CN105800986B - A kind of preparation method of cement water reducing agent - Google Patents
A kind of preparation method of cement water reducing agent Download PDFInfo
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- CN105800986B CN105800986B CN201610131910.2A CN201610131910A CN105800986B CN 105800986 B CN105800986 B CN 105800986B CN 201610131910 A CN201610131910 A CN 201610131910A CN 105800986 B CN105800986 B CN 105800986B
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- reducing agent
- water reducing
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A kind of preparation method of cement water reducing agent, it is characterised in that：Chinese chestnut thorn shell is crushed with plant pulverizer, cross 80 mesh sieves, take g Chinese chestnuts thorn shell powder, diatomite, PAMA, cornstarch 0.9g and toluenesulfonic acid 0.5g, it is added in 150ml water, it is heated to 40 DEG C, constant temperature stirs 2h, gained suspension is filtrated to get leaching liquor, filtrate is concentrated, and obtains concentrate A, then 1.5g starch and 1mlspan 80 are added in concentrate A, 0.5h is stirred under 1000rpm, the uniform emulsion of character is obtained, emulsion is concentrated again, is spray-dried to obtain modified tannin extract particle；Take above-mentioned gained modified tannin extract particle 20g, it is added to 3 ~ 5g of alkenes compounds, 0.5 ~ 1g of catalyst, 50 ~ 80g of water, catalytic synergist A is 1 ~ 2g and emulsifying agent 0.2g, 1 ~ 3h is reacted in 70 ~ 90 DEG C, add 3.5 ~ 5g of sodium hydrogensulfite, synergist B is that 0.2 ~ 0.4g reacts 2h in 60 ~ 80 DEG C, and add metal complex 0.3g, stirring reaction 2h at 60 ~ 80 DEG C, emulsion is obtained to concentrate again, it is spray-dried to obtain cement water reducing agent, gained cement water reducing agent, the preparation method is simple to operate, it is environment-friendly, there is excellent diminishing and dispersive property through polysulfonate type cement water reducing agent made from this method.
Description
Technical field
The present invention relates to a kind of preparation method of water reducer, more particularly to a kind of preparation method of cement water reducing agent.
Background technology
At present, four major classes can be largely classified into according to water reducer diminishing and enhancing ability, water reducer：First, with Lignins
Based on ordinary water-reducing agent, such water reducer is mostly powdery low air-entraining performance retarder, has micro- bleed, can improve concrete
Impervious freeze thawing performance.But for the molecular structure of such water reducer based on aromatic rings, compliance is poor.Second, using naphthalene water reducer as
The high efficiency water reducing agent of representative, this kind of water reducer are resistance to by parent with green and higher plasticity.But naphthalene water reducer is by molecule
The restriction of structure, the problem of can not fundamentally improving the function of slump protection and excessive volume of concrete.Third, the high property of polycarboxylic acid
There is ultra-dispersed property to turn into the focus studied at present for energy water reducer, this kind of water reducer, and development is swift and violent.But it, can shadow intolerant to hard water
Ring volume.Fourth, aliphatic sulfonic salt water reducer, it has excellent diminishing characteristic, and wherein sulfonic group hydrophily is strong, can provide
Forceful electric power lotus, while also can be resistant to hard water.Aliphatic sulfonic salt water reducer is that the main non-naphthalene system to grow up in recent years subtracts
One of aqua, it is its production technology letter for primary raw material with acetone, formaldehyde, sodium sulfite, sodium pyrosulfite etc.
It is single, it is with short production cycle.But more based on single sulfonic group and disulfonic acid base, its water-reducing property is bad, while raw material has pollution, spinosity
Swash property smell, do not meet the requirement of green production.
Henan is Chinese chestnut big producing province of China, and discarded object thorn shell is always to be difficult to what is effectively utilized caused by Chinese chestnut plantation
Resource, using Chinese chestnut thorn shell production water reducer, the recycling of discarded object can be accomplished, turned waste into wealth.
The content of the invention
It is an object of the invention to provide a kind of preparation method of cement water reducing agent, the preparation method is simple to operate, ring
Border is friendly, has excellent diminishing and dispersive property through polysulfonate type cement water reducing agent made from this method.
Cement water reducing agent by modified tannin extract particle, alkenes compounds, catalyst g, catalytic synergist A and emulsifying agent,
Sodium hydrogensulfite, synergist B, the active stronger double bond of alkenes compounds, reacted with modified tannin extract and in NaHSO3 work
After lower sulfonation, the water-soluble polymer of multi-sulfonic is made, multi-sulfonic can provide forceful electric power lotus, can be stretched in the aqueous solution
In, formed with certain thickness hydrophily solid adsorption layer, so that in the cement particle surface adsorbed formed with certain thickness
Hydrophily solid adsorption layer preferably play its water-reduction, additionally it is possible to resistance to hard water.Meanwhile contained alkene can strengthen
Steric hindrance and molecular flexibility, when cement granules close to when, adsorption layer starts overlapping, and space can be produced between cement granules
Steric hindrance, overlapping more, steric hindrance repulsion is bigger, also bigger the obstruction of cohesion cement granules, thus strengthens
The dispersive property of cement.
A kind of preparation method of cement water reducing agent, it is characterised in that：
(1) Chinese chestnut is pierced into shell to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and 0.5g silicon
Diatomaceous earth, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, are heated to 40
DEG C, constant temperature stirring 2h, gained suspension being filtrated to get leaching liquor, filtrate is concentrated, and obtains concentrate A, then in concentrate A
Add under 1.5g cornstarch and 1mlspan-80,1000rpm and stir 0.5h, obtain the uniform emulsion of character, by emulsion again
Concentration, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, is added to 3 ~ 5g of alkenes compounds, 0.5 ~ 1g of catalyst, water 50
~ 80g, catalytic synergist A are 1 ~ 2g and emulsifying agent 0.2g, react 1 ~ 3h in 70 ~ 90 DEG C, add 3.5 ~ 5g of sodium hydrogensulfite, increasing
It is that 0.2 ~ 0.4g reacts 2h in 60 ~ 80 DEG C to imitate agent B, and adds metal complex 0.3g, stirring reaction 2h at 60 ~ 80 DEG C, is obtained
Emulsion concentrates again, is spray-dried to obtain cement water reducing agent.
Its alkenes compounds is any one in gefarnate, linolenic acid, acrylamide, methacrylic acid；It is urged
Agent is triethylene diamine, ammonium persulfate, N- cyclohexyl para toluene sulfonamide, titanium dioxide dicyclopentadiene, azo dicyano
Any one in valeric acid, 2,5- dimethyl -2,5- two (t-butylperoxy) hexane；
Catalytic synergist A is any one of D-Cycloserine, tetramethylethylenediamine；Emulsifying agent is diatomite, anion
Any one of type polyacrylamide；Synergist B is 2- allyls pentylcyclohexanone, 4- tert. butyl cyclohexanols, sodium cyclamate, glucose
Any one；Metallic compound is the aluminium of trialkyl tri-chlorination two, polyaluminium sulfate, two (ethyl acetoacetate base) aluminic acid isopropyls
Any one of ester, aluminium ethylate.
The invention has the characteristics that：
（1）Raw radical reaction is issued in catalyst action using alkenes compounds and tannin extract, is grafted on tannin extract,
Tannin extract molecular weight is improved, is substituted using sodium hydrogensulfite and tannin extract, replaced, reaction, addition etc. are reacted on heterocycle, raising evergreen chinquapin
Sulfonate radical ratio in glue.
（2）Prepared water reducer has and can provide forceful electric power lotus, while also can be resistant to hard water.
（3）Toluenesulfonic acid makes cornstarch fracture have double bond generation, and gained material is gathered with tannin extract, alkenes compounds
Close, form the water reducer with certain degree of polymerization.
（4）The aluminium of trialkyl tri-chlorination two, polyaluminium sulfate, two (ethyl acetoacetate base) aluminic acid isopropyl esters, alum
With carboxyl reaction, improve water reducer stability in hard water, two (ethyl acetoacetate base) aluminic acid isopropyl esters, aluminium ethylate buy inHangzhou is outstanding Xi Ka Chemical Co., Ltd.s。
（5）Raw materials used can purchase of the present invention all uses in the rank such as any producer, analysis level, chemical pure, technical grade.
（6）Span-80 isSorbester p17.
Embodiment
Example one
(1) Chinese chestnut is pierced into shell 800g to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and
0.5g diatomite, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, add
Gained suspension constant temperature stirring 2h, is filtrated to get leaching liquor, filtrate is concentrated, and obtains the concentration of solid content 20% by heat to 40 DEG C
Liquid A, then added in concentrate A and stir 0.5h under 1.5g cornstarch and 1mlspan-80,1000rpm, it is uniform to obtain character
Emulsion, emulsion is condensed into the concentrate of solid content 25% again, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, is added to gefarnate 3g, triethylene diamine 0.5g, water 50g, D- ring
Serine is 1g and diatomite 0.2g, reacts 1h in 70 DEG C, add sodium hydrogensulfite 3.5g, 2- allyl pentylcyclohexanone be 0.2g in
60 DEG C of reaction 2h, and trialkyl tri-chlorination two aluminium 0.3g is added, stirring reaction 2h at 60 DEG C, obtain emulsion and concentrate again, spray
Dry cement water reducing agent.
Example two
(1) Chinese chestnut is pierced into shell 800g to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and
0.5g diatomite, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, add
Gained suspension constant temperature stirring 2h, is filtrated to get leaching liquor, filtrate is concentrated, and obtains the concentration of solid content 20% by heat to 40 DEG C
Liquid A, then added in concentrate A and stir 0.5h under 1.5g cornstarch and 1mlspan-80,1000rpm, it is uniform to obtain character
Emulsion, emulsion is concentrated to the concentrate of solid content 25% again, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, is added to and adds linolenic acid 5g, ammonium persulfate 1g, water 80g, four
Methyl ethylenediamine is 2g and anion-polyacrylamide 0.2g, reacts 3h in 90 DEG C, adds sodium hydrogensulfite 5g, 4- tert-butyl group
Cyclohexanol is that 0.4g reacts 2h in 80 DEG C, and adds polyaluminium sulfate 0.3g, stirring reaction 2h at 80 DEG C, it is dense again to obtain emulsion
Contracting, is spray-dried to obtain cement water reducing agent.
Example three
(1) Chinese chestnut is pierced into shell 2000g to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and
0.5g diatomite, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, add
Gained suspension constant temperature stirring 2h, is filtrated to get leaching liquor, filtrate is concentrated, and obtains the concentration of solid content 20% by heat to 40 DEG C
Liquid A, then added in concentrate A and stir 0.5h under 1.5g cornstarch and 1mlspan-80,1000rpm, it is uniform to obtain character
Emulsion, emulsion is condensed into the concentrate of solid content 25% again, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, is added to and adds acrylamide 4g, N- cyclohexyl tolysulfonyl
Amine 0.75g, water 65g, tetramethylethylenediamine are 1.5g and diatomite 0.2g, react 2h in 80 DEG C, add sodium hydrogensulfite 4.2g,
Sodium cyclamate is that 0.3g reacts 2h in 70 DEG C, and adds two (ethyl acetoacetate base) aluminic acid isopropyl ester 0.3g, is stirred at 70 DEG C
2h is reacted, emulsion is obtained and concentrates again, be spray-dried to obtain cement water reducing agent.
Example four
(1) Chinese chestnut is pierced into shell 1200g to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and
0.5g diatomite, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, add
Gained suspension constant temperature stirring 2h, is filtrated to get leaching liquor, filtrate is concentrated, and obtains the concentration of solid content 20% by heat to 40 DEG C
Liquid A, then added in concentrate A and stir 0.5h under 1.5g starch and 1mlspan-80,1000rpm, it is uniformly newborn to obtain character
Liquid, emulsion is condensed into the concentrate of solid content 25% again, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, is added to methacrylic acid 3g, titanium dioxide dicyclopentadiene
0.5g, water 70g, tetramethylethylenediamine are 1g and diatomite 0.2g, react 1h in 75 DEG C, add sodium hydrogensulfite 4g, synergist B
It is that 0.25g reacts 2h in 75 DEG C, and adds aluminium ethylate 0.3g, stirring reaction 2h at 75 DEG C, obtains emulsion and concentrate again, spraying is dry
It is dry to obtain cement water reducing agent.
Example five
(1) Chinese chestnut is pierced into shell 2000g to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and
0.5g diatomite, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, add
Gained suspension constant temperature stirring 2h, is filtrated to get leaching liquor, filtrate is concentrated, and obtains the concentration of solid content 20% by heat to 40 DEG C
Liquid A, then added in concentrate A and stir 0.5h under 1.5g cornstarch and 1mlspan-80,1000rpm, it is uniform to obtain character
Emulsion, emulsion is condensed into the concentrate of solid content 25% again, is spray-dried to obtain modified tannin extract particle；
（2）Above-mentioned gained modified tannin extract particle 20g is taken, adds acrylamide 3.5g, azo dicyano valeric acid 0.8g, water
70g, tetramethylethylenediamine are 1g and diatomite 0.2g, react 3h in 75 DEG C, add sodium hydrogensulfite 5g, glucose be 0.4g in
80 DEG C of reaction 2h, and aluminium ethylate 0.3g and alum 0.2g is added, stirring reaction 2h at 80 DEG C, obtain emulsion and concentrate again,
It is spray-dried to obtain cement water reducing agent.
The present invention is further illustrated with reference to example.
The cement water reducing agent performance comparison of table one
Ordinary water-reducing agent uses Hubei Ai Jin Chemical Co., Ltd.s, and water reducer of the invention is better than ordinary water-reducing agent.
Claims (1)
- A kind of 1. preparation method of cement water reducing agent, it is characterised in that：(1) Chinese chestnut is pierced into shell to be crushed with plant pulverizer, crosses 80 mesh sieves, take gained 100g Chinese chestnuts thorn shell powder and 0.5g diatoms Soil, 0.9g PAMAs, cornstarch 0.9g and toluenesulfonic acid 0.5g, are added in 150ml water, are heated to 40 DEG C, constant temperature stirring 2h, gained suspension being filtrated to get leaching liquor, filtrate is concentrated, and obtains concentrate A, then in concentrate A Add under 1.5g cornstarch and 1mlspan-80,1000rpm and stir 0.5h, obtain the uniform emulsion of character, by emulsion again Concentration, is spray-dried to obtain modified tannin extract particle；（2）Take above-mentioned gained modified tannin extract particle 20g, be added to 3 ~ 5g of alkenes compounds, 0.5 ~ 1g of catalyst, water 50 ~ In 80g, catalytic synergist A1 ~ 2g and emulsifying agent 0.2g, 1 ~ 3h is reacted in 70 ~ 90 DEG C, adds 3.5 ~ 5g of sodium hydrogensulfite, synergy Agent B0.2 ~ 0.4g, 2h are reacted in 60 ~ 80 DEG C, and add metal complex 0.3g, stirring reaction 2h at 60 ~ 80 DEG C, obtain emulsion Concentrate again, be spray-dried to obtain cement water reducing agent, alkenes compounds are gefarnate, linolenic acid, acrylamide, methyl-prop Any one in olefin(e) acid, catalyst are triethylene diamine, ammonium persulfate, N- cyclohexyl para toluene sulfonamide, titanium dioxide dimerization Any one in cyclopentadiene, azo dicyano valeric acid, 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane, catalysis Synergist A is any one of D-Cycloserine, tetramethylethylenediamine, and emulsifying agent is diatomite, anion-polyacrylamide Any one, synergist B be 2- allyls pentylcyclohexanone, 4- tert. butyl cyclohexanols, sodium cyclamate, glucose any one, Metal complex is the aluminium of trialkyl tri-chlorination two, polyaluminium sulfate, two (ethyl acetoacetate base) aluminic acid isopropyl esters, aluminium ethylate Any one.
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| CN101492267A (en) * | 2009-03-06 | 2009-07-29 | 中南林业科技大学 | Method for producing high-efficiency concrete additive by using bark rich in tannic acid |
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| CN104450992A (en) * | 2014-11-17 | 2015-03-25 | 烟台大学 | Preparation method of modified tannin extract particles |
| CN105384380A (en) * | 2015-12-07 | 2016-03-09 | 安徽省阜南绿原化工有限公司 | Tannin extract/polycarboxylate concrete water reducer and preparation method thereof |
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| JP2007237026A (en) * | 2006-03-06 | 2007-09-20 | Kenjiro Makino | Method for manufacturing functional product using biomass |
| CN101492267A (en) * | 2009-03-06 | 2009-07-29 | 中南林业科技大学 | Method for producing high-efficiency concrete additive by using bark rich in tannic acid |
| CN101870849A (en) * | 2009-04-22 | 2010-10-27 | 中国科学院过程工程研究所 | New method for producing tanning extracts by ultrasonic-enhanced extraction of castanea mollissima bud |
| CN104450992A (en) * | 2014-11-17 | 2015-03-25 | 烟台大学 | Preparation method of modified tannin extract particles |
| CN105384380A (en) * | 2015-12-07 | 2016-03-09 | 安徽省阜南绿原化工有限公司 | Tannin extract/polycarboxylate concrete water reducer and preparation method thereof |
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