CN101671142B - Cement reinforced grinding aid prepared with hydrolyzed polymaleic acid - Google Patents
Cement reinforced grinding aid prepared with hydrolyzed polymaleic acid Download PDFInfo
- Publication number
- CN101671142B CN101671142B CN200910172396A CN200910172396A CN101671142B CN 101671142 B CN101671142 B CN 101671142B CN 200910172396 A CN200910172396 A CN 200910172396A CN 200910172396 A CN200910172396 A CN 200910172396A CN 101671142 B CN101671142 B CN 101671142B
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- CN
- China
- Prior art keywords
- polymaleic acid
- grinding aid
- cement reinforced
- reaction
- monomethyl ether
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000227 grinding Methods 0.000 title claims abstract description 34
- 239000004568 cement Substances 0.000 title claims abstract description 31
- 229920001444 polymaleic acid Polymers 0.000 title claims abstract description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 51
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 15
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 18
- 229920000151 polyglycol Polymers 0.000 claims description 18
- 239000010695 polyglycol Substances 0.000 claims description 18
- CUTSCJHLMGPBEJ-UHFFFAOYSA-N [N].CN(C)C=O Chemical compound [N].CN(C)C=O CUTSCJHLMGPBEJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 39
- 238000006243 chemical reaction Methods 0.000 abstract description 26
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 150000007530 organic bases Chemical class 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 abstract 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000002650 habitual effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
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- Polyethers (AREA)
Abstract
The invention relates to a cement reinforced grinding aid prepared with polymaleic acid. The preparation method of the grinding aid comprises the following steps: placing hydrolyzed polymaleic acid, methoxy polyethylene glycol, N,N-dimethylformamide and sodium sulphate in a container according to a defined proportion to fully mix and dissolve, then adding catalyst triethylamine, heating at the temperature of 85+/-5DEG C to react for 3-5 hours and obtaining the cement reinforced grinding aid. The invention adopting organic base triethylamine as a catalyst has the advantages of mild reaction conditions and low requirement on devices, wherein the reaction temperature is not more than 90 DEG C. Meanwhile, polymerization inhibitor is not needed to be added during the reaction and the reaction product is not needed to be purified. The process is relatively simple and the reaction time is short.
Description
(1) technical field
The present invention relates to a kind of cement reinforced grinding aid, particularly use the cement grinding aid of polymaleic acid as feedstock production.
(2) background technology
Grinding aid uses in the cement production enterprise grinding operation, is one and helps saving energy and reduce the cost, reducing discharging sharp useless measure.In cement in China industry, grinding pow consumption is higher, and the most of areas power supply shortage, therefore must pay attention to the exploitation and the application of grinding aid, and the application of grinding aid can be promoted as an effective energy-saving measure.Using more grinding aid in China is thanomin and one type of chemical substance of polyvalent alcohol.Habitual grinding aid such as trolamine etc. though the grinding of cement is had good grinding-aid effect, because of costing an arm and a leg, make the cost of cement per ton increase much during use, not having economic benefit can say.And the source shortage, so be difficult to apply.
(3) summary of the invention
The objective of the invention is with polymaleic acid etc. as raw material, the exploitation synthesis condition is gentle, and equipment requirements is low, the simple a kind of cement reinforced grinding aid of technology.
The concrete technical scheme of the present invention is following: polymaleic acid, poly glycol monomethyl ether, nitrogen dimethylformamide (DMF) are placed fully stirring and dissolving of container in proportion with sodium sulfate; Add catalyst of triethylamine then; Reacting by heating is 3～5 hours under 85 ± 5 ℃ of temperature, has both got cement reinforced grinding aid;
More than the mass ratio of various raw materials be: polymaleic acid: poly glycol monomethyl ether=1: 0.5～0.8; Polymaleic acid: nitrogen dimethylformamide (DMF)=1: 0.3～0.5; Polymaleic acid: sodium sulfate=1: 0.04～0.06; The catalyst of triethylamine consumption is 3%～5% of polymaleic acid and a poly glycol monomethyl ether total amount.
The molecular-weight average of described polymaleic acid is 800, and the poly glycol monomethyl ether molecular-weight average is 1000 or 2000.
Advantage of the present invention:
1. reaction conditions is gentle, uses the organic bases triethylamine to make catalyzer, and low for equipment requirements, temperature of reaction is no more than 90 ℃.
2. need not add stopper in the reaction, reaction product does not need to purify.
3. technology is relatively simple and the reaction times is short.
(4) embodiment
Embodiment 1: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 4.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 2: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 2000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 4.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 3: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 80.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 6.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 4: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 2000 poly glycol monomethyl ether 80.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 6.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 5: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 50.0g, sodium sulfate 4.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 6: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 2000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 50.0g, sodium sulfate 6.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 7: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 4.0g adds reaction vessel, and the back that stirs adds the 7.5g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 8: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 2000 poly glycol monomethyl ether 80.0g; Nitrogen dimethylformamide (DMF) 30.0g, sodium sulfate 6.0g adds reaction vessel, and the back that stirs adds the 9.0g triethylamine; Add reaction 3 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 9: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 50.0g; Nitrogen dimethylformamide (DMF) 50.0g, sodium sulfate 4.0g adds reaction vessel, and the back that stirs adds the 4.5g triethylamine; Add reaction 5 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 10: be 800 polymaleic acid 100.0g with molecular weight; Molecular-weight average is 1000 poly glycol monomethyl ether 80.0g; Nitrogen dimethylformamide (DMF) 50.0g, sodium sulfate 6.0g adds reaction vessel, and the back that stirs adds the 9.0g triethylamine; Add reaction 5 hours at 85 ± 5 ℃, both got cement reinforced grinding aid after the cooling.
Embodiment 11: embodiment 1 to embodiment 10 prepared cement reinforced grinding aids, press 2/10000ths of cement clinker and blended material weight and adds in the test mills and ground 21 minutes, and measurement fineness, specific surface area, 3 days and 28 days intensity, the result is as shown in the table.Cement clinker and blended material proportioning are: rotary kiln cement clinker: 65wt%; Slag: 15wt%; Flyash: 10wt%; Wingdale: 6wt%; Gypsum: 4wt%.The sample of admixture grinding aid is not as blank.
2 synthetic products of the embodiment of the invention are tested in certain cement mill, and the result shows that the adding of this grinding aid can reduce cement clinker consumption 8%, when improving the grinding machine platform more than 15%.
Claims (2)
1. cement reinforced grinding aid with polymaleic acid preparation; It is characterized in that polymaleic acid, poly glycol monomethyl ether, nitrogen dimethylformamide and sodium sulfate abundant stirring and dissolving in container in proportion; Add catalyst of triethylamine then; Reacting by heating is 3～5 hours under 85 ± 5 ℃ of temperature, has both got cement reinforced grinding aid;
More than the mass ratio of various raw materials be: polymaleic acid: poly glycol monomethyl ether=1: 0.5～0.8; Polymaleic acid: nitrogen dimethylformamide DMF=1: 0.3～0.5; Polymaleic acid: sodium sulfate=1: 0.04～0.06;
The catalyst of triethylamine consumption is 3%～5% of polymaleic acid and a poly glycol monomethyl ether total amount.
2. the cement reinforced grinding aid with the polymaleic acid preparation according to claim 1, the molecular-weight average that it is characterized in that used polymaleic acid is 800, the molecular-weight average of poly glycol monomethyl ether is 1000 or 2000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910172396A CN101671142B (en) | 2009-10-13 | 2009-10-13 | Cement reinforced grinding aid prepared with hydrolyzed polymaleic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910172396A CN101671142B (en) | 2009-10-13 | 2009-10-13 | Cement reinforced grinding aid prepared with hydrolyzed polymaleic acid |
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| Publication Number | Publication Date |
|---|---|
| CN101671142A CN101671142A (en) | 2010-03-17 |
| CN101671142B true CN101671142B (en) | 2012-09-26 |
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| CN200910172396A Expired - Fee Related CN101671142B (en) | 2009-10-13 | 2009-10-13 | Cement reinforced grinding aid prepared with hydrolyzed polymaleic acid |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199016A (en) * | 2010-10-15 | 2011-09-28 | 河南理工大学 | Cement containing early strength agent |
| CN102199015A (en) * | 2010-10-15 | 2011-09-28 | 河南理工大学 | Cement containing polycarboxylic acid water reducing agent |
| CN103387351A (en) * | 2012-05-11 | 2013-11-13 | 天津博克尼科技发展有限公司 | Compound liquid cement grinding aid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6849703B2 (en) * | 2001-05-22 | 2005-02-01 | Basf Aktiengesellschaft | Water-soluble polymers of esters made from acrylic acid and alkylpolyalkylene glycols |
| CN101182149A (en) * | 2007-11-19 | 2008-05-21 | 李军 | Composite activated cement reinforced grinding aids containing polycarboxylic acid series and method for preparing the same |
| 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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2009
- 2009-10-13 CN CN200910172396A patent/CN101671142B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6849703B2 (en) * | 2001-05-22 | 2005-02-01 | Basf Aktiengesellschaft | Water-soluble polymers of esters made from acrylic acid and alkylpolyalkylene glycols |
| CN101182149A (en) * | 2007-11-19 | 2008-05-21 | 李军 | Composite activated cement reinforced grinding aids containing polycarboxylic acid series and method for preparing the same |
| 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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| CN101671142A (en) | 2010-03-17 |
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| CB03 | Change of inventor or designer information |
Inventor after: Qian Changchun Inventor after: Wang Jigang Inventor after: Guan Xin Inventor after: Zhao Songhai Inventor after: Shang Haitao Inventor after: Wang Wenzhan Inventor after: Zhang Dongdong Inventor after: Li Haikang Inventor before: Wang Tao Inventor before: Zhang Haibo |
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Effective date of registration: 20160628 Address after: 454950 former Liu Zhuang, Sanyang Township, Wuzhi County, Jiaozuo, Henan Patentee after: JIAOZUO QIANGNAI BUILDING MATERIALS CO., LTD. Address before: 454851, No. four, Lane 2, Minsheng Road, Wenquan Town, Henan, Wenxian County Patentee before: Wang Tao Patentee before: Zhang Haibo |
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Address after: 454950 former Liu Zhuang, Sanyang Township, Wuzhi County, Jiaozuo, Henan Patentee after: Henan strong new material Limited by Share Ltd Address before: 454950 former Liu Zhuang, Sanyang Township, Wuzhi County, Jiaozuo, Henan Patentee before: JIAOZUO QIANGNAI BUILDING MATERIALS CO., LTD. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120926 Termination date: 20201013 |