CN106750076A - A kind of preparation method and applications of cement water reducing agent - Google Patents
A kind of preparation method and applications of cement water reducing agent Download PDFInfo
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- CN106750076A CN106750076A CN201710062899.3A CN201710062899A CN106750076A CN 106750076 A CN106750076 A CN 106750076A CN 201710062899 A CN201710062899 A CN 201710062899A CN 106750076 A CN106750076 A CN 106750076A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Processing Of Solid Wastes (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of preparation method and applications of cement water reducing agent, it is used as raw material by concentrating the tannic acid extracted in liquid and tea waste using percolate, after sequentially passing through alkalization, sulfonation, Mannich reaction, can be prepared by cement water reducing agent, tannic acid in humic acid and tea waste that garbage disposal is produced is made full use of, it is turned waste into wealth, realize secondary economic worth, the cycling and reutilization to promoting resource is significant.
Description
Technical field
It is mixed more particularly, to being produced using percolate and tea waste the present invention relates to chemical assistant technical field
A kind of preparation method and applications of the cement water reducing agent of solidifying soil water reducer.
Background technology
Cement water reducing agent is one of staple product of building materials industry, and Water-reducing Admixtures To Cements are added in concrete mix
Particle has peptizaiton, can improve the mobility of concrete mix, reduces unit cement consumption, saves cement, while ensureing
The workability and intensity of concrete.Conventional water reducer mainly has lignin sulfonate, naphthalene water reducer class and poly- carboxylic at present
Sour based water reducer class, wherein poly carboxylic acid series water reducer have that water-reducing rate is high, enhancing effect significantly, the workability of concrete preferably,
The advantages of environmental protection, but in actual concrete works when using, poly carboxylic acid series water reducer is present is asked with cement compatibility
Topic, its using effect is larger by cement composition composition influence, when particularly containing compositions such as clays, due to the Inter layer adsorption of clay
Effect, the diminishing dispersive property influence on polycarboxylate water-reducer is serious, and making the service behaviour of concrete reduces, and constrains polycarboxylic acids
The extensive use and development of based water reducer, in industrial processes, production cost is to determine product competitiveness commercially
One of key factor, if if the production cost of product is too high, preferable competitiveness cannot be often obtained in price.
In China, tea culture has passed on thousands of years, and many people are visiting gathering between relatives and friends or business partner
When, can all be made tea happy feelings, therefore the demand of tealeaves also increasingly rises, and the residue of many can be produced during Tea Processing
Or clout is pruned, often enterprise can all be burned and be used as fuel, and this is a kind for the treatment of of very uneconomical environmental protection
Mode, due to a large amount of tannic acid contained in tealeaves balloonflower root, waste residue, and tannic acid belongs to polycarboxylic acid, if can be extracted
Out using use is carried out in cement water reducing agent, that will substantially reduce the production cost of cement water reducing agent,
Secondary economic benefit can be brought to the Solid state fermentation of Tea Processing.
In addition, with Chinese society expanding economy, the quickening of urbanization process, the municipal refuse quantity of China increases different
It is often rapid, and during numerous urban garbage disposals, substantial amounts of rubbish air storage or landfill do not only take up largely
Soil, and great secondary pollution easily is caused to soil, underground water, air, as serious environmental problem, because rubbish exists
Carry out that during aerobic fermentation abundant humic acid can be produced, and humic acid is a kind of unbodied organic high molecular compound,
There is research surface at present, applied as cement water reducing agent after humic acid is carried out into sulfonation modifying, can be to cement granules
There is different degrees of peptizaiton, cement can be made to meet the wadding block condensed after water and crushed, reduce the viscosity of cement mortar, increase stream
Dynamic property, and the strength of cement after hardening can be improved so that in the case of fixing intensity demand, reduce the use of cement
Amount, therefore the humic acid in rubbish garbage processing procedure is used for carry out production cement water reducing agent, the energy to improving China
It is significant using environment and heat recovery.
The content of the invention
In order to solve the deficiencies in the prior art, tea waste residue and garbage filter are utilized it is an object of the invention to provide one kind
Liquid is used as raw material, technical process is simple, be capable of achieving the preparation method and applications of the cement water reducing agent of industrialized production.
In order to realize above-mentioned technical purpose, the technical scheme is that：
A kind of preparation method of cement water reducing agent, it is original that the tea tannin in liquid and tea waste is concentrated with percolate
Material, after sequentially passing through alkalization, sulfonation, Mannich reaction, you can cement water reducing agent is obtained.
Further, it includes step in detail below：
(1) sieved by 35~50 eye mesh screens after tea waste is crushed, be then added to acetone-water system
Extract solution in, the tea tannin in extraction tea waste is carried out using microwave method；
(2) by said extracted to tea tannin be added in percolate concentration liquid and be well mixed, and add pH
Conditioning agent adjusts to after 9~13 the pH value of mixed solution, adds sulfonating agent, and by the temperature control of reaction system 60~
90 DEG C, carry out 1.5~3h of reaction；
(3) toward sequentially adding catalyst, aldehyde compound, aminated compounds and water to enter in above-mentioned reacted mixed solution
Row Mannich reaction, and by the temperature adjustment of reaction system to 65~85 DEG C, carry out 1~3.5h of reaction；
(4) step (3) reacted solution is filtered, is taken after solid content washed with ethanol, be added to spraying
It is spray-dried in drying equipment, you can the cement water reducing agent of brown powder shape is obtained.
Preferably, the addO-on therapy and mass fraction in each step are：
Preferably, described tea waste be tea place prune branches and leaves, the tea ash of tea leaf refining factory, produce instant tea or ice
At least one in tea cake, tea fruit, tea stalk, tea dust after the oil expression of tea grounds, tea grounds after tea beverage is mixed.
Preferably, described percolate concentration liquid is percolate stoste by dense after biochemical film concentration
Contracting liquid, described percolate concentration fluid solid content is 15%~55%.
Preferably, described pH adjusting agent is NaOH, potassium carbonate, sodium carbonate sodium citrate, potassium citrate, bicarbonate
At least one in trisodium, sodium dihydrogen citrate is mixed.
Preferably, described sulfonating agent be ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, sodium sulfite in extremely
Few one kind is mixed.
Preferably, described catalyst is in hydrogen peroxide, the concentrated sulfuric acid, iodine, acetophenone, benzaldehyde, phenyl ethylamine, bismuth chloride
At least one mix.
Preferably, described aldehyde compound is in formaldehyde, acetaldehyde, glutaraldehyde, methacrylaldehyde, metaformaldehyde, paraformaldehyde
At least one mix.
Preferably, described aminated compounds is in piperidines, dimethylamine, acrylamide, phthalimide, ethylenediamine
At least one mix.
Preferably, the temperature of described spray drying device is 140~350 DEG C, and equipment outlet temperature is 70~95 DEG C, its
The middle dry powder rate of recovery through after spraying is more than 95%.
Preferably, the relative molecular mass of the cement water reducing agent of brown powder shape obtained in the step (4) is 15000
~33000.
A kind of application of cement water reducing agent according to obtained by a kind of above-mentioned preparation method of cement water reducing agent, will make
The cement water reducing agent for obtaining is added in concrete by the 0.1%~7% of concrete gross mass addition and is used.
Using above-mentioned technical scheme, beneficial effects of the present invention are：Liquid and tealeaves are concentrated by using percolate
The tannic acid extracted in waste material as raw material, after sequentially passing through alkalization, sulfonation, Mannich reaction, you can prepared concrete diminishing
Agent, the tannic acid in humic acid and tea waste that garbage disposal is produced is made full use of, and it is turned waste into wealth, and realizes two
Secondary economic worth, the cycling and reutilization to promoting resource is significant.
Specific embodiment
A kind of preparation method of cement water reducing agent, it is original that the tea tannin in liquid and tea waste is concentrated with percolate
Material, after sequentially passing through alkalization, sulfonation, Mannich reaction, you can cement water reducing agent is obtained.
Further, it includes step in detail below：
(1) sieved by 35~50 eye mesh screens after tea waste is crushed, be then added to acetone-water system
Extract solution in, the tea tannin in extraction tea waste is carried out using microwave method；
(2) by said extracted to tea tannin be added in percolate concentration liquid and be well mixed, and add pH
Conditioning agent adjusts to after 9~13 the pH value of mixed solution, adds sulfonating agent, and by the temperature control of reaction system 60~
90 DEG C, carry out 1.5~3h of reaction；
(3) toward sequentially adding catalyst, aldehyde compound, aminated compounds and water to enter in above-mentioned reacted mixed solution
Row Mannich reaction, and by the temperature adjustment of reaction system to 65~85 DEG C, carry out 1~3.5h of reaction；
(4) step (3) reacted solution is filtered, is taken after solid content washed with ethanol, be added to spraying
It is spray-dried in drying equipment, you can the cement water reducing agent of brown powder shape is obtained.
Preferably, the addO-on therapy and mass fraction in each step are：
Preferably, described tea waste be tea place prune branches and leaves, the tea ash of tea leaf refining factory, produce instant tea or ice
At least one in tea cake, tea fruit, tea stalk, tea dust after the oil expression of tea grounds, tea grounds after tea beverage is mixed.
Preferably, described percolate concentration liquid is percolate stoste by dense after biochemical film concentration
Contracting liquid, described percolate concentration fluid solid content is 15%~55%.
Preferably, described pH adjusting agent is NaOH, potassium carbonate, sodium carbonate sodium citrate, potassium citrate, bicarbonate
At least one in trisodium, sodium dihydrogen citrate is mixed.
Preferably, described sulfonating agent be ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, sodium sulfite in extremely
Few one kind is mixed.
Preferably, described catalyst is in hydrogen peroxide, the concentrated sulfuric acid, iodine, acetophenone, benzaldehyde, phenyl ethylamine, bismuth chloride
At least one mix.
Preferably, described aldehyde compound is in formaldehyde, acetaldehyde, glutaraldehyde, methacrylaldehyde, metaformaldehyde, paraformaldehyde
At least one mix.
Preferably, described aminated compounds is in piperidines, dimethylamine, acrylamide, phthalimide, ethylenediamine
At least one mix.
Preferably, the temperature of described spray drying device is 140~350 DEG C, and equipment outlet temperature is 70~95 DEG C, its
The middle dry powder rate of recovery through after spraying is more than 95%.
Preferably, the relative molecular mass of the cement water reducing agent of brown powder shape obtained in the step (4) is 15000
~33000.
A kind of application of cement water reducing agent according to obtained by a kind of above-mentioned preparation method of cement water reducing agent, will make
The cement water reducing agent for obtaining is added in concrete by the 0.1%~7% of concrete gross mass addition and is used.
Embodiment 1
A kind of preparation method of cement water reducing agent, it is comprised the following steps：
(1) sieved by 40 eye mesh screens after the tea stalk of 300Kg tea leaf refinings factory is crushed, be then added to third
In the extract solution of ketone-aqueous systems, the tea tannin in extraction tea waste is carried out using microwave method；
(2) by said extracted to tea tannin be added in percolate that 300Kg solid contents are 55% concentration liquid
Row is well mixed, and adds 20Kg NaOH to adjust to after 9 the pH value of mixed solution, add 89Kg with ammonium sulfate with
The mixture that sulfamic acid is mixed into by 3: 1 mass ratio, and the temperature control of reaction system is reacted at 60 DEG C
1.5h；
(3) toward sequentially adding 1.5Kg hydrogen peroxide, 125Kg formaldehyde, 69Kg with piperazine in above-mentioned reacted mixed solution
The mixture and 95.5Kg water that pyridine, dimethylamine, acrylamide are mixed into by 1: 2: 3 mass ratio carry out Mannich reaction, and will
The temperature adjustment of reaction system carries out reaction 1.5h to 65 DEG C；
(4) step (3) reacted solution is filtered, is taken after solid content washed with ethanol, be added to equipment
It is spray-dried in the spray drying device that temperature is 140 DEG C, outlet temperature is 70 DEG C, you can the mixed of brown powder shape is obtained
Solidifying soil water reducer, wherein be 96.6% through the dry powder rate of recovery after spraying, the average molecular matter of obtained cement water reducing agent
Measure is 15000.
Embodiment 2
A kind of preparation method of cement water reducing agent, it is comprised the following steps：
(1) sieved by 50 eye mesh screens after the tea stalk of 460Kg tea leaf refinings factory is crushed, be then added to third
In the extract solution of ketone-aqueous systems, the tea tannin in extraction tea waste is carried out using microwave method；
(2) by said extracted to tea tannin be added in percolate that 250Kg solid contents are 15% concentration liquid
Row is well mixed, and adds the 16Kg will to mix molten by the mixture that 3: 1 mass ratio is mixed into potassium citrate with NaOH
The pH value of liquid is adjusted to after 11, adds the mixing being mixed into by 2: 1 mass ratio with sulfamic acid and sodium sulfite of 60Kg
Thing, and by the temperature control of reaction system at 80 DEG C, carry out reaction 2.5h；
(3) toward sequentially adding in above-mentioned reacted mixed solution 1Kg to be mixed by 1: 1 mass ratio with benzaldehyde and phenyl ethylamine
The mixture of synthesis, 69Kg metaformaldehydes, 40Kg phthalimides and 104Kg water carry out Mannich reaction, and will reaction
The temperature adjustment of system carries out reaction 2h to 70 DEG C；
(4) step (3) reacted solution is filtered, is taken after solid content washed with ethanol, be added to equipment
It is spray-dried in the spray drying device that temperature is 350 DEG C, outlet temperature is 90 DEG C, you can the mixed of brown powder shape is obtained
Solidifying soil water reducer, wherein be 97.4% through the dry powder rate of recovery after spraying, the average molecular matter of obtained cement water reducing agent
Measure is 31000.
Embodiment 3
A kind of preparation method of cement water reducing agent, it is comprised the following steps：
(1) sieved by 35 eye mesh screens after the tea stalk of 380Kg tea leaf refinings factory is crushed, be then added to third
In the extract solution of ketone-aqueous systems, the tea tannin in extraction tea waste is carried out using microwave method；
(2) by said extracted to tea tannin be added in percolate that 350Kg solid contents are 35% concentration liquid
Row is well mixed, and adds the 62Kg will to mix molten by the mixture that 3: 1 mass ratio is mixed into potassium citrate with NaOH
The pH value of liquid is adjusted to after 13, adds the mixing being mixed into by 2: 1 mass ratio with sulfamic acid and sodium sulfite of 35Kg
Thing, and by the temperature control of reaction system at 90 DEG C, carry out reaction 3h；
(3) toward sequentially add in above-mentioned reacted mixed solution 1.2Kg with benzaldehyde and phenyl ethylamine by 1: 1 mass ratio
Mixture, 43Kg metaformaldehydes, 100Kg phthalimides and the 28.8Kg water being mixed into carry out Mannich reaction, and will
The temperature adjustment of reaction system carries out reaction 3h to 85 DEG C；
(4) step (3) reacted solution is filtered, is taken after solid content washed with ethanol, be added to equipment
It is spray-dried in the spray drying device that temperature is 300 DEG C, outlet temperature is 95 DEG C, you can the mixed of brown powder shape is obtained
Solidifying soil water reducer, wherein be 98.5% through the dry powder rate of recovery after spraying, the average molecular matter of obtained cement water reducing agent
Measure is 33000.
Performance test
Using reference cement, the cement water reducing agent obtained by embodiment 1 is carried out into performance test, as a result such as following table institute
Show：
Table one：Concrete mixture characteristic (the solid volume 0.5% of water reducer)
| Index | Air content | Compressive strength rate (28d) | Shrinkage ratio (28d) | Presetting period | Final setting time |
| Test | 3.5% | 170% | 115% | 2.5h | 3.5h |
Mud fluidity test is carried out to the cement of different compositions with water reducer obtained above, it is as a result as follows：
Table two：Dispersiveness of the water reducer in different composition cement
| Cement type | Water reducer volume (%) | Initial flow degree (mm) | 1h fluidities (mm) |
| Striaght cement | 0.5% | 250 | 245 |
| The cement of clay content 5% | 0.5% | 245 | 236 |
The above is embodiments of the invention, for the ordinary skill in the art, religion of the invention
Lead, without departing from the principles and spirit of the present invention all impartial changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to covering scope of the invention.
Claims (10)
1. a kind of preparation method of cement water reducing agent, it is characterised in that：With in percolate concentration liquid and tea waste
Tea tannin is raw material, after sequentially passing through alkalization, sulfonation, Mannich reaction, you can cement water reducing agent is obtained.
2. the preparation method of a kind of cement water reducing agent according to claim 1, it is characterised in that：It is included in detail below
Step：
（1）Sieved by 35~50 eye mesh screens after tea waste is crushed, be then added to carrying for acetone-water system
Take in liquid, the tea tannin in extraction tea waste is carried out using microwave method；
（2）By said extracted to tea tannin be added in percolate concentration liquid and be well mixed, and add pH to adjust
Agent adjusts to after 9~13 the pH value of mixed solution, adds sulfonating agent, and by the temperature control of reaction system 60~90
DEG C, carry out 1.5~3h of reaction；
（3）Catalyst, aldehyde compound, aminated compounds and water is sequentially added to carry out toward above-mentioned reacted mixed solution graceful
Ni Xi reacts, and by the temperature adjustment of reaction system to 65~85 DEG C, carries out 1~3.5h of reaction；
（4）By step（3）Reacted solution is filtered, and is taken after solid content washed with ethanol, is added to spray drying
It is spray-dried in equipment, you can the cement water reducing agent of brown powder shape is obtained.
3. the preparation method of a kind of cement water reducing agent according to claim 2, it is characterised in that：In each step
AddO-on therapy and mass fraction are：
Tea waste 30%~46%；
Percolate concentrates liquid 25%~35%；
PH adjusting agent 1.6%~6.2%；
Sulfonating agent 3.5%~8.9%；
Catalyst 0.1%~0.15%；
Aldehyde compound 4.3%~12.5%；
Aminated compounds 4%~10%；
Water 2.88%~10.4%.
4. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described tealeaves
Waste material be tea place prune branches and leaves, the tea ash of tea leaf refining factory, produce the tea grounds after instant tea or ice tea drink, tea grounds oil expression after
Tea cake, tea fruit, tea stalk, tea dust at least one mix.
5. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described rubbish
Diafiltration concentrated liquor is percolate stoste by the concentrate after biochemical film concentration, described percolate concentration
Fluid solid content is 15%~55%.
6. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described pH is adjusted
Section agent is at least in NaOH, potassium carbonate, sodium carbonate sodium citrate, potassium citrate, sodium sesquicarbonate, sodium dihydrogen citrate
Plant and mix.
7. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described sulfonation
Agent is that at least one in ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, sodium sulfite is mixed；Described catalysis
Agent is that at least one in hydrogen peroxide, the concentrated sulfuric acid, iodine, acetophenone, benzaldehyde, phenyl ethylamine, bismuth chloride is mixed.
8. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described aldehydes
Compound is that at least one in formaldehyde, acetaldehyde, glutaraldehyde, methacrylaldehyde, metaformaldehyde, paraformaldehyde is mixed；Described
Aminated compounds is that at least one in piperidines, dimethylamine, acrylamide, phthalimide, ethylenediamine is mixed.
9. the preparation method of a kind of cement water reducing agent according to Claims 2 or 3, it is characterised in that：Described spraying
The temperature of drying equipment is 140~350 DEG C, and equipment outlet temperature is 70~95 DEG C, wherein big through the dry powder rate of recovery after spraying
In 95%；The step（4）The relative molecular mass of the cement water reducing agent of obtained brown powder shape is 15000~33000.
10. the concrete diminishing obtained by a kind of a kind of preparation method of cement water reducing agent as described in claim 1,2 or 3
The application of agent, it is characterised in that：Obtained cement water reducing agent is pressed the 0.1%~7% of concrete gross mass addition addition
Used in concrete.
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| CN107586538A (en) * | 2017-09-27 | 2018-01-16 | 中石化石油工程技术服务有限公司 | A kind of low frictional resistance high-performance cement slurry system of suitable small size oil pipe |
| CN108503251A (en) * | 2018-04-18 | 2018-09-07 | 吉林建筑大学 | A kind of concrete admixture and preparation method |
| CN111560104A (en) * | 2020-06-29 | 2020-08-21 | 贵州师范学院 | Star polycarboxylic acid water reducing agent prepared by using tannic acid azo compound as initiator |
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| CN111560104B (en) * | 2020-06-29 | 2023-02-24 | 贵州师范学院 | Star polycarboxylic acid water reducing agent prepared by using tannic acid azo compound as initiator |
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