CN103183793B - Synthetic method of polycarboxylic acid type highly slump loss resistant water-reducing agent - Google Patents
Synthetic method of polycarboxylic acid type highly slump loss resistant water-reducing agent Download PDFInfo
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- CN103183793B CN103183793B CN201310097839.7A CN201310097839A CN103183793B CN 103183793 B CN103183793 B CN 103183793B CN 201310097839 A CN201310097839 A CN 201310097839A CN 103183793 B CN103183793 B CN 103183793B
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Abstract
The invention relates to the technical field of building material synthesis and particularly discloses a synthetic method of polycarboxylic acid type highly slump loss resistant water-reducing agent. The method comprises the following steps: 1, water treatment agent and acrylic acid-maleic anhydride copolymer are added into tap water until the content of acrylic acid-maleic anhydride copolymer is 3-8mg/L so as to obtain treating water; and 2, backing material formed by unsaturated polyoxyethylene ether, maleic anhydride, functional small monomer, and treating water is added into a polyreactor, the temperature is increased to be 40 DEG C and stirring is performed till the mixture is completely dissolved resolution, NaOH solution is used for adjusting pH to 4, then a proper amount of hydrogen peroxide is added, and mixed solution composed of acrylic acid, ammonium ferrous sulfate, a cross-linking agent, a chain transfer agent and treating water well prepared in advance is dripped; dripping is finished within 2.5 to 4 h, thermal insulation is continuously performed for 0.5 to 1 h after dripping, and NaOH solution is used for neutralization to pH 5-6. The method provided by the invention has the advantages that the process is simple, the conditions are mild, the feedstock conversion rate is high, tap water can be used as raw materials, the cost is greatly reduced, and the slump loss resistance of products is obviously superior to that in the prior art.
Description
Technical field
The present invention relates to the synthesis technical field of material of construction, be specifically related to a kind of synthetic method of the reinforcement of concrete poly carboxylic acid series water reducer, more specifically relate to a kind of synthetic method of polyocarboxy acid type high-thin arch dam water reducer.
Background technology
Poly carboxylic acid series water reducer is because of excellent performance and the advantages such as environmental protection are called as third generation high-performance water reducing agent.Along with country continues to greatly develop capital construction, and require more and more higher to concrete, shared by poly carboxylic acid series water reducer, the market share is increasing.Have high water reducing rate, the polycarboxylate water-reducer of high-thin arch dam performance has the more favourable market competitiveness.
The production technique of current polycarboxylate water-reducer mainly contains two classes, and a kind of is ester type, take MPEG as raw material, and by first esterification, prepared by resynthesis.Although this technique cost of material is cheap, due to complex procedures, length consuming time, quality difficulty controls, and the temperature required height of esterification, therefore energy consumption cost and cost of labor high; Another kind is polyether-type, with unsaturated Soxylat A 25-7 and unsaturated carboxylic acid and other monomer, and direct polymerization under initiator effect.This technique comparatively ester type is simple, consuming time short, and production capacity is large, energy consumption and cost of labor low.But guarantor's ability of collapsing of polyether-type product needs to be improved further at present.
Current polycarboxylate water-reducer is higher to water quality requirement in producing, and is generally all through softening water or the deionized water of process, if tap water can be used to synthesize will simplify widely production technique to go forward side by side a step-down low cost.
Summary of the invention
The object of the invention is to solve current Polyether polycarboxylic-acid water reducer and protect scarce capacity problem of collapsing, with unsaturated Soxylat A 25-7 for raw material, at a lower temperature, synthesize a kind of water reducer with high-thin arch dam performance with tap water.
The object of the invention is to be achieved through the following technical solutions:
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
(1) preparation of water, is processed: in tap water, add water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA), be 3-8mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of described acrylic acid-maleic anhydride copolymer is 2000-5000, vinylformic acid in described acrylic acid-maleic anhydride copolymer: the mol ratio of maleic anhydride is 1.1-1.5:1.
(2), synthesis: bed material (is comprised unsaturated Soxylat A 25-7, maleic anhydride, functional minor comonomer and process water) add polymerization reaction kettle, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add proper amount of hydrogen peroxide again, drip prepare in advance by vinylformic acid, ferrous ammonium sulphate, linking agent, the mixing solutions of chain-transfer agent and process water composition, within 2.5-4 hour, drip, dropwise follow-up continuation of insurance temperature 0.5-1.5 hour, being neutralized to pH value with the 32wt%NaOH aqueous solution is 5-6, obtain product, tap water adjustment solids content to 40% is added before using.
In described step (2), the molecular weight of unsaturated Soxylat A 25-7 is at 1000-3000;
In described step (2), unsaturated Soxylat A 25-7 is isopentenol polyoxyethylene ether and/or methacrylic Soxylat A 25-7;
In described step (2), functional minor comonomer is 2-acrylamide-2-methyl propane sulfonic (AMPS) and/or methylpropene sodium sulfonate (MAS);
In described step (2), linking agent is N, N'-methylene-bisacrylamide;
In described step (2), chain-transfer agent is thiohydracrylic acid or methylpropene sodium sulfonate (MAS);
Described maleic anhydride and acrylic acid molar weight sum are 3.0-5.0 times of unsaturated Soxylat A 25-7, and wherein the molar weight of maleic anhydride accounts for the 5%-50% of maleic anhydride and vinylformic acid integral molar quantity;
Described functional minor comonomer and unsaturated Soxylat A 25-7 mol ratio 0.05-0.5:1;
Described hydrogen peroxide accounts for the 0.5-3% of all monomer total masses;
The 30%-50% that water accounts for bed material total mass is processed in described bed material;
Ferrous ammonium sulphate in described mixing solutions and described hydrogen peroxide mol ratio 1:2-5, described chain-transfer agent accounts for the 0.1-2% of all monomer total masses, and linking agent accounts for the 0.1-0.5% of all monomer total masses;
Described all monomers comprise unsaturated Soxylat A 25-7, vinylformic acid, maleic anhydride and functional minor comonomer;
The 70-90% that water accounts for mixing solutions total mass is processed in described mixing solutions.
Compared with prior art, advantage of the present invention and beneficial effect are:
1, have employed ferrous ammonium sulphate-hydrogen peroxide redox system, and ferrous ammonium sulphate has the function of adjustment polymerization activity, the transformation efficiency of maleic anhydride can be improved while reducing temperature of reaction.
2, by adding the metal ion in organic sequestering agent PAA-PMA shielding tap water in tap water, it is eliminated on the impact of synthesizing, lower than the preparation cost of general water technology process water, the cost of new production line equipment can also be saved.
3, maleic anhydride replaces part acrylic acid, and 40 DEG C of synthesis, cost is lower.
Embodiment
Applicant will be described in further detail the inventive method in conjunction with specific embodiments below.
Embodiment 1
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 6mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 5000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.5:1.
Second step, synthesis: drop into isopentenol polyoxyethylene ether (molecular weight 2400) 240g in the reactor being furnished with thermometer and electric stirring, maleic anhydride 20g, 2-acrylamide-2-methyl propane sulfonic AMPS4g and process water 110g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 1.8g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 11g vinylformic acid, 1.4g ferrous ammonium sulphate, 0.6g N, N'-methylene-bisacrylamide, the mixing solutions of 0.8g thiohydracrylic acid and 130g process water composition, within 3 hours, drip and finish, then insulation 1 hour is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-1, adding tap water adjustment solids content is 40%, for subsequent use.
Embodiment 2
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 3mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 4000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.4:1.
Second step, synthesis: drop into isopentenol polyoxyethylene ether (molecular weight 2400) 252g in the reactor being furnished with thermometer and electric stirring, maleic anhydride 20g, AMPS6g and process water 116g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 1.47g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 10g vinylformic acid, 1.33g ferrous ammonium sulphate, 0.64g N, N'-methylene-bisacrylamide, the mixing solutions of 2.1g methylpropene sodium sulfonate (MAS) and 130g process water composition, within 3.5 hours, drip and finish, then insulation 1 hour is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-2, adding tap water adjustment solids content is 40%, for subsequent use.
Embodiment 3
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 8mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 2000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.1:1.
Second step, synthesis: drop into methyl allyl alcohol polyoxyethylene ether (molecular weight 2400) 360g in the reactor being furnished with thermometer and electric stirring, maleic anhydride 20g, methylpropene sodium sulfonate 4g and process water 165g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 1.9g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 15g vinylformic acid, 1.75g ferrous ammonium sulphate, 0.55g N, N'-methylene-bisacrylamide, the mixing solutions of 0.6g thiohydracrylic acid and 185g process water composition, within 4 hours, drip and finish, then insulation 0.5 hour is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-3, adding by tap water adjustment solids content is 40%, for subsequent use.
Embodiment 4
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 4mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 3000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.3:1.
Second step, synthesis: drop into isopentenol polyoxyethylene ether (molecular weight 2400) 225g in the reactor being furnished with thermometer and electric stirring, methyl allyl alcohol polyoxyethylene ether (molecular weight 2400) 100g, maleic anhydride 25g, 2-acrylamide-2-methyl propane sulfonic 10g and process water 125g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 3.6g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 24g vinylformic acid, 3g ferrous ammonium sulphate, 1.5gN, N'-methylene-bisacrylamide, the mixing solutions of 1.6g methylpropene sodium sulfonate and 160g process water composition, within 3 hours, drip and finish, then insulation 1 hour is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-4, adding tap water adjustment solids content is 40%, for subsequent use.
Embodiment 5
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 6mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 4000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.2:1.
Second step, synthesis: drop into methyl allyl alcohol polyoxyethylene ether (molecular weight 2400) 198g in the reactor being furnished with thermometer and electric stirring, maleic anhydride 24g, AMPS4g and process water 118g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 2.5g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 8g vinylformic acid, 2.2g ferrous ammonium sulphate, 1.1g N, N'-methylene-bisacrylamide, the mixing solutions of 1.2g MAS and 83g process water composition, within 2.5 hours, drip and finish, then insulation 1.5 hours is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-5, adding tap water adjustment solids content is 40%, for subsequent use.
Embodiment 6
A synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
The preparation of the first step, process water: adding water conditioner acrylic acid-maleic anhydride copolymer (PAA-PMA) in tap water, is 6mg/L to PAA-PMA content, obtains process water, for subsequent use;
The molecular weight of PAA-PMA used is 5000, wherein, and vinylformic acid: the mol ratio of maleic anhydride is 1.3:1.
Second step, synthesis: drop into isopentenol polyoxyethylene ether (molecular weight 2400) 191g in the reactor being furnished with thermometer and electric stirring, maleic anhydride 16g, AMPS4g, MAS0.7g and process water 126g, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by 32wt%NaOH aqueous solution adjusted to ph, add 1.3g31% hydrogen peroxide again, maintain the temperature at 40 DEG C, start that continuous dropping prepares in advance by 15g vinylformic acid, 0.8g ferrous ammonium sulphate, 0.7g N, N'-methylene-bisacrylamide, the mixing solutions of 0.4g thiohydracrylic acid and 92g process water composition, within 3 hours, drip and finish, then insulation 1 hour is continued, be 5-6 by 32wt%NaOH aqueous solution adjusted to ph, obtain polyocarboxy acid type high-thin arch dam water reducer, be designated as X-W-6, adding tap water adjustment solids content is 40%, for subsequent use.
Respectively following test is carried out to the polyocarboxy acid type high-thin arch dam water reducer of above six embodiments synthesis:
Below test and complete according to the regulation of GB/T8077-2000, the public all can consult this standard.
Test 1: product and the current commercially available polycarboxylate water-reducer product (the WLH-031 high performance water reducing agent of polyocarboxy acid that Wuhan Lianhe Petroleum Chemical Co., Ltd. produces) of the inventive method synthesis starch Experimental Comparison only
This test cement used be Yadong P.042.5, cement 300g, water reducer and tap water be 87g altogether, specific experiment result as shown in Table 1:
(volume: the mass ratio referring to admixture used and cement, in table one, experiment is exactly admixture and the 300g cement of 1.2g40% solids content.）
Table one cement paste is tested
As can be seen from the degree of mobilization result of table one, polycarboxylate water-reducer prepared by the inventive method all has the dispersing property to cement excellence, and has stronger hold facility.
Test 2: product and current commercially available poly carboxylic acid product (the WLH-031 high performance water reducing agent of polyocarboxy acid that Wuhan Lianhe Petroleum Chemical Co., Ltd. produces) concrete test of the inventive method synthesis contrast
This experiment cement be Yadong P.042.5, grain fineness number modulus 2.5-2.8, stone 5-25mm continuous grading, flyash is GB II grade, and breeze is S95 level.Fit quality is than being water: cement: sand: stone: flyash: breeze=175:200:762:1052:96:80.
Table two concrete performance experimental result
As can be seen from table two slump and diffusibleness, polycarboxylate water-reducer of the present invention is compared with having longer slump retention ability under low-dosage, water-reducing effect is good, excellent combination property, and product cost is high.
Should be understood that; the foregoing is only preferred embodiment of the present invention; object is clearly to set forth technical scheme of the present invention; be not limited to the scope of request of the present invention protection; to those skilled in the art; can be improved according to above-described embodiment or convert, and all these improve and conversion all should be included in protection scope of the present invention.
Claims (1)
1. a synthetic method for polyocarboxy acid type high-thin arch dam water reducer, its step is as follows:
(1) preparation of water, is processed: in tap water, add water conditioner acrylic acid-maleic anhydride copolymer, be 3-8mg/L to acrylic acid-maleic anhydride copolymer content, obtains process water, for subsequent use;
The molecular weight of described acrylic acid-maleic anhydride copolymer is 2000-5000, vinylformic acid in described acrylic acid-maleic anhydride copolymer: the mol ratio of maleic anhydride is 1.1-1.5:1;
(2), synthesize: bed material is added polymerization reaction kettle, be warming up to 40 DEG C and be stirred to and dissolve completely, be 4 by NaOH aqueous solution adjusted to ph, add proper amount of hydrogen peroxide again, drip the mixing solutions be made up of vinylformic acid, ferrous ammonium sulphate, linking agent, chain-transfer agent and process water prepared in advance, within 2.5-4 hour, drip, dropwise follow-up continuation of insurance temperature 0.5-1.5 hour, being neutralized to pH value with the NaOH aqueous solution is 5-6, obtains product;
Described bed material comprises unsaturated Soxylat A 25-7, maleic anhydride, functional minor comonomer and process water;
In described step (2), the molecular weight of unsaturated Soxylat A 25-7 is at 1000-3000;
In described step (2), unsaturated Soxylat A 25-7 is isopentenol polyoxyethylene ether and/or methacrylic Soxylat A 25-7;
In described step (2), functional minor comonomer is 2-acrylamide-2-methyl propane sulfonic and/or methylpropene sodium sulfonate;
In described step (2), linking agent is N, N'-methylene-bisacrylamide;
In described step (2), chain-transfer agent is thiohydracrylic acid or methylpropene sodium sulfonate;
Described maleic anhydride and acrylic acid molar weight sum are 3.0-5.0 times of unsaturated Soxylat A 25-7,
Wherein the molar weight of maleic anhydride accounts for the 5%-50% of maleic anhydride and vinylformic acid integral molar quantity;
Described functional minor comonomer and unsaturated Soxylat A 25-7 mol ratio 0.05-0.5:1;
Described hydrogen peroxide accounts for the 0.5-3% of all monomer total masses;
The 30%-50% that water accounts for bed material total mass is processed in described bed material;
Ferrous ammonium sulphate in described mixing solutions and described hydrogen peroxide mol ratio 1:2-5, described chain-transfer agent accounts for the 0.1-2% of all monomer total masses, and linking agent accounts for the 0.1-0.5% of all monomer total masses;
Described all monomers comprise unsaturated Soxylat A 25-7, vinylformic acid, maleic anhydride and functional minor comonomer;
The 70-90% that water accounts for mixing solutions total mass is processed in described mixing solutions.
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| CN103553409A (en) * | 2013-11-01 | 2014-02-05 | 长沙加美乐素化工有限公司 | High-performance polycarboxylate superplasticizer synthetized by low temperature method, and preparation method thereof |
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| CN104446093A (en) * | 2014-12-04 | 2015-03-25 | 河北铁园科技发展有限公司 | Polycarboxylate-based water reducing agent with integrated functions of water reduction and slump retaining |
| CN107759743A (en) * | 2016-08-22 | 2018-03-06 | 北京时代思动科技有限公司 | A kind of diminishing collapse protective poly-carboxylic acid water reducing agent and preparation method thereof |
| CN107573466A (en) * | 2017-09-11 | 2018-01-12 | 科之杰新材料集团有限公司 | A kind of preparation method of micro- long-acting slump retaining agent of crosslinking |
| CN109437387A (en) * | 2018-11-28 | 2019-03-08 | 山东大学 | A method of modified polycarboxylic acid salt is decomposed using ultraviolet oxidation |
| CN109705834B (en) * | 2018-12-29 | 2021-09-24 | 山东诺尔生物科技有限公司 | Composition, temperature-resistant salt-resistant fracturing fluid thickening agent prepared from composition and preparation method of thickening agent |
| CN110407506B (en) * | 2019-07-30 | 2022-03-15 | 广东建盛高新材料有限公司 | Synthetic method of polycarboxylic acid type high slump loss resistant water reducer |
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