CN104556771B - A kind of clay inhibitor and preparation method and application - Google Patents
A kind of clay inhibitor and preparation method and application Download PDFInfo
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Abstract
A kind of clay inhibitor that the present invention provides,-ium compound A and polyhydric alcohol amine compound B by mass ratio is 1～5:1 are uniformly mixed at normal temperatures.Present invention also offers the preparation method of above-mentioned clay inhibitor and the application in suppression side effect of clay thereof.This clay inhibitor preparation technology is simple, easy to use, with low cost；-ium compound and the polyhydric alcohol amine compound synergism wherein contained, effectively reduces the clay negative effect to polycarboxylate water-reducer performance.
Description
Technical field
The invention belongs to the preparation field of cement water reducing agent auxiliary agent, be specifically related to a kind of clay suppressing side effect of clay and press down
Preparation and preparation method thereof.
Background technology
China's infrastructure project construction scale is huge in recent years, high-speed railway, highway, large bridge, hydroelectric project,
Urbanization Construction propelled at high velocity, concrete amount accounted for the whole world total amount more than half.But, quick along with engineering construction
Development, Aggregate consumption is huge, and the natural sand and stone resources of high-quality is the deficientest；The most remote arid area, it is impossible to
Aggregate is effectively cleaned so that the Aggregate clay content of some areas is gradually increased.Therefore, Machine-made Sand by
Gradually it is used widely in concrete, also the finest clayey stone powder, mud powder is brought in concrete simultaneously,
Causing concrete initial fluidity poor, fluidity loss is big, has a strong impact on the fresh mixing performance of concrete.
A large amount of engineering experiences and result of study show, the clayey micropowder in Aggregate is to Traditional Wood mahogany sulfonate diminishing
The impact of agent, aliphatic high-efficiency water reducing agent and naphthalene series high-efficiency water-reducing agent is relatively small, and for high performance water reducing agent of polyocarboxy acid
Impact relatively large；On the one hand higher due to the volume of conventional water reducing agents, on the other hand intrinsic due to polycarboxylate water-reducer
Molecular structure cause it the most sensitive for clay.Clay in Aggregate is mostly lamellar aluminosilicate class mineral,
The most easily imbibition, causes Free water in concrete to reduce, and slurry amount more than needed reduces, thus reduces concrete
Mobility；On the other hand layer structure specific surface area is big, and the enrichment of surface high-valence cationic, and a large amount of absorption polycarboxylic acids subtract
Water preparation, causes the water reducer molecular amounts for disperse cement particles to be greatly reduced, then reduces the dispersion of water reducer
Effect, concrete flowability is deteriorated.
In order to improve the mobility of concrete, the most conventional solution is to improve the initial volume of poly carboxylic acid series water reducer
Or use the approach repeatedly filling water reducer, but so not only increased considerably construction cost, and repeatedly add operation not
Convenient, easily cause water reducer and cross and mix, bleeding isolate to cause concrete to occur, workability variation, affects concrete construction
Performance, deteriorates concrete durability.
Based on this, increasing researcher begins to focus on the adaptability how improving poly carboxylic acid series water reducer to clay.One
Aspect, researcher first from change polycarboxylic acids molecular structure start with: as CN102923989 discloses a kind of anti-stick soil type
The preparation method of polycarboxylate water-reducer, this water reducer by two kinds of unsaturated polyoxy vinyl monomers, unsaturated monocarboxylic acid and
Derivatives monomer, unsaturated alkenyl sulphonate mixing copolymerization, then use polyethylene polyamine neutralization to form；CN102875051
Disclose a kind of polycarboxylate water-reducer that can resist clay adverse effect, its by thiazolinyl polyoxyethylene polyoxypropylene monomer, third
Olefin(e) acid or methacrylic acid, acrylamide derivative monomer are obtained by free-radical polymerized.But, changed poly-by part
The comonomer of carboxylic acid water reducer, can not be from substantially changing the clay absorption to polycarboxylic acids, because clay is to polycarboxylic acids
The hydroxyl of the absorption of water reducer, mainly surface of clay and the strong hydrogen bonding effect of polycarboxylate water-reducer side chain polyoxyethylene ehter bond
Caused, and unsaturated polyoxy vinyl monomer is the synthesis indispensable critical materials of polycarboxylate water-reducer.Meanwhile, such
Polycarboxylate water-reducer volume of water reducer when clay content is higher is the most at a relatively high, has increased considerably cost.On the other hand,
Researcher also begins to be considered as the scheme of additive compound: as CN101798197A discloses a kind of clay content that suppresses to gather materials
The control slow release polycarboxylate water reducing agent of impact, its main method is to use the polycarboxylate water-reducer of 75～95 parts and 2～5 parts
Retarder, 5～25 parts of slow releasing agents carry out physical compounding, thus reduce the clay negative effect to poly carboxylic acid series water reducer.
By additive compound, not changing the molecular structure of polycarboxylate water-reducer own and performance, motility is higher, and applicable surface is wider,
But the retarder of large dosage easily causes concrete coagulating time and extends, and it is easily caused air content rising, to later strength
Adversely affect.Such as, CN102718430A report one mix poly carboxylic acid series water reducer concrete clay content suppression
The preparation method of agent, its use the earth dispersed component of phosphoric acid salt, earth absorbed component and ion complexation exchange component by
Certain proportion carries out physical mixed, and it is mixed together with polycarboxylate water-reducer in concrete, improves polycarboxylic acids diminishing
The performance of agent.But it is owing to being that the compound of little molecule compounds, and volume is significantly higher, and cost performance is relatively low.
Therefore, develop and a kind of can effectively reduce the inhibitor that in aggregate, water reducer dispersive property is had side effects by clay, logical
Cross itself and water reducer, especially polycarboxylate water-reducer and carry out compounding use, under the conditions of certain clay content, can effectively drop
The side effect of low clay, improves initial dispersion ability and the dispersion holding capacity of polycarboxylate water-reducer, improves concrete flowing
Property, to promoting low-grade aggregate and the application of Machine-made Sand, it is achieved the sustainable development of concrete is significant.
Summary of the invention
Goal of the invention: in order to overcome above-mentioned the deficiencies in the prior art, it is an object of the invention to provide one and subtracts with polycarboxylic acids
Water preparation compounds the clay inhibitor extremely preparation method of use, and it solves the technical problem that and is: can be in higher clay content condition
Under, it is effectively ensured or improves initial dispersion ability and the dispersion holding capacity of polycarboxylate water-reducer, do not affect concrete simultaneously
Other performances such as setting time, air content, intensity.
Technical scheme: a kind of clay inhibitor that the present invention provides, by pure solid gauge, is 1～5:1 () by mass ratio
-ium compound A and polyhydric alcohol amine compound B be uniformly mixed at normal temperatures；
The structural formula of described-ium compound A is shown in formula I:
Wherein, R1ForN is the integer of 1～5；
The structural formula of described polyhydric alcohol amine compound B is as shown in Formula II:
Wherein, m is the integer of 1～5；EO is oxyethylene group, and PO is oxypropylene group；X, y respectively aoxidize second
Thiazolinyl and the number of repeat unit of oxypropylene group, 1≤x+y≤25, and x:y=2～10:1.
Preferably, the molecular weight of described polyhydric alcohol amine compound B is 500～5000.
Present invention also offers the preparation method of above-mentioned clay inhibitor, comprise the following steps:
(1) preparation of-ium compound A aqueous solution: at 10-60 DEG C, in polyamine compounds aqueous solution
It is slowly added dropwise quaternary ammonium reagent aqueous solution, is warming up to 60～90 DEG C of insulation reaction 1～4h after dripping off, to obtain final product；
(2) preparation of polyhydric alcohol amine compound B: in the presence of alkoxylating catalyst, polyamine compounds and epoxy second
Alkane, expoxy propane generation alkoxylation, to obtain final product；
(3) preparation of clay inhibitor: by-ium compound A aqueous solution and polyhydric alcohol amine compound B often
Under temperature, uniform mix homogeneously, to obtain final product.
Wherein, described polyamine compounds structural formula is as shown in formula III:
Wherein, p is the integer of 1～5；
Preferably, described polyamine compounds include ethylenediamine, diethylenetriamine, triethylene tetramine, TEPA, five
One or more in hexamine mix with arbitrary proportion.
Wherein, in step (1), described quaternary ammonium reagent is 2,3-epoxypropyltrimethylchloride chloride or 3-chloro-2-hydroxypropyl
Trimethyl ammonium chloride.
Wherein, in step (1), described quaternary ammonium reagent and the total mole number of all active hydrogens on polyamine compounds nitrogen-atoms
Identical, such as, polyamine compounds is the ethylenediamine of 1mol, and on its nitrogen-atoms, the total mole number of active hydrogen is 4mol, then
The consumption of quaternary ammonium reagent is 4mol.The time for adding of quaternary ammonium reagent aqueous solution is 2～6h, and rate of addition is fast, easily leads
Cause temperature rise is violent, and side reaction is many；Dripped slow, then efficiency is the lowest.In reaction system, solid content is 30-60%；Dense
Spending height, system viscosity increases, and is unfavorable for that reaction mass transfer conducts heat；Concentration is too low, then reduce reaction efficiency.Quaternary ammoniated
After reagent dropwise, properly increase reaction temperature, be conducive to improving reaction conversion ratio；Simultaneously as this reaction is to put
Thermal response, should suitably take cooling measure according to system temperature rise situation in preparation process, to ensure the stationarity of reaction.
Wherein, in step (2), described polyhydric alcohol amine compound B is sent out with oxirane and expoxy propane by polyamine compounds
Raw alkoxylation gained；This alkoxylation is the chemical reaction process known to pertinent art, described alkane
Epoxide catalyst includes metallic potassium, metallic sodium, naphthalene potassium, naphthalene sodium, hydrofining, sodium hydride, alkyl potassium alcoholate, alkylol
Sodium, potassium hydroxide, sodium hydroxide；Alkoxylating catalyst consumption is products therefrom weight (theoretical yield) after alkoxylate
0.02～0.2%；The reaction temperature of alkoxylate is 80～150 DEG C, and reaction pressure is 0.1～0.4MPa.Improve reaction temperature
Degree and pressure, be on the one hand conducive to accelerating alkoxylation and carry out, improve reaction efficiency, and on the other hand, too high is anti-
Answering temperature and pressure, be easily caused reaction excessively violent, by-product increases, and reacts poor controllability.
Wherein, in step (2), the mol ratio of oxirane and expoxy propane is 2～10:1, oxirane and expoxy propane
The amount of total material be 6～109:1 with the ratio of the amount of the material of polyamine compounds；By oxirane and the use of expoxy propane
Amount, the molecular weight controlling polyhydric alcohol amine compound B is 500～5000.
Present invention also offers the application in suppression side effect of clay of the above-mentioned clay inhibitor, this clay inhibitor can be with
It is used together after water reducer is compounding, it is also possible to be used alone；Conventional volume in use is that active component accounts for the material that is always gelled
The 0.01～0.3% of material weight, optimum adding quantity of pulverized is 0.02～0.1%.Volume is too low, then can not make us the inhibition of clay
Satisfied；Volume is too high, causes waste economically, and clay inhibition increases the most further；Engineering staff can root
Carried out preferably by test in this range according to practical situation.
Beneficial effect: the clay inhibitor preparation technology that the present invention provides is simple, easy to use, with low cost；Wherein,
-ium compound quaternary ammoniated degree is high, can produce Electrostatic Absorption with the negative charge of surface of clay, and it is brilliant to embed clay
Layer, thus stop the entrance of hydrone, therefore can effectively suppress the hydration swelling of clay, reduce clay to slurry freely
The consumption of water；Wherein, polyhydric alcohol amine compound contains a large amount of ehter bond and hydroxyl, can with surface of clay generation adsorption by hydrogen bond,
Forming adsorption layer, introduce the higher expoxy propane of steric hindrance and oxirane copolymerization, its hydrophilic-hydrophobic structure further increases
Adsorbent layer thickness, thus prevent the clay absorption to polycarboxylic admixture, therefore can make more polycarboxylate water-reducer
Dispersion for cement granules；-ium compound and polyhydric alcohol amine compound synergism, effectively reduces clay pair
The negative effect of polycarboxylate water-reducer performance.
Detailed description of the invention
Following example describe in further detail the method according to the invention and prepare the process of clay inhibitor, and these are real
Execute example to be given by way of illustration, its object is to allow person skilled in the art will appreciate that present disclosure evidence
To implement, but these embodiments are in no way intended to limit the scope of the present invention.
The preparation of the-ium compound A of embodiment 1
Equipped with thermometer, agitator, Dropping funnel 1L glass round bottom flask in, add 49.6g water and 32.9g second
Diamidogen, is uniformly mixed, constant temperature to 20 DEG C, then by 330.5g 2, and 3-epoxypropyltrimethylchloride chloride and 491.6g
The mixed solution of water composition, persistently drops in round-bottomed flask with constant speed, time for adding 4h, after dropping, rises
Temperature, to 60 DEG C, continues stirring constant temperature 4h, obtains the-ium compound A-1 aqueous solution that solid content is 40%.
The preparation of the-ium compound A of embodiment 2
Equipped with thermometer, agitator, Dropping funnel 1L glass round bottom flask in, add 58.8g water and 25.1g bis-
Ethylene triamine, is uniformly mixed, constant temperature to 60 DEG C, then by 229.4g 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride with
The mixed solution of 536.2g water composition, persistently drops in round-bottomed flask with constant speed, time for adding 6h, drips complete
After, it is warming up to 90 DEG C, continues stirring constant temperature 1h, obtain the-ium compound A-2 that solid content is 30% water-soluble
Liquid.
The preparation of the-ium compound A of embodiment 3
Equipped with thermometer, agitator, Dropping funnel 1L glass round bottom flask in, add 61.1g water and 61.1g tri-
Ethylene tetramine, is uniformly mixed, constant temperature to 45 DEG C, then by 378.9g 2,3-epoxypropyltrimethylchloride chloride with
The mixed solution of 378.9g water composition, persistently drops in round-bottomed flask with constant speed, time for adding 4h, drips complete
After, it is warming up to 60 DEG C, continues stirring constant temperature 3h, obtain the-ium compound A-3 that solid content is 50% water-soluble
Liquid.
The preparation of the-ium compound A of embodiment 4
Equipped with thermometer, agitator, Dropping funnel 1L glass round bottom flask in, add 45.8g water, 13.1g second
Diamidogen and 43.6g TEPA, be uniformly mixed, constant temperature to 10 DEG C, then by chloro-for 468.3g 3-2-hydroxypropyl three
Ammonio methacrylate and the mixed solution of 312.2g water composition, persistently drop in round-bottomed flask with constant speed, time for adding
3h, after dropping, is warming up to 80 DEG C, continues stirring constant temperature 2h, obtains the organic cation that solid content is 60%
Compound A-4 aqueous solution.
The preparation of the-ium compound A of embodiment 5
Equipped with thermometer, agitator, Dropping funnel 1L glass round bottom flask in, add 66.8g water and 68.2g five
Hexamine, is uniformly mixed, constant temperature to 30 DEG C, then by 354.8g 2,3-epoxypropyltrimethylchloride chloride with
The mixed solution of 433.6g water composition, persistently drops in round-bottomed flask with constant speed, time for adding 2h, drips complete
After, it is warming up to 70 DEG C, continues stirring constant temperature 2h, obtain the-ium compound A-5 that solid content is 45% water-soluble
Liquid.
The preparation of embodiment 6 polyhydric alcohol amine compound B
85.4g ethylenediamine is placed in the rustless steel autoclave that 1L is dried, adds 0.72g Feldalat NM, stir,
Sealed reactor.With air three times in nitrogen displacement still, then by reactor evacuation, open heating, be warming up to 80 DEG C
After, persistently it is slowly introducing containing 492.8g oxirane and the mixture of 321.4g expoxy propane, maintains pressure in still
0.2～0.3MPa, reaction temperature 80～100 DEG C.After mixed material adds, continue isothermal reaction and no longer decline to pressure,
Maintain after 30min, be evacuated to below 0.08MPa and maintain 10min, by the oxirane of residual and expoxy propane from body
System removes, cools to 40 DEG C of dischargings, obtain the polyhydric alcohol amine compound B-1 that molecular weight is about 620.
The basic operational steps of embodiment 7～13 is same as in Example 6, reaction temperature, pressure and other parameters and conventional alcoxyl
Base metallization processes is suitable.Polyamines raw material, the molar ratio of ethylene oxide/propylene oxide and the gained polyhydric alcohol amine chemical combination used
The molecular weight of thing is as shown in Table 1 below.
The raw material of table 1 polyhydric alcohol amine compound and molecular weight
The preparation of embodiment 14 clay inhibitor
Under normal temperature condition, in the three neck round bottom flask of band stirring, it is sequentially added into 424.6g water, 392.9g organic cation
Compound A-1 aqueous solution and 142.8g polyhydric alcohol amine compound B-1, stir 30min mix homogeneously, and discharging obtains clay suppression
Agent CR-1, solid content is 31.2%.
The operating procedure of embodiment 15～23 is basically identical with embodiment 14, specifically used-ium compound A
Aqueous solution and the kind of polyhydric alcohol amine compound B and consumption are shown in Table 2.
The composition of table 2 clay inhibitor
Application Example
Prepared clay inhibitor is used for Mortar'S Flowability test, and experimental temperature is 25 DEG C.Wherein cement uses the south of the River
Little wild water in field mud P II 52.5 grades；Test sand uses iso standard sand, and cement-sand ratio is 1:2, and the ratio of mud is 0.44.Subtract
The volume of water preparation and clay inhibitor, on the basis of cement quality, by the solid gauge of folding, controls each group of mortar by defoamer and holds
Weight is basically identical.Wherein, the water reducer used is the polycarboxylate water-reducer of commercially available normal conventional；Clay selects 50%
Montmorillonite and the kaolinic homogeneous mixture of 50%, clay addition is by the mass percent accounting for sand.Mortar'S Flowability
Testing time stir respectively after initial flow degree and stand the fluidity being stirred for 30s after 30min, 60min.
Table 3 clay inhibitor is tested for Mortar'S Flowability
As seen from Table 3, in Mortar'S Flowability test, the clay content of 2% directly results in mixes water reducer mortar initial flow
Dynamic degree is greatly lowered, and fluidity loss is serious.The volume of water reducer is brought up to 0.26% by 0.15%, although energy
Be effectively improved initial Mortar'S Flowability, but through time fluidity still lose bigger, it is impossible to reach to be not added with the effect of clay.
And under conditions of keeping water reducer volume constant, by being properly added clay inhibitor, mortar initial flow can not only be improved
Moving degree, and fluidity keeps effect to be also obviously improved, bulk testing effect is better than individually improving the volume of water reducer.
Simultaneously it will be seen that the clay suppression that Application Example 11 and 12 is added is only one-component, it is at identical addition
Under the conditions of, action effect is limited, it is impossible to reach the mortar performance of Application Example 4～10.
Claims (6)
1. a clay inhibitor, it is characterised in that: by pure solid gauge,-ium compound A and polyhydric alcohol amine compound B by mass ratio is 1～5:1 are uniformly mixed at normal temperatures；
The structural formula of described-ium compound A is shown in formula I:
Wherein, R1ForN is the integer of 1～5；
The structural formula of described polyhydric alcohol amine compound B is as shown in Formula II:
Wherein, m is the integer of 1～5；EO is oxyethylene group, and PO is oxypropylene group；X, y are respectively the number of repeat unit of oxyethylene group and oxypropylene group, 1≤x+y≤25, and x:y=2～10:1.
A kind of clay inhibitor the most according to claim 1, it is characterised in that: the molecular weight of described polyhydric alcohol amine compound B is 500～5000.
3. the preparation method of a kind of clay inhibitor described in claim 1 or 2, it is characterised in that: comprise the following steps:
(1) preparation of-ium compound A aqueous solution: at 10-60 DEG C, be slowly added dropwise quaternary ammonium reagent aqueous solution in polyamine compounds aqueous solution, is warming up to 60～90 DEG C of insulation reaction 1～4h, to obtain final product after dripping off；
(2) preparation of polyhydric alcohol amine compound B: in the presence of alkoxylating catalyst, polyamine compounds and oxirane, expoxy propane generation alkoxylation, to obtain final product；
(3) preparation of clay inhibitor: by-ium compound A aqueous solution and polyhydric alcohol amine compound B uniform mix homogeneously at normal temperatures, to obtain final product；
In step (1), described polyamine compounds structural formula is as shown in formula III:
Wherein, p is the integer of 1～5；
Described quaternary ammonium reagent is 2,3-epoxypropyltrimethylchloride chloride or 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride.
The preparation method of a kind of clay inhibitor the most according to claim 3, it is characterised in that: in step (1), described quaternary ammonium reagent is identical with the total mole number of all active hydrogens on polyamine compounds nitrogen-atoms；In reaction system, solid content is 30-60%.
The preparation method of a kind of clay inhibitor the most according to claim 3, it is characterized in that: in step (2), described alkoxylating catalyst includes metallic potassium, metallic sodium, naphthalene potassium, naphthalene sodium, hydrofining, sodium hydride, alkyl potassium alcoholate, sodium alkyl alcohol, potassium hydroxide, sodium hydroxide；Alkoxylating catalyst consumption is after alkoxylate the 0.02～0.2% of products therefrom weight；The reaction temperature of alkoxylate is 80～150 DEG C, and reaction pressure is 0.1～0.4MPa.
The preparation method of a kind of clay inhibitor the most according to claim 3, it is characterized in that: in step (2), the mol ratio of oxirane and expoxy propane is 2～10:1, and the amount of total material of oxirane and expoxy propane is 6～109:1 with the ratio of the amount of the material of polyamine compounds.
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| CN105293976B (en) * | 2015-10-14 | 2017-10-31 | 广东红墙新材料股份有限公司 | A kind of pile tube and preparation method thereof |
| CN105647506B (en) * | 2016-01-21 | 2018-12-21 | 中国石油化工股份有限公司 | Oil-gas field fracturing clay stabilizer and preparation method thereof |
| CN111116898B (en) * | 2019-12-16 | 2022-04-01 | 江苏万邦新材料科技有限公司 | Clay inhibitor for polycarboxylate superplasticizer and preparation method thereof |
| CN111302721B (en) * | 2020-03-27 | 2022-04-08 | 浙江广天构件股份有限公司 | Preparation method of concrete slurry and pattern concrete prefabricated part |
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| CN101798197A (en) * | 2010-03-08 | 2010-08-11 | 南昌大学 | Controlled/slow release polycarboxylate water reducing agent for inhabiting aggregate mud content influence and preparation method thereof |
| CN101861360A (en) * | 2007-11-14 | 2010-10-13 | 阿克佐诺贝尔股份有限公司 | Asphalt modifiers for 'warm mix' applications including adhesion promoter |
| CN102923989A (en) * | 2012-11-16 | 2013-02-13 | 北京建筑工程学院 | Clay-resistant polycarboxylate water reducer and preparation method thereof |
| CN103723941A (en) * | 2013-12-11 | 2014-04-16 | 江苏苏博特新材料股份有限公司 | Clay inhibitor combined with polycarboxylic water reducer for use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101765641B (en) * | 2007-07-26 | 2016-09-21 | 阿克佐诺贝尔股份有限公司 | The adhesion of Colophonium and cohesion modifiers |
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| CN101861360A (en) * | 2007-11-14 | 2010-10-13 | 阿克佐诺贝尔股份有限公司 | Asphalt modifiers for 'warm mix' applications including adhesion promoter |
| CN101798197A (en) * | 2010-03-08 | 2010-08-11 | 南昌大学 | Controlled/slow release polycarboxylate water reducing agent for inhabiting aggregate mud content influence and preparation method thereof |
| CN102923989A (en) * | 2012-11-16 | 2013-02-13 | 北京建筑工程学院 | Clay-resistant polycarboxylate water reducer and preparation method thereof |
| CN103723941A (en) * | 2013-12-11 | 2014-04-16 | 江苏苏博特新材料股份有限公司 | Clay inhibitor combined with polycarboxylic water reducer for use |
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