CN106750076B - 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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- CN106750076B CN106750076B CN201710062899.3A CN201710062899A CN106750076B CN 106750076 B CN106750076 B CN 106750076B CN 201710062899 A CN201710062899 A CN 201710062899A CN 106750076 B CN106750076 B CN 106750076B
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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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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (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, the tannic acid extracted in liquid and tea waste is concentrated as raw material by using landfill leachate, successively after alkalization, sulfonation, Mannich reaction, it can be prepared by cement water reducing agent, tannic acid in the humic acid and tea waste of garbage disposal generation is made full use of, so that it is turned waste into wealth, realize secondary economic value, is of great significance to the cycling and reutilization for promoting resource.
Description
Technical field
The present invention relates to chemical assistant technical fields, mixed more particularly, to being produced using landfill leachate and tea waste
A kind of preparation method and applications of cement water reducing agent of solidifying soil water-reducing agent.
Background technique
Cement water reducing agent is one of the 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, guarantees simultaneously
The workability and intensity of concrete.Currently used water-reducing agent mainly has lignin sulfonate, naphthalene water reducer class and poly- carboxylic
Sour based water reducer class, wherein poly carboxylic acid series water reducer is high with water-reducing rate, reinforcing effect is significant, concrete workability is preferable,
The advantages that environmentally protective, but in practical concrete works in use, poly carboxylic acid series water reducer exists asks with cement compatibility
Topic, using effect is larger by cement composition composition influence, when especially containing the ingredients such as clay, due to the Inter layer adsorption of clay
Effect influences seriously, to reduce the working performance of concrete, constrain polycarboxylic acids on the diminishing dispersion performance of polycarboxylate water-reducer
The extensive use and development of based water reducer, in industrial processes, production cost is to determine product competitiveness in the market
One of an important factor for, if if the production cost of product is excessively high, preferable competitiveness can not be often obtained in price.
In China, tea culture has passed on thousands of years, and many people are met between relatives and friends or business partner visiting
When, can all make tea happy feelings, therefore the demand of tealeaves also increasingly rises, and many residues can be generated during tea processing
Or trimming clout, often enterprise can all be carried out burning and be used as fuel, this is a kind of processing of very uneconomical environmental protection
Mode, due to a large amount of tannic acid contained in tealeaves campanulaceae, 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 will be greatly reduced the production cost of cement water reducing agent,
Secondary economic benefit can be brought to the Solid state fermentation of tea processing.
In addition, the municipal refuse quantity in China increases different with Chinese society expanding economy, the quickening of urbanization process
Often rapidly, and during numerous urban garbage disposals, a large amount of rubbish air storage or landfill are not only taken up largely
Soil, and great secondary pollution easily is caused to soil, underground water, atmosphere, become serious environmental problem, since rubbish exists
It carries out that humic acid abundant can be generated during aerobic fermentation, and humic acid is a kind of unbodied organic high molecular compound,
There is research surface at present, is used as cement water reducing agent to apply after humic acid is carried out sulfonation modifying, it can be to cement granules
There is different degrees of peptizaiton, cement can be made to meet, and the wadding block agglomerated after water is broken, reduces the viscosity of cement slurry, increases stream
Dynamic property, and the strength of cement after hardening can be improved, so that reducing the use of cement in the case where fixing intensity demand
Amount, therefore the humic acid in rubbish garbage processing procedure is used to carry out production cement water reducing agent, to the energy for improving China
It is of great significance using environment and heat recovery.
Summary of the invention
In order to solve the deficiencies in the prior art, tea waste residue and garbage filter are utilized the purpose of the present invention is to provide a kind of
Preparation method and applications of the liquid as raw material, the cement water reducing agent of simple, the achievable industrialized production of technical process.
In order to realize above-mentioned technical purpose, the technical solution of the present invention is as follows:
A kind of preparation method of cement water reducing agent, it is original that the tea tannin in liquid and tea waste, which is concentrated, with landfill leachate
Material, successively after alkalization, sulfonation, Mannich reaction, can be prepared by cement water reducing agent.
Further comprising step in detail below:
(1) it is sieved after being crushed tea waste by 35~50 mesh screens, is then added to acetone-water system
Extracting solution in, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added in landfill leachate concentration liquid and carry out uniformly mixed, and pH is added
After the pH value of mixed solution is adjusted to 9~13 by regulator, add sulfonating agent, and by the control of the temperature of reaction system 60~
90 DEG C, carry out 1.5~3h of reaction；
(3) be sequentially added into the mixed solution after above-mentioned reaction catalyst, aldehyde compound, aminated compounds and water into
Row Mannich reaction, and the temperature of reaction system is adjusted to 65~85 DEG C, carry out 1~3.5h of reaction；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to spraying
It is spray-dried in drying equipment, can be prepared by the cement water reducing agent of brown powder shape.
Preferably, the addO-on therapy and mass fraction in each step are as follows:
Preferably, the tea ash of the tea waste is trimmed for tea place branches and leaves, tea leaf refining factory produces instant tea or ice
At least one of tea cake after tea grounds, tea grounds oil expression, tea fruit, tea stalk, tea dust after tea beverage mix.
Preferably, landfill leachate concentration liquid is that landfill leachate stoste is dense after biochemical film concentration
Contracting liquid, the landfill leachate concentration fluid solid content is 15%~55%.
Preferably, the pH adjusting agent is sodium hydroxide, potassium carbonate, sodium carbonate sodium citrate, potassium citrate, bicarbonate
At least one of trisodium, sodium dihydrogen citrate mix.
Preferably, the sulfonating agent be ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, in sodium sulfite extremely
Few one kind mixes.
Preferably, the catalyst is hydrogen peroxide, in the concentrated sulfuric acid, iodine, acetophenone, benzaldehyde, phenyl ethylamine, bismuth chloride
At least one mix.
Preferably, the aldehyde compound is formaldehyde, in acetaldehyde, glutaraldehyde, methacrylaldehyde, metaformaldehyde, paraformaldehyde
At least one mix.
Preferably, the aminated compounds is piperidines, in dimethylamine, acrylamide, phthalimide, ethylenediamine
At least one mix.
Preferably, the temperature of the spray drying device is 140~350 DEG C, and equipment export temperature is 70~95 DEG C,
The middle dry powder rate of recovery after spraying is greater than 95%.
Preferably, the relative molecular mass of the cement water reducing agent of brown powder shape made from the step (4) is 15000
~33000.
A kind of application of the cement water reducing agent according to obtained by a kind of above-mentioned preparation method of cement water reducing agent, will make
Cement water reducing agent be added in concrete by 0.1%~7% additive amount of concrete gross mass carry out using.
Using above-mentioned technical solution, the invention has the benefit that liquid and tealeaves is concentrated by using landfill leachate
The tannic acid extracted in waste material is as raw material, successively after alkalization, sulfonation, Mannich reaction, can be prepared by concrete diminishing
Tannic acid in the humic acid and tea waste of garbage disposal generation is made full use of, it is made to turn waste into wealth by agent, realizes two
Secondary economic value is of great significance to the cycling and reutilization for promoting resource.
Specific embodiment
A kind of preparation method of cement water reducing agent, it is original that the tea tannin in liquid and tea waste, which is concentrated, with landfill leachate
Material, successively after alkalization, sulfonation, Mannich reaction, can be prepared by cement water reducing agent.
Further comprising step in detail below:
(1) it is sieved after being crushed tea waste by 35~50 mesh screens, is then added to acetone-water system
Extracting solution in, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added in landfill leachate concentration liquid and carry out uniformly mixed, and pH is added
After the pH value of mixed solution is adjusted to 9~13 by regulator, add sulfonating agent, and by the control of the temperature of reaction system 60~
90 DEG C, carry out 1.5~3h of reaction；
(3) be sequentially added into the mixed solution after above-mentioned reaction catalyst, aldehyde compound, aminated compounds and water into
Row Mannich reaction, and the temperature of reaction system is adjusted to 65~85 DEG C, carry out 1~3.5h of reaction；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to spraying
It is spray-dried in drying equipment, can be prepared by the cement water reducing agent of brown powder shape.
Preferably, the addO-on therapy and mass fraction in each step are as follows:
Preferably, the tea ash of the tea waste is trimmed for tea place branches and leaves, tea leaf refining factory produces instant tea or ice
At least one of tea cake after tea grounds, tea grounds oil expression, tea fruit, tea stalk, tea dust after tea beverage mix.
Preferably, landfill leachate concentration liquid is that landfill leachate stoste is dense after biochemical film concentration
Contracting liquid, the landfill leachate concentration fluid solid content is 15%~55%.
Preferably, the pH adjusting agent is sodium hydroxide, potassium carbonate, sodium carbonate sodium citrate, potassium citrate, bicarbonate
At least one of trisodium, sodium dihydrogen citrate mix.
Preferably, the sulfonating agent be ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, in sodium sulfite extremely
Few one kind mixes.
Preferably, the catalyst is hydrogen peroxide, in the concentrated sulfuric acid, iodine, acetophenone, benzaldehyde, phenyl ethylamine, bismuth chloride
At least one mix.
Preferably, the aldehyde compound is formaldehyde, in acetaldehyde, glutaraldehyde, methacrylaldehyde, metaformaldehyde, paraformaldehyde
At least one mix.
Preferably, the aminated compounds is piperidines, in dimethylamine, acrylamide, phthalimide, ethylenediamine
At least one mix.
Preferably, the temperature of the spray drying device is 140~350 DEG C, and equipment export temperature is 70~95 DEG C,
The middle dry powder rate of recovery after spraying is greater than 95%.
Preferably, the relative molecular mass of the cement water reducing agent of brown powder shape made from the step (4) is 15000
~33000.
A kind of application of the cement water reducing agent according to obtained by a kind of above-mentioned preparation method of cement water reducing agent, will make
Cement water reducing agent be added in concrete by 0.1%~7% additive amount of concrete gross mass carry out using.
Embodiment 1
A kind of preparation method of cement water reducing agent comprising following steps:
(1) it is sieved after being crushed the tea stalk of 300Kg tea leaf refining factory by 40 mesh screens, is then added to third
In ketone-aqueous systems extracting solution, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added to 300Kg solid content be 55% landfill leachate be concentrated liquid in into
Row is uniformly mixed, and is added after the pH value of mixed solution is adjusted to 9 by 20Kg sodium hydroxide, add 89Kg with ammonium sulfate with
The mixture that sulfamic acid is mixed by 3: 1 mass ratio, and the temperature of reaction system is controlled at 60 DEG C, it is reacted
1.5h；
(3) 1.5Kg hydrogen peroxide, 125Kg formaldehyde, 69Kg is added sequentially into the mixed solution after above-mentioned reaction with piperazine
The mixture and 95.5Kg water that pyridine, dimethylamine, acrylamide are mixed by 1: 2: 3 mass ratio carry out Mannich reaction, and will
The temperature of reaction system is adjusted to 65 DEG C, carries out reaction 1.5h；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to equipment
It is spray-dried in the spray drying device that temperature is 140 DEG C, outlet temperature is 70 DEG C, can be prepared by the mixed of brown powder shape
Solidifying soil water-reducing agent, wherein the dry powder rate of recovery after spraying is 96.6%, the average molecular matter of obtained cement water reducing agent
Amount is 15000.
Embodiment 2
A kind of preparation method of cement water reducing agent comprising following steps:
(1) it is sieved after being crushed the tea stalk of 460Kg tea leaf refining factory by 50 mesh screens, is then added to third
In ketone-aqueous systems extracting solution, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added to 250Kg solid content be 15% landfill leachate be concentrated liquid in into
Row be uniformly mixed, and be added 16Kg will be mixed with sodium hydroxide with the mixture that potassium citrate is mixed by 3: 1 mass ratio it is molten
After the pH value of liquid is adjusted to 11, the mixing of 60Kg being mixed into sulfamic acid and sodium sulfite by 2: 1 mass ratio is added
Object, and the temperature of reaction system is controlled at 80 DEG C, carry out reaction 2.5h；
(3) it is mixed by 1: 1 mass ratio with benzaldehyde and phenyl ethylamine that 1Kg is sequentially added into the mixed solution after above-mentioned reaction
Mixture, 69Kg metaformaldehyde, 40Kg phthalimide and the 104Kg water of synthesis carry out Mannich reaction, and will reaction
The temperature of system is adjusted to 70 DEG C, carries out reaction 2h；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to equipment
It is spray-dried in the spray drying device that temperature is 350 DEG C, outlet temperature is 90 DEG C, can be prepared by the mixed of brown powder shape
Solidifying soil water-reducing agent, wherein the dry powder rate of recovery after spraying is 97.4%, the average molecular matter of obtained cement water reducing agent
Amount is 31000.
Embodiment 3
A kind of preparation method of cement water reducing agent comprising following steps:
(1) it is sieved after being crushed the tea stalk of 380Kg tea leaf refining factory by 35 mesh screens, is then added to third
In ketone-aqueous systems extracting solution, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added to 350Kg solid content be 35% landfill leachate be concentrated liquid in into
Row be uniformly mixed, and be added 62Kg will be mixed with sodium hydroxide with the mixture that potassium citrate is mixed by 3: 1 mass ratio it is molten
After the pH value of liquid is adjusted to 13, the mixing of 35Kg being mixed into sulfamic acid and sodium sulfite by 2: 1 mass ratio is added
Object, and the temperature of reaction system is controlled at 90 DEG C, carry out reaction 3h；
(3) be sequentially added into the mixed solution after above-mentioned reaction 1.2Kg with benzaldehyde and phenyl ethylamine by 1: 1 mass ratio
Mixture, 43Kg metaformaldehyde, 100Kg phthalimide and the 28.8Kg water being mixed into carry out Mannich reaction, and will
The temperature of reaction system is adjusted to 85 DEG C, carries out reaction 3h；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to equipment
It is spray-dried in the spray drying device that temperature is 300 DEG C, outlet temperature is 95 DEG C, can be prepared by the mixed of brown powder shape
Solidifying soil water-reducing agent, wherein the dry powder rate of recovery after spraying is 98.5%, the average molecular matter of obtained cement water reducing agent
Amount is 33000.
Performance test
Using reference cement, cement water reducing agent obtained by embodiment 1 is tested for the property, as a result such as following table institute
Show:
Table one: concrete mixture characteristic (water-reducing agent consolidates volume 0.5%)
| 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 with cement of the water-reducing agent obtained above to different compositions, as a result as follows:
Table two: dispersibility of the water-reducing agent in different composition cement
| Cement type | Water-reducing agent volume (%) | Initial flow degree (mm) | 1h fluidity (mm) |
| Striaght cement | 0.5% | 250 | 245 |
| 5% cement of clay content | 0.5% | 245 | 236 |
The above is the embodiment of the present invention, for the ordinary skill in the art, religion according to the present invention
Lead, without departing from the principles and spirit of the present invention all equivalent changes done according to scope of the present invention patent, repair
Change, replacement and variant, is all covered by the present invention.
Claims (10)
1. a kind of preparation method of cement water reducing agent, it is characterised in that: be concentrated in liquid and tea waste with landfill leachate
Tea tannin is raw material, successively after alkalization, sulfonation, Mannich reaction, can be prepared by cement water reducing agent.
2. a kind of preparation method of cement water reducing agent according to claim 1, it is characterised in that: it includes in detail below
Step:
(1) it is sieved after being crushed tea waste by 35~50 mesh screens, is then added to mentioning for acetone-water system
It takes in liquid, the tea tannin in tea waste is extracted using microwave method；
(2) by said extracted to tea tannin be added to landfill leachate concentration liquid in carry out it is uniformly mixed, and be added pH adjusting
After the pH value of mixed solution is adjusted to 9~13 by agent, sulfonating agent is added, and the temperature of reaction system is controlled 60~90
DEG C, carry out 1.5~3h of reaction；
(3) it is graceful that catalyst, aldehyde compound, aminated compounds and water progress are sequentially added into the mixed solution after above-mentioned reaction
Ni Xi reaction, and the temperature of reaction system is adjusted to 65~85 DEG C, carry out 1~3.5h of reaction；
(4) solution after step (3) reaction is filtered, after taking solid content to be washed with ethyl alcohol, is added to spray drying
It is spray-dried in equipment, can be prepared by the cement water reducing agent of brown powder shape.
3. a kind of preparation method of cement water reducing agent according to claim 2, it is characterised in that: in each step
AddO-on therapy and mass fraction are as follows:
Tea waste 30%~46%；
Liquid 25%~35% is concentrated in landfill leachate；
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. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: the tealeaves
Waste material be the branches and leaves of tea place trimming, tea leaf refining factory tea ash, produce the tea grounds after instant tea or ice tea drink, after tea grounds oil expression
Tea cake, tea fruit, tea stalk, at least one of tea dust.
5. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: the rubbish
Diafiltration concentrated liquor is concentrate of the landfill leachate stoste after biochemical film concentration, the landfill leachate concentration
Fluid solid content is 15%~55%.
6. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: the pH tune
Section agent be sodium hydroxide, potassium carbonate, sodium carbonate, sodium citrate, potassium citrate, sodium sesquicarbonate, in sodium dihydrogen citrate at least
It is a kind of.
7. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: the sulfonation
Agent is at least one of ammonium persulfate, ammonium bisulfite, sulfamic acid, sulfuric acid, sodium sulfite；The catalyst is peroxide
Change at least one of hydrogen, the concentrated sulfuric acid, bismuth chloride.
8. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: the aldehydes
Compound is at least one of formaldehyde, acetaldehyde, glutaraldehyde, methacrylaldehyde, paraformaldehyde；The aminated compounds be piperidines,
At least one of dimethylamine, acrylamide, phthalimide, ethylenediamine.
9. a kind of preparation method of cement water reducing agent according to claim 2 or 3, it is characterised in that: described is sprayed
The temperature of drying equipment is 140~350 DEG C, and equipment export temperature is 70~95 DEG C, wherein the dry powder rate of recovery after spraying is big
In 95%；The relative molecular mass of the cement water reducing agent of brown powder shape made from the step (4) is 15000~33000.
10. concrete diminishing obtained by a kind of a kind of preparation method of cement water reducing agent as claimed in claim 1,2 or 3
The application of agent, it is characterised in that: cement water reducing agent obtained is added by 0.1%~7% additive amount of concrete gross mass
Carried out into concrete using.
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| CN108503251B (en) * | 2018-04-18 | 2020-07-17 | 吉林建筑大学 | Concrete additive and preparation method thereof |
| 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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| CN100515976C (en) * | 2007-04-29 | 2009-07-22 | 晋城市炬坤生物科技有限公司 | Preparation method of humic acids cement water reducing agent |
| CN101492267B (en) * | 2009-03-06 | 2011-08-10 | 中南林业科技大学 | Method for producing high-efficiency concrete additive by using bark rich in tannic acid |
| CN103539952B (en) * | 2012-07-10 | 2017-04-12 | 厦门大学 | Novel humic acid sulfonatiion process |
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