CN103964735B - The preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer - Google Patents
The preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer Download PDFInfo
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- CN103964735B CN103964735B CN201410183717.4A CN201410183717A CN103964735B CN 103964735 B CN103964735 B CN 103964735B CN 201410183717 A CN201410183717 A CN 201410183717A CN 103964735 B CN103964735 B CN 103964735B
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- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 37
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 101100476962 Drosophila melanogaster Sirup gene Proteins 0.000 claims abstract description 24
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims abstract description 24
- 235000020357 syrup Nutrition 0.000 claims abstract description 24
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- 239000012986 chain transfer agent Substances 0.000 claims abstract description 10
- QVDTXNVYSHVCGW-ONEGZZNKSA-N isopentenol Chemical compound CC(C)\C=C\O QVDTXNVYSHVCGW-ONEGZZNKSA-N 0.000 claims abstract description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 9
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 230000002829 reductive effect Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000012452 mother liquor Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004160 Ammonium persulphate Substances 0.000 claims description 2
- 108010058643 Fungal Proteins Proteins 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 2
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
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- 239000003607 modifier Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000006835 compression Effects 0.000 abstract description 2
- 238000007906 compression Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000004568 cement Substances 0.000 description 13
- 239000002351 wastewater Substances 0.000 description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- CZMRCDWAGMRECN-UHFFFAOYSA-N Rohrzucker Natural products OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 238000005485 electric heating Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
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- 229930091371 Fructose Natural products 0.000 description 2
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- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 2
- 230000000740 bleeding effect Effects 0.000 description 2
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- DSLZVSRJTYRBFB-LLEIAEIESA-N D-glucaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O DSLZVSRJTYRBFB-LLEIAEIESA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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- 239000002956 ash Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
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- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
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- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer.Under 30 DEG C ~ 60 DEG C conditions, vinylformic acid, initiator, reductive agent, chain-transfer agent and beet sirup yeast waste liquor properties-correcting agent are slowly dropped in isopentenol polyoxyethylene ether solution, dropping controls to complete at 3h ~ 5h, temperature remains unchanged slaking 1h ~ 3h, after being cooled to room temperature, obtain beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer.The inventive method is simple, reaction conditions is easy to control, reaction times is short, and by yeast waste liquor reluctant in industry and beet sirup with the use of, for water reducer provides slow setting component, in addition, because calcification molasses are alkalescence, do not need post-synthesis phase to add sheet alkali again to regulate the pH of water reducer, reduce synthesis cost.The concrete of the beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer preparation adopting the present invention to obtain, can effectively reduce initial stage hydration heat, and improves concrete 28d ultimate compression strength and obtain.
Description
Technical field
The present invention relates to the preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, belong to concrete admixture field.
Background technology
Molasses are as the important byproduct of sugar refinery, and solid concentration is up to 70% ~ 90%, and its main component is sucrose, glucose and fructose.Molasses may be used for the raw material such as alcohol, fermentation mother, soy sauce, monosodium glutamate, but molasses are used for fermentation industry causes by product waste water and yeast waste liquor can pollute soil, water source etc., and therefore Appropriate application waste molasses and yeast waste liquor have very important significance.
Carbohydrate in molasses has the effect necessarily delaying aquation.The molasses such as lime saccharate, calisanin and the fructose calcium that are obtained through simple modification by molasses are a kind of hydrophilic surfactant's things; after sugar calcium is adsorbed onto cement particle surface; cement granules is mutually exclusive; can not mutually be agglomerated into comparatively macroparticle; delay cement hydration process, made concrete improve plasticity-and extend time of coagulation.Therefore, molasses can join in polycarboxylate water-reducer as slow setting component.And vitriol is main component in yeast wastewater, also containing have an appointment 0.5% dry-matter, main component is the residual sugar be not fully utilized in yeast protein, Mierocrystalline cellulose, colloidalmaterial and waste molasses.Cellulosic component wherein has certain slow setting function, and has certain effect to the segregation of mass concrete and bleeding, also can improve concrete increasing and stick guarantor and mould function.And the sulphate component in yeast waste liquor forms SO owing to can comparatively fast dissolve
4- 2-decrease polycarboxylate water-reducer wrapped up by hydrolysis product of cement and consume, reduce liquid solution surface tension, increase surfactivity, improve micro-air-entraining effect, be conducive to improving polycarboxylate water-reducer dispersing property, improve the mobility of slurry.Therefore molasses all can be used as the admixture in building trade with yeast waste liquor.
Along with the development of social economy's level, mass concrete has been widely used in the structure such as high level and high-rise building, long-span bridge girder construction and Industrial buildings of field of civil engineering.And initial stage hydration heat is too high, concrete segregation all result in the crack problem of mass concrete with bleeding, therefore a kind of polycarboxylate water-reducer that there is diminishing and reduce hydration heat double properties is developed, ensure intensity and the work-ing life of mass concrete, improving concrete durability is very meaningful and value.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, the method technique is simple, easily-controlled reaction conditions, and the waste that can utilize that sugar industry is produced, environmental protection.
Technical scheme of the present invention is: the preparation method of a kind of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, it is characterized in that: its raw material composition and ratio is by weight: vinylformic acid 14% ~ 63%, isopentenol polyoxyethylene ether 33% ~ 80%, initiator 1% ~ 10%, reductive agent 0.2% ~ 3%, chain-transfer agent 0.2% ~ 3%, beet sirup yeast waste liquor properties-correcting agent 2.6% ~ 9%, beet sirup built agent accounts for 6% ~ 8% of synthesis mother liquid.
By such scheme, described initiator is the mixture of a kind of or two or more any proportioning in hydrogen peroxide, ammonium persulphate; Be more preferably one wherein.
By such scheme, described reductive agent is the mixture of a kind of or two or more any proportioning in ferrous sulfate, xitix; Be more preferably one wherein.
By such scheme, described chain-transfer agent is the mixture of a kind of or two or more any proportioning in Thiovanic acid, thiohydracrylic acid, mercaptoethanol; Be more preferably one wherein.
By such scheme, described beet sirup yeast waste liquor properties-correcting agent is beet sirup and yeast waste liquor mixed solution, its ratio 1:1.2 ~ 1:2.6.
During use, beet sirup the present invention prepared-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, adds different volumes according to different demands and drops in concrete in concrete mixer and stir according to normal concrete stirring technology.
The invention has the advantages that: (1) adopts beet sugar calcium; be not only water reducer and provide slow setting component; also make not need in building-up reactions to add sheet alkali to regulate pH air entrapment agent, the molasses of industrial waste are utilized in concrete admixture, meets the requirement of current environmental protection chemical industry.(2) vitriol that make use of in yeast wastewater improves the dispersing property of polycarboxylate water-reducer, and Mierocrystalline cellulose then can provide retarding performance for poly carboxylic acid, has also digested reluctant yeast wastewater in industry simultaneously, has met the requirement of current environmental protection chemical industry.(3) have employed the binary slow setting system of beet sirup and yeast wastewater, make polycarboxylate water-reducer of the present invention can realize the performance of initial stage ultra-low hydration heat, and the flowing property at initial stage does not reduce.
Embodiment
Below in conjunction with specific examples, the present invention will be further described.
In application example of the present invention, cement used is the new P.O42.5 of China, and breeze is S95 level, and flyash is secondary ash, and the fineness modulus of river sand is the medium sand of 2.7, and rubble is the stone of 5mm ~ 31.5mm continuous grading.
Concrete water-reducing rate, air content, the slump, divergence and ultimate compression strength are all carried out according to relating operation in GB8076-2008 and GB50081-2002.
Flowing degree of net paste of cement is according to the standard detection of GB8077-2000.
Hydration heat of cement adopts SHR-650D tester for cement hydration heat to measure.
Embodiment 1:
The there-necked flask that agitator is housed is positioned in control-temperature electric heating cover, add isopentenol polyoxyethylene ether 182.5g, water 100g, hydrogen peroxide 1g(concentration 30%) stir, be warming up to 45 DEG C, dropping 18.5g vinylformic acid is dissolved in the monomer solution in 20g water simultaneously, xitix 0.15g is dissolved in the reductant solution of 10g water, Thiovanic acid 0.3g is dissolved in the chain-transfer agent solution of 10g water, drip 2.5 hours, insulation slaking 1.5 hours, add in the NaOH solution of 32.1g30% and polymkeric substance to pH=7, obtain polycarboxylate water-reducer.Be diluted with water to the water reducer mother liquor of 10%, be designated as blank.
Embodiment 2:
The there-necked flask that agitator is housed is positioned in control-temperature electric heating cover, add beet sirup yeast waste liquor properties-correcting agent 56g(beet sugar calcium 24g, yeast wastewater 32g), isopentenol polyoxyethylene ether 192.5g, water 133g, hydrogen peroxide 0.7g(concentration 30%) stir, be warming up to 45 DEG C, dropping 21.5g vinylformic acid is dissolved in the monomer solution in 30g water simultaneously, xitix 0.15g is dissolved in the reductant solution of 10g water, and Thiovanic acid 0.25g is dissolved in the chain-transfer agent solution of 10g water, drips 2.5 hours, insulation slaking 1.5 hours, obtains polycarboxylate water-reducer.After adding beet sirup yeast waste liquor built agent, be diluted to the water reducer mother liquor of 10%, be designated as P1.
Embodiment 3:
The there-necked flask that agitator is housed is positioned in control-temperature electric heating cover, add molasses yeast waste liquor properties-correcting agent 56g(beet sugar calcium 17g, yeast wastewater 49g), isopentenol polyoxyethylene ether 192.5g, water 133g, hydrogen peroxide 0.7g(concentration 30%) stir, be warming up to 45 DEG C, dropping 21.5g vinylformic acid is dissolved in the monomer solution in 30g water simultaneously, xitix 0.15g is dissolved in the reductant solution of 10g water, and Thiovanic acid 0.25g is dissolved in the chain-transfer agent solution of 10g water, drips 2.5 hours, insulation slaking 1.5 hours, obtains polycarboxylate water-reducer.After adding beet sirup yeast waste liquor built agent, be diluted to the water reducer mother liquor of 10%, be designated as P2.
Water reducer mother liquor synthesized by embodiment is respectively used in the production of commerical ready-mixed concrete, its preparation method is: proportioning raw materials is: cement: breeze: flyash: water: river sand: rubble=1.0:0.38:0.41:0.67:3.21:5.10, and synthesis water reducer volume is 0.2%.Strength grade of concrete is C40.
Its detected result is table 1:
Table 1 concrete experiments result
Product water heat-transmission performance test results is as table 2:
Table 2 hydration heat performance test results
T
max: cement slurry hydration heat reaches the corresponding time of top temperature;
T
max: temperature corresponding when cement slurry hydration heat reaches top temperature;
Q
(1d): the cement slurry aquation thermal discharge of 1 day;
Q
(3d): the cement slurry aquation thermal discharge of 3 days.
Each raw material cited by the present invention, and the bound of each raw material of the present invention, interval value, and the bound of processing parameter (as temperature, time etc.), interval value can realize the present invention, do not enumerate embodiment at this.
Claims (4)
1. the preparation method of beet sirup-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, it is characterized in that: its raw material composition and ratio vinylformic acid 16% ~ 63% by weight, isopentenol polyoxyethylene ether 33% ~ 80%, initiator 1% ~ 10%, reductive agent 0.2% ~ 3%, chain-transfer agent 0.2% ~ 3%, beet sirup yeast waste liquor properties-correcting agent 2.4% ~ 9% is the mother liquor of synthesis water reducer, and beet sirup yeast waste liquor built agent accounts for synthesis water reducer mother liquor 6% ~ 8%; Preparation process is: add the isopentenol polyoxyethylene ether aqueous solution, beet sirup yeast waste liquor properties-correcting agent and initiator, heat up and stir, drip acrylic acid solution, chain-transfer agent solution and reductant solution respectively, dropwise slaking dilution discharging, obtained water reducer product after adding beet sirup yeast waste liquor built agent;
Wherein, vinylformic acid and isopentenol polyoxyethylene ether concentration of aqueous solution are 35wt% ~ 50wt%, and the concentration of initiator, reductive agent and the chain-transfer agent aqueous solution is 0.2wt% ~ 3wt%, and beet sirup yeast waste liquor modifier concentration is 65wt% ~ 80wt%; Described initiator is the one in hydrogen peroxide, ammonium persulphate, and described reductive agent is the one in ferrous sulfate, xitix, and described chain-transfer agent is the one in Thiovanic acid, thiohydracrylic acid, mercaptoethanol;
Described beet sirup yeast waste liquor properties-correcting agent and beet sirup yeast waste liquor built agent are the mixed solution of calcification beet sirup with yeast waste liquor, wherein calcification beet sirup component accounts for 45% ~ 70% of properties-correcting agent, and yeast waste liquor component accounts for 30% ~ 55% of properties-correcting agent.
2. the preparation method of a kind of beet sirup according to claim 1-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, is characterized in that: the molecular weight ranges of described isopentenol polyoxyethylene ether is 2200 ~ 3000.
3. the preparation method of a kind of beet sirup according to claim 1-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, is characterized in that: in described calcification beet sirup, the quality of reducing sugar is 5% ~ 40% of molasses solid substance.
4. the preparation method of a kind of beet sirup according to claim 1-yeast waste liquor ultra-low hydration heat polycarboxylate water-reducer, it is characterized in that: described yeast waste liquor main component is vitriol, and the residual sugar be not fully utilized in yeast protein, Mierocrystalline cellulose, colloidalmaterial and waste molasses accounts for 0.5% ~ 20% of total mass.
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| CN106966629A (en) * | 2017-04-13 | 2017-07-21 | 贵州科之杰新材料有限公司 | A kind of preparation method of polycarboxylate superplasticizer mother liquor |
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| CN102212175B (en) * | 2011-04-07 | 2012-08-29 | 江苏博特新材料有限公司 | Preparation method and application of molasses retarding and water-reducing agent |
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