CN103694420B - A kind of polycarboxylate system's cement grinding aid preparation method - Google Patents
A kind of polycarboxylate system's cement grinding aid preparation method Download PDFInfo
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- CN103694420B CN103694420B CN201310631683.6A CN201310631683A CN103694420B CN 103694420 B CN103694420 B CN 103694420B CN 201310631683 A CN201310631683 A CN 201310631683A CN 103694420 B CN103694420 B CN 103694420B
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Abstract
A kind of polycarboxylate system's cement grinding aid preparation method, relate to a kind of cement grinding aid preparation method, preparation process is as follows: maleic anhydride and polyoxyethylene glycol carry out esterification under the condition of catalyzer; By methacrylic acid and stopper and step a) products therefrom Hybrid Heating under the effect of initiator, carry out polyreaction; With sodium hydroxide, solution alkaline is titrated to polymerisate and obtains final product; Wherein: catalyzer is tosic acid, its consumption is 5.5% of monomer total mass; The mol ratio of maleic anhydride and polyoxyethylene glycol is 1:1; Initiator is benzoyl peroxide, and its consumption is 0.8% of monomer total mass; Product of the present invention has obvious grinding-aid effect, and can significantly improve grinding machine abrasive dust effect, its processing method is special, and raw material is simple, has good adaptability with other additives, has good water-reducing effect in later stage concrete preparation.
Description
Technical field
The present invention relates to a kind of cement grinding aid preparation method, particularly relate to a kind of polycarboxylate system's cement grinding aid preparation method.
Background technology
In cement production process, power consumption for grinding is very high, data is had to show, the utilization ratio of cement grinding stage energy is extremely low, have the power loss of 95% ~ 99%, the method also do not settled the matter once and for all both at home and abroad. therefore the application of grinding aid become during current Cement industry is produced be used for improving mill efficiency, improve cement performance, save energy and reduce the cost, one of the Main Means that reduces costs.Grinding aid market is huge, various in style, in addition a lot of detour has been walked in the development of China's grinding aid, there is many problems, most of cement production enterprise is hung back to it, form resentment, be unfavorable for popularization and the use of grinding aid. commercially available grinding aid mainly adopts that organic and inorganic material is composite to be formed, and is not the product of proper organic synthesis. the main drawback of its product is that poor stability, cost are higher. therefore, to the further investigation of cement grinding aid and apply imperative.
Summary of the invention
The object of the present invention is to provide a kind of polycarboxylate system's cement grinding aid preparation method, the method carries out esterification by maleic anhydride and polyoxyethylene glycol under the effect of catalyzer, then under the effect of initiator, methacrylic acid is added and stopper carries out polyreaction, obtain target product, grinding machine abrasive dust effect can be significantly improved, have good water-reducing effect in later stage concrete preparation.
The object of the invention is to be achieved through the following technical solutions:
A kind of polycarboxylate system's cement grinding aid preparation method, it is as follows that described method comprises preparation process:
A) maleic anhydride and polyoxyethylene glycol carry out esterification under the condition of catalyzer;
B) under the effect of initiator by methacrylic acid and stopper and step a) products therefrom Hybrid Heating, carry out polyreaction;
C) with sodium hydroxide, solution alkaline is titrated to polymerisate and obtains final product;
Wherein: catalyzer is tosic acid, its consumption is 5.5% of monomer total mass; The mol ratio of maleic anhydride and polyoxyethylene glycol is 1:1; Initiator is benzoyl peroxide, and its consumption is 0.8% of monomer total mass;
Described a kind of polycarboxylate system's cement grinding aid preparation method, drips sodium hydroxide solution in described step c), forms polycarboxylate.
Described a kind of polycarboxylate system's cement grinding aid preparation method, in described step a), esterification temperature is 90 DEG C, and in step b), polymerization temperature is 80 DEG C.
Described a kind of polycarboxylate system's cement grinding aid preparation method, in described step a), esterification time is 3h, and in step b), polymerization time is 3.5h.
Accompanying drawing explanation
Fig. 1 is present invention process schematic diagram.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
The present invention carries out esterification by maleic anhydride and polyoxyethylene glycol under the effect of catalyzer, then under the effect of initiator, add methacrylic acid and stopper carries out polyreaction, after being finally titrated to alkalescence with sodium hydroxide solution, obtain target product---methacrylic acid-toxilic acid polyglycol ester interpolymer (grinding aid).
Maleic anhydride and polyoxyethylene glycol 1:1 join in there-necked flask by the present invention, and add toluene and make solvent, heating in water bath is to reactants dissolved, when temperature rises to 80 DEG C, add the tosic acid of 5.5%, reaction to theoretical aquifer yield or aquifer yield invariable, stopped reaction.Methacrylic acid and 2.0% stopper are added reaction product in (1), during heating in water bath to 80 DEG C, add the initiator benzoyl peroxide of 0.8%; Reaction 3h.Heating steams solvent, recycles.Drop to alkalescence with sodium hydroxide solution, after oven dry, obtain product.
Embodiment 1:
Add 5.39g maleic anhydride in reactor, then add 20g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 110 DEG C, reacts 5 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 80 DEG C, reacts 4 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Embodiment 2:
Add 5.39g maleic anhydride in reactor, then add 20g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 100 DEG C, reacts 5 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 80 DEG C, reacts 4 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Embodiment 3:
Add 5.39g maleic anhydride in reactor, then add 20g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 110 DEG C, reacts 4 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 80 DEG C, reacts 4 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Embodiment 4
Add 5.39g maleic anhydride in reactor, then add 20g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 110 DEG C, reacts 5 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 90 DEG C, reacts 4 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Embodiment 5:
Add 5.39g maleic anhydride in reactor, then add 20g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 110 DEG C, reacts 5 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 80 DEG C, reacts 5 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Embodiment 6:
Add 5.39g maleic anhydride in reactor, then add 30g polyoxyethylene glycol, it is some to add catalyzer; Stirring is warming up to 110 DEG C, reacts 5 hours; Add methacrylic acid 8.61g after cooling, it is some to add initiator; Stirring is warming up to 80 DEG C, reacts 4 hours; Then regulate PH to neutral with sodium hydroxide solution, both obtain cement grinding aid.
Grinding-aid effect contrast experiment:
When using the cement grinding process condition raw material types of production 32.5 grade and proportioning to be consistent, add cement grinding aid of the present invention prepared by trolamine, toxilic acid triethanolamine salt and above-described embodiment 1-6 respectively, abrasive dust test result is as shown in the table together with grog gypsum and blended material:
As can be seen from the above table, grinding aid of the present invention is more better than the net effect entering trolamine, toxilic acid triethanolamine salt, and when add-on accounts for 0,02% of total amount, net effect is best.Grinding aid of the present invention also has advantage very much in cost.
Claims (1)
1. polycarboxylate system's cement grinding aid preparation method, is characterized in that, it is as follows that described method comprises preparation process:
A) maleic anhydride and polyoxyethylene glycol carry out esterification under the condition of catalyzer;
B) under the effect of initiator by methacrylic acid and stopper and step a) products therefrom Hybrid Heating, carry out polyreaction;
C) with sodium hydroxide, solution alkaline is titrated to polymerisate and obtains final product;
Wherein: catalyzer is tosic acid, its consumption is 5.5% of monomer total mass; The mol ratio of maleic anhydride and polyoxyethylene glycol is 1:1; Initiator is benzoyl peroxide, and its consumption is 0.8% of monomer total mass;
Drip sodium hydroxide solution in described step c), form polycarboxylate;
In described step a), esterification temperature is 90 DEG C, and in step b), polymerization temperature is 80 DEG C;
In described step a), esterification time is 3h, and in step b), polymerization time is 3.5h.
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| CN201310631683.6A CN103694420B (en) | 2013-12-02 | 2013-12-02 | A kind of polycarboxylate system's cement grinding aid preparation method |
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| CN201310631683.6A CN103694420B (en) | 2013-12-02 | 2013-12-02 | A kind of polycarboxylate system's cement grinding aid preparation method |
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| CN103694420A CN103694420A (en) | 2014-04-02 |
| CN103694420B true CN103694420B (en) | 2016-02-24 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525403A (en) * | 2009-03-26 | 2009-09-09 | 山东宏艺科技有限公司 | Method for synthesizing cement grinding reinforcing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525403A (en) * | 2009-03-26 | 2009-09-09 | 山东宏艺科技有限公司 | Method for synthesizing cement grinding reinforcing agent |
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Effective date of registration: 20190603 Address after: 226200 Linhai Bridge, Qidong and Hezhen, Nantong City, Jiangsu Province Patentee after: Qidong Xishi Cement Co.,Ltd. Address before: No. 11, economic and Technological Development Zone, Shenyang, Liaoning Province, Liaoning Patentee before: Shenyang University of Chemical Technology |
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Effective date of registration: 20210914 Address after: 226200 group 1, hehe village, Yinyang Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Yincheng Equipment Technology Co., Ltd Address before: 226200 Linhai Bridge, Qidong and Hezhen, Nantong City, Jiangsu Province Patentee before: Qidong Xishi Cement Co.,Ltd. |
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