CN103030817A - Modified sodium lignosulfonate and application thereof as cement grinding aid - Google Patents
Modified sodium lignosulfonate and application thereof as cement grinding aid Download PDFInfo
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- CN103030817A CN103030817A CN201310013199.7A CN201310013199A CN103030817A CN 103030817 A CN103030817 A CN 103030817A CN 201310013199 A CN201310013199 A CN 201310013199A CN 103030817 A CN103030817 A CN 103030817A
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- sodium lignosulfonate
- modified sodium
- cement
- grinding aid
- cement grinding
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- 239000004568 cement Substances 0.000 title claims abstract description 35
- 238000000227 grinding Methods 0.000 title claims abstract description 32
- 229920005552 sodium lignosulfonate Polymers 0.000 title claims abstract description 23
- 150000003385 sodium Chemical class 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000000855 fermentation Methods 0.000 claims description 5
- 230000004151 fermentation Effects 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 4
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000008098 formaldehyde solution Substances 0.000 claims description 2
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000006277 sulfonation reaction Methods 0.000 abstract description 2
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 229920001732 Lignosulfonate Polymers 0.000 description 9
- 235000019357 lignosulphonate Nutrition 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 240000008042 Zea mays Species 0.000 description 3
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 235000009973 maize Nutrition 0.000 description 3
- 239000010902 straw Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241000158728 Meliaceae Species 0.000 description 1
- 241000775848 Syringa oblata Species 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- PCHPORCSPXIHLZ-UHFFFAOYSA-N diphenhydramine hydrochloride Chemical class [Cl-].C=1C=CC=CC=1C(OCC[NH+](C)C)C1=CC=CC=C1 PCHPORCSPXIHLZ-UHFFFAOYSA-N 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000002921 fermentation waste Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Abstract
Aiming at the defects of the existing sodium lignosulfonate and a synthesis method thereof as a cement grinding aid in the prior art, the invention provides a novel preparation method of modified sodium lignosulfonate, and finds good application effect in the cement grinding aid. The method takes cellulosic ethanol waste residue as a raw material, and modified sodium lignosulfonate is obtained through reactions such as dissolution, sulfonation reaction, modification and the like. The modified sodium lignosulfonate obtained by the invention has a good grinding-aiding function on cement at a low addition amount. The product of the invention originally takes the waste cellulosic ethanol residues as the raw material, solves the problem of residue pollution, has simple and feasible production process, and has better grinding-aiding effect than the prior art when being used as a cement auxiliary agent.
Description
Technical field
Modified sodium lignosulfonate and as the application of cement grinding aid.
Background technology
Cement grinding aid is the general name of adding chemical agent in the cement grog grinding process in the system.They mainly are comprised of some tensio-active agents; in the material grinding process; cement grinding aid is adsorbed in solid particles surface; weaken the solid surface electrostatic repulsion; reduce solid grinding surface energy; weaken the trend that fine particle gathers, thereby reach the effect that improves mill efficiency, increase unit-hour output, reduces grinding pow consumption.Cement grinding aid has good dispersed composition, can be adsorbed on the material surface, reduce intergranular frictional force and adhesive power, increase the flowability of material, the electrostatic coagulation power that produces in the shielding grinding process, reduce between particle, the mutual gathering between particle and grinding element, elimination bag ball, bag are forged phenomenon effectively, improve mill efficiency, make 3 ~ 32 μ m granule contents increase in the cement, optimize the cement granules grating, be conducive to the raising of strength of cement.Along with the increasing of cement total demand, the application of cement grinding aid is more and more extensive.At present, the application of hydramine series cement grinding aid is comparatively extensive, and application performance also generally obtains the market approval, but because these series product come from fossil feedstock, cost is more and more higher along with the rise of crude oil price.In order to reduce the cost of cement grinding aid, lignin derivative is used for the prescription of liquid cement grinding additive in a large number in recent years, use at present more lignin derivative and be mainly sulfonated lignin, it comes from the lignin sulfonate that the acid system papermaking wastewater extracts, comprise sodium, calcium, magnesium and ammonium salt etc., have the source complexity, sulfonic group content is lower, relative molecular mass (being called for short molecular weight, lower same) the wide characteristics of distribution range.Because sulfonated lignin are lower in the adsorptive power of cement surface, and because range of molecular weight distributions is wide, the molecule utilising efficiency of sulfonated lignin is lower, absorption fraction of coverage at cement particle surface is also lower, therefore, these shortcomings of sulfonated lignin cause its grinding aid poor-performing in cement grinding, have also caused it to be difficult to apply as a kind of high performance cement grinding aid.
The present invention is directed to the general relatively poor present situation of application performance of present lignin-base cement grinding aid, xylogen is as main raw material in the cellulosic ethanol waste residue, improving its grinding aid to cement clinker and mixing material by chemical modification strengthens the property, show with the performance comparison result of trolamine, sulfonated lignin cement grinding aid after the modification belongs to a kind of high-efficiency concrete grinding aid, and this will provide technical support for the widespread use of lignin-base cement grinding aid.
Summary of the invention
One of content of the present invention provides a kind of method of producing modified sodium lignosulfonate, and the method is utilized maize straw to steam quick-fried rear enzymatic hydrolysis and fermentation cellulosic ethanol waste residue processed to be raw material, to make through following reactions steps:
(1) collect 100 parts of cellulosic ethanol slag qualities and add entry and mix, control solid content is 30-75%, adds the sodium hydroxide solution of 10%-20%, and in the 60-90 ℃ of lower 0.2-1h that stirs, filtration obtains filtrate;
(2) in filtrate, add the anhydrous sodium sulphate of 1-10 part and 0.1-1 part iron trichloride, will react pH regulator to 10-11, in 80-90 ℃ of lower reaction 4-5h, obtain reaction solution 1;
(3) reaction solution 1 is cooled to 25-45 ℃, control pH is 10-11, at the uniform velocity adds 5-10 part formaldehyde solution in reaction solution, reacts 1-2 hour, is cooled to room temperature and obtains product stoste.
The method of production modified sodium lignosulfonate of the present invention, pH regulator agents useful for same are sodium hydroxide or sulfuric acid.
Two of content of the present invention provides according to the described method production of invention and obtains the modified sodium lignosulfonate product.
Three of content of the present invention is product application in cement grinding aid.
Beneficial effect of the present invention is:
(1) provide a kind of novel method for preparing modified sodium lignosulfonate, with respect to traditional preparation technology, the method is simple and easy to operate, and is with low cost.
(2) provide a kind of modified sodium lignosulfonate product.
(3) application of this modified sodium lignosulfonate in cement grinding aid has good effect.
(4) this invention raw material uses the alcohol fuel fermentation residue, efficiently solves the residue contamination problem of fuel ethanol production producer, has reduced environmental pollution, has increased income.
Description of drawings
Fig. 1. the modified sodium lignosulfonate infrared spectrogram.
Embodiment
Embodiment 1
The structure difference of present embodiment explanation modified sodium lignosulfonate and Traditional Wood quality sodium sulfonate.Fig. 1 example the infrared spectrogram of modified lignin mahogany sulfonate product.
The modified product sulfonated lignin are at 1598 cm
-1, 1514 cm
-1All there is typical aromatic nucleus vibration absorption peak; At 1457cm
-1Asymmetric C-O key distortion appears; At 3342 cm
-1The flexible absorption peak of O-H occurs, these typical absorption peaks show that modified product still has the structure construction of xylogen.By Figure 10 also as can be known, modified product is at 1370 cm
-1Syringa oblata Lindl. base absorption peak has appearred, modification is described after Syringa oblata Lindl. base content increased.1042 cm
-1The place is sulfonic stretching vibration peak, 531 cm
-1The place be sulfonated lignin at the characteristic peak of infrared spectra fingerprint region, sulfonated lignin have absorption peak herein, xylogen are described after sulfonation reaction, methoxy content reduces in the molecule, and has introduced sulfonic acid group.
Concrete synthetic method and the method for modifying of present embodiment explanation sodium lignosulfonate.The method is utilized maize straw to steam quick-fried rear enzymatic hydrolysis and fermentation cellulosic ethanol waste residue processed to be raw material, to make through following reactions steps:
(1) collect 100 parts of cellulosic ethanol slag qualities and add entry and mix, the control solid content is 30%, adds 10% sodium hydroxide solution, stirs 0.2h in 60 times, filters and obtains filtrate;
(2) in filtrate, add 1 part anhydrous sodium sulphate and 0.1 part iron trichloride, will react pH regulator to 10 with sodium hydroxide solution, in 80 ℃ of lower reaction 4h, obtain reaction solution 1;
(3) reaction solution 1 is cooled to 25 ℃, control pH is 10, at the uniform velocity adds 5 parts of formaldehyde solutions in reaction solution, reacts 1 hour, is cooled to room temperature and obtains product stoste.
Embodiment 3
Another synthetic method and the method for modifying of present embodiment explanation sodium lignosulfonate.One of content of the present invention provides a kind of method of producing modified sodium lignosulfonate, and the method is utilized maize straw to steam quick-fried rear enzymatic hydrolysis and fermentation cellulosic ethanol waste residue processed to be raw material, to make through following reactions steps:
(1) collect 100 parts of cellulosic ethanol slag qualities and add entry and mix, the control solid content is 75%, adds 20% sodium hydroxide solution, in 90 ℃ of lower 1h that stir, filters and obtains filtrate;
(2) in filtrate, add 10 parts anhydrous sodium sulphate and 1 part iron trichloride, will react pH regulator to 11, in 90 ℃ of lower reaction 5h, obtain reaction solution 1;
(3) reaction solution 1 is cooled to 45 ℃, control pH is 11, at the uniform velocity adds 10 parts of formaldehyde solutions in reaction solution, reacts 2 hours, is cooled to room temperature and obtains product stoste.
Embodiment 4
The application of present embodiment explanation modified sodium lignosulfonate in cement grinding aid.After the cement grinding aid that utilizes the cellulose alcoholic fermentation waste residue to carry out making after the modification was applied in the slag cement, product is had certain diminishing and delayed coagulation; Cement 3 days and 28 days folding strengths slightly are improved.The ultimate compression strength of its 3 days and 28 days obviously improves when pH=7, and its physicals assay is such as table 3-5, and the xylogen of modification represents with code name PH.
Table 1 cement grinding aid physicals survey report
Claims (5)
1. a method of producing modified sodium lignosulfonate is characterized in that utilizing xylogen to be raw material, makes through following reactions steps:
(1) collect 100 parts of xylogen quality and add entry and mix, control solid content is 30-75%, adds the sodium hydroxide solution of 10%-20%, and in the 60-90 ℃ of lower 0.2-1h that stirs, filtration obtains filtrate;
(2) in filtrate, add the anhydrous sodium sulphate of 1-10 part and 0.1-1 part iron trichloride, will react pH regulator to 10-11, in 80-90 ℃ of lower reaction 4-5h, obtain reaction solution 1;
(3) reaction solution 1 is cooled to 25-45 ℃, control pH is 10-11, at the uniform velocity adds 5-10 part formaldehyde solution in reaction solution, reacts 1-2 hour, is cooled to room temperature and obtains product stoste.
2. the method for production modified sodium lignosulfonate according to claim 1 is characterized in that described xylogen raw material is the waste residue that stalk steams quick-fried rear enzymatic hydrolysis and fermentation cellulosic ethanol processed.
3. the method for production modified sodium lignosulfonate according to claim 1, the pH regulator agents useful for same is sodium hydroxide or sulfuric acid.
4. described method is produced resulting modified sodium lignosulfonate product according to claim 1-2.
5. the application of product according to claim 3 in cement grinding aid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310013199.7A CN103030817A (en) | 2013-01-15 | 2013-01-15 | Modified sodium lignosulfonate and application thereof as cement grinding aid |
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| CN201310013199.7A CN103030817A (en) | 2013-01-15 | 2013-01-15 | Modified sodium lignosulfonate and application thereof as cement grinding aid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497342A (en) * | 2013-09-27 | 2014-01-08 | 山东龙力生物科技股份有限公司 | Method for producing enzymatic hydrolysis lignin sulfonate |
| CN104844051A (en) * | 2015-04-01 | 2015-08-19 | 淮安市楚城水泥有限公司 | Cement grinding aid and preparation method therefor |
| CN105837078A (en) * | 2016-04-18 | 2016-08-10 | 南京工业大学 | Composite cement grinding aid and preparation method and application thereof |
| CN106242340A (en) * | 2016-08-16 | 2016-12-21 | 仇颖莹 | A kind of preparation method of multicomponent biological matter cement grinding aid |
| CN107446218A (en) * | 2017-09-25 | 2017-12-08 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of maleylation sodium lignin sulfonate filled plastics composite |
| CN107501691A (en) * | 2017-09-25 | 2017-12-22 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of sodium lignin sulfonate filled plastics composite |
| CN109777353A (en) * | 2019-03-22 | 2019-05-21 | 泉州欧米克生态建材科技有限公司 | A kind of clay grinding aid and preparation method thereof |
| CN110982089A (en) * | 2019-11-25 | 2020-04-10 | 南京工业大学 | Dark lignin and application thereof in inner paper of outer bag of fruit cultivation sleeve |
| CN112479622A (en) * | 2020-11-06 | 2021-03-12 | 霸州市砚创科技有限公司 | Method for preparing cement by using low-grade limestone |
-
2013
- 2013-01-15 CN CN201310013199.7A patent/CN103030817A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497342A (en) * | 2013-09-27 | 2014-01-08 | 山东龙力生物科技股份有限公司 | Method for producing enzymatic hydrolysis lignin sulfonate |
| CN103497342B (en) * | 2013-09-27 | 2015-11-11 | 山东龙力生物科技股份有限公司 | A kind of method of producing enzymolysis xylogen sulfonate |
| CN104844051A (en) * | 2015-04-01 | 2015-08-19 | 淮安市楚城水泥有限公司 | Cement grinding aid and preparation method therefor |
| CN105837078A (en) * | 2016-04-18 | 2016-08-10 | 南京工业大学 | Composite cement grinding aid and preparation method and application thereof |
| CN106242340A (en) * | 2016-08-16 | 2016-12-21 | 仇颖莹 | A kind of preparation method of multicomponent biological matter cement grinding aid |
| CN107446218A (en) * | 2017-09-25 | 2017-12-08 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of maleylation sodium lignin sulfonate filled plastics composite |
| CN107501691A (en) * | 2017-09-25 | 2017-12-22 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of sodium lignin sulfonate filled plastics composite |
| CN109777353A (en) * | 2019-03-22 | 2019-05-21 | 泉州欧米克生态建材科技有限公司 | A kind of clay grinding aid and preparation method thereof |
| CN110982089A (en) * | 2019-11-25 | 2020-04-10 | 南京工业大学 | Dark lignin and application thereof in inner paper of outer bag of fruit cultivation sleeve |
| CN110982089B (en) * | 2019-11-25 | 2020-11-03 | 南京工业大学 | Dark lignin and application thereof in inner paper of outer bag of fruit cultivation sleeve |
| CN112479622A (en) * | 2020-11-06 | 2021-03-12 | 霸州市砚创科技有限公司 | Method for preparing cement by using low-grade limestone |
| CN112479622B (en) * | 2020-11-06 | 2022-06-21 | 霸州市砚创科技有限公司 | Method for preparing cement by using low-grade limestone |
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Application publication date: 20130410 |