slump retaining agent and preparation method thereof |
| CN106749965A (en) * | 2016-12-01 | 2017-05-31 | 科之杰新材料集团有限公司 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
| CN107446088A (en) * | 2017-07-27 | 2017-12-08 | 安徽中铁工程材料科技有限公司 | A kind of preparation method of the high water reducing type polycarboxylate water-reducer of high solids content ethers |
| CN107739424A (en) * | 2017-11-07 | 2018-02-27 | 上海三瑞高分子材料股份有限公司 | A kind of solid protects the polycarboxylate water-reducer and preparation method thereof that collapses |
| CN107987223A (en) * | 2017-11-30 | 2018-05-04 | 湖北工业大学 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
| CN108047392A (en) * | 2017-12-18 | 2018-05-18 | 广东瑞铠实业发展有限公司 | The preparation method of high concentration polycarboxylate water-reducer |
| CN108349806A (en) * | 2015-11-30 | 2018-07-31 | 罗门哈斯公司 | High solids content polycarboxylate for cement super plasticizer synthesizes |
| CN108409918A (en) * | 2018-03-08 | 2018-08-17 | 安徽中铁工程材料科技有限公司 | Preparation method of high-solid-content ether slump-retaining type polycarboxylate superplasticizer |
| CN108675828A (en) * | 2018-06-28 | 2018-10-19 | 来安县塔鑫建材有限公司 | A kind of highway good concrete of heat-insulated durability |
| CN109250960A (en) * | 2017-07-14 | 2019-01-22 | 浙江和业科技有限公司 | A kind of polycarboxylic acids makes the application of concrete in Machine-made Sand |
| CN109928661A (en) * | 2019-04-15 | 2019-06-25 | 山西格瑞特建筑科技股份有限公司 | A kind of viscosity reduction type solid polycarboxylic acid water reducing agent and preparation method thereof |
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| CN113603839A (en) * | 2021-08-27 | 2021-11-05 | 贵州凯襄新材料有限公司 | Composite polycarboxylic acid water reducing agent and preparation method and application thereof |
| CN115073678A (en) * | 2021-10-08 | 2022-09-20 | 长沙理工大学 | High-adaptability ether polycarboxylic acid and preparation method thereof |
| CN115340640A (en) * | 2021-05-12 | 2022-11-15 | 南京博特新材料有限公司 | Preparation method of viscosity-reduction type solid polycarboxylate superplasticizer |
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