CN104909602B - Modifier for magnesium oxychloride cement as well as preparation method and applications thereof - Google Patents
Modifier for magnesium oxychloride cement as well as preparation method and applications thereof Download PDFInfo
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- CN104909602B CN104909602B CN201510290353.4A CN201510290353A CN104909602B CN 104909602 B CN104909602 B CN 104909602B CN 201510290353 A CN201510290353 A CN 201510290353A CN 104909602 B CN104909602 B CN 104909602B
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Abstract
The invention provides a modifier for magnesium oxychloride cement as well as a preparation method and applications thereof. The modifier contains H3PO4 and/or styrene-acrylic emulsion; and preferably, the modifier is composed of H3PO4 and styrene-acrylic emulsion, wherein in parts by weight, the modifier is composed of 0. 5-2 parts of the H3PO4 and 0.5-5 parts of the styrene-acrylic emulsion. By using the modifier provided by the invention, the water resistance and early strength of the cement are significantly improved.
Description
Technical field
The invention belongs to composition modified dose of field, and in particular to a kind of modifying agent and its preparation for magnesia oxychloride cement
Method and purposes.
Background technology
Magnesium oxychloride cementing material (magnesium oxychloride cement, MOC) MgO-MgCl2-H2The weight of O compositions
Inorganic gel system is wanted, because material strength losses are big after its poor water resistance, water suction so that it is subject to the very day of one's doom in engineer applied
System.From the point of view of current research is actual, although there has been proposed many active measures obtain preferable effect, chlorine oxygen magnesium glue
Gel material water resistance problem is solved not yet at all；Phosphoric acid and soluble phosphate are to be currently used in improve the gelling of chlorine oxygen magnesium
Material water repelling property it is main material modified, but phosphoric acid to cement retardative act on it is huge, under cement early strength can be caused serious
Drop；There is researcher to attempt waterresistant polymeric protection is formed in magnesia oxychloride cement hardenite by mixing emulsion polymerization
Film, covers hydrated product surface, fills hardenite hole, so as to improve the water resistance of magnesium oxychloride cementing material, but tries mostly
Test proving effect not good.The author is sent out in using the emulsion modified magnesia oxychloride cement water resistant test of the multiple polymers such as phenylpropyl alcohol, butylbenzene
Show most of high molecular polymers almost no modified effect, or even reduce the original water-fast and mechanical property of system.
The present invention intend the polymer such as phosphoric acid and phenylpropyl alcohol it is single it is modified on the basis of, using phosphoric acid with styrene-acrylic emulsion to chlorine oxygen
Magnesium cement carries out compound water resistance modified test, and research phosphoric acid/polymer is combined the effect for improving magnesia oxychloride cement water resistance
Really.
The content of the invention
Part, of the invention by distinguishing single modified in phosphoric acid, styrene-acrylic emulsion in order to overcome the above-mentioned deficiencies of the prior art
On the basis of research, magnesia oxychloride cement is carried out using phosphoric acid, styrene-acrylic emulsion composite modified, maximized favourable factors and minimized unfavourable ones, to playing this
The best effects of the bright modifying agent, searching out improves the optimal path of water resistance, finally obtains good novel building material
Material.
First purpose of the present invention is to provide a kind of modifying agent for magnesia oxychloride cement；
Second object of the present invention is to provide a kind of purposes of above-mentioned modifying agent in modified magnesium oxychloride cement is prepared；
Third object of the present invention is to provide a kind of modified magnesium oxychloride cement；
Fourth object of the present invention is to provide a kind of preparation method of above-mentioned modified magnesium oxychloride cement.
Technical scheme for realizing above-mentioned purpose is as follows：
A kind of modifying agent for magnesia oxychloride cement, the modifying agent include H3PO4And/or styrene-acrylic emulsion；Preferably, institute
Modifying agent is stated by H3PO4Constitute with styrene-acrylic emulsion；It is highly preferred that the H3PO4For liquid.
The modifying agent is by H3PO4Constitute with styrene-acrylic emulsion, wherein, count by weight, H in the modifying agent3PO4
0.5～2 part, 0.5～5 part of styrene-acrylic emulsion；Preferably, H in the modifying agent3PO4For 0.5 part or 1 part；Preferably, the phenylpropyl alcohol
Emulsion is 1 part or 4 parts.
The modifying agent is by H3PO4Constitute with styrene-acrylic emulsion, wherein, count by weight, H in the modifying agent3PO4
0.5 part, 1 part of styrene-acrylic emulsion.
Purposes of the modifying agent of the present invention in modified magnesium oxychloride cement is prepared.
A kind of modified magnesium oxychloride cement, the cement is using modifying agent of the present invention and MgO, MgCl2It is prepared.
The raw material of the cement includes 90～110 parts of MgO, MgCl235.5～43.5 parts, H3PO40.5～2 part, phenylpropyl alcohol
0.5～5 part of emulsion；Preferably, count by weight, the cement raw material includes 100 parts of MgO, MgCl2, 39.5 parts,
H3PO40.5 part, 1 part of styrene-acrylic emulsion.
The preparation method is comprised the following steps：Each raw material of the modified magnesium oxychloride cement is stirred into mixing in proportion,
Molding；
Preferably, the preparation method is comprised the following steps：
(1) by MgCl2The solution that Baume degrees are 24～26 ° of B é is made, then with H3PO4, styrene-acrylic emulsion mixing；
(2) MgO is added to step (1) mixture for obtaining, after forming even slurry, molding, maintenance；
Preferably, the modified magnesium oxychloride cement molding is conserved in air；It is highly preferred that conserving as 24 hours afterwards
The demoulding；
Preferably, the preparation method is further comprising the steps of：
(4) continue maintenance at least 7 days after the demoulding.
The present invention is described as follows：
In order to verify effect of each component to magnesia oxychloride cement resistance to water in the modifying agent for providing of the invention, carry out following
Research.
1st, test H
3
PO
4
Impact with styrene-acrylic emulsion respectively as single modifying agent to magnesia oxychloride cement water resistance
Raw material and reagent：
The light-burning magnesium powder in Liaoning Yingkou, Yancheng Xiangshui County halogen piece, industrial phosphoric acid liquid, styrene-acrylic emulsion.
Instrument and equipment：
SJD-30 type concrete mixers, SHBY-40A type cement standard curing boxes, 101A-3B type electric heating forced air dryings
Case, electronic balance, YAW-300B type pressure testing machines, QANTA-200 type scanning electron microscopes.
Test method：
The preparation of magnesia oxychloride cement matrix：The benchmark match ratio adopted in process of the test is for MgO: MgCl2=6: 1 (mole
Than), MgCl2Cement matrix is prepared using solution form, the Baume degrees (° B é) of the solution should be controlled 24～26.Will be prior
Weighing and the light-burned MgO powder for preparing, MgCl2Solution and modifying agent to be tested pour stirring (liquid in concrete mixer into
Modifying agent and MgCl2Solution mixes, and adds MgO), after forming even slurry, pour in 100mm × 100mm × 100mm moulds
Molding, the in atmosphere demoulding after natural curing 24h are conserved 3 days and 7 days respectively, soaked 7 days after 7 days, are divided in these three cases
Its comprcssive strength is not tested, according to GB/T17671-1999《Test method for strength of hydraulic cement mortar (ISO methods)》The side that standard specifies
Method is tested.
Sample after resistance to compression is used for SEM and XRD analysis.
Coefficient of softing is with reference to JG/T 1169-2005《Light lath for building partition wall》Middle assay method is carried out.Softening system
Number I=R1/R0, in formula：R1 be conserve 7 days after the comprcssive strength meansigma methodss of soaked 7 days again, R0 is absolute dry condition after maintenance 7 days
Under comprcssive strength meansigma methodss.
Blank testing sample, is the magnesia oxychloride cement for not adding modifying agent of the present invention simultaneously.
The comprcssive strength of different larval instar, different addition quantity (mass percent of modifying agent and MgO powder) modified magnesium oxychloride cement
And coefficient of softing result is as follows：
(1) H of magnesia oxychloride cement3PO4Modified effect is tested
The phosphoric acid for choosing 0.5%, 1%, 1.5%, 2% volume respectively is modified to magnesia oxychloride cement, different addition quantity
Modified effect is as shown in table 1.
Table 1：Modified effect of the phosphoric acid to magnesia oxychloride cement
As can be seen from Table 1, with the increase of phosphoric acid volume, the coefficient of softing of magnesia oxychloride cement is improved therewith, resistance to water
Significantly increase, but the early anti pressured intension of cement declines rapidly therewith, shows phosphoric acid to MgO-MgCl2-H2O systems Binder Materials have
Significantly deferred action.When volume phosphoric acid is 2%, the coefficient of softing of cement is up to 0.81, but 3 days comprcssive strength is only
42.3MPa, have dropped 29.3Mpa compared with blank sample.
Phosphoric acid can improve the resistance to water of magnesia oxychloride cement system and be because that phosphoric acid is reacted with hydrated product, in hydrated product
Surface defines the indissoluble magnesium phosphate protecting film of densification；The addition of phosphoric acid have also been changed the surface shape of hydrated product crystalline phase simultaneously
Looks so that sturdy 5Mg (OH)2·MgCl2·8H2O phase column crystals become elongated and round and smooth bar-shaped, so as to cause
Cement strength decline, before and after phosphoric acid incorporation, the SEM figures of magnesia oxychloride cement sample are respectively as Fig. 1 (a) and (b) are shown.
(2) the Modification of Styrene-Acrylate Emulsion measure of merit of magnesia oxychloride cement
The styrene-acrylic emulsion for choosing 0.5%, 1%, 2%, 3%, 5% volume respectively is modified to magnesia oxychloride cement, different
The modified effect of volume is as shown in table 2.
Table 2：Modified effect of the styrene-acrylic emulsion to magnesia oxychloride cement
As shown in table 2, styrene-acrylic emulsion almost no modified effect, or even reduce the original water-fast and mechanical property of system.
Its main cause is analyzed, the polymer binding property poor with hydrated product causes which be formed on hydrated product crystalline phase surface
Effectively fine and close water-fast protecting film, can not form in hydrated product structural system and preferably disperse and sprawl.
2nd, test H
3
PO
4
Impact of the combination with styrene-acrylic emulsion to magnesia oxychloride cement water resistance
Using 0.5% phosphoric acid and 1% styrene-acrylic emulsion, 1% phosphoric acid and 1% styrene-acrylic emulsion, 1% phosphoric acid and 4% styrene-acrylic emulsion
Respectively magnesia oxychloride cement is carried out composite modified, modified effect is as shown in table 3.
Table 3：The modified effect of phosphoric acid and styrene-acrylic emulsion to magnesia oxychloride cement
From table 3, appropriate phosphoric acid is compound not only excellent to the modified effect of magnesia oxychloride cement resistance to water with styrene-acrylic emulsion
In individually admixture styrene-acrylic emulsion, and it is much better than individually to fill phosphoric acid, coefficient of softing is close to 1, and overcomes phosphoric acid modification slow setting
The defect declined with early strength.But in the presence of appropriate phosphoric acid, the consumption for increasing styrene-acrylic emulsion is not The more the better；
Resistance to water when 0.5% phosphoric acid is filled and 1% styrene-acrylic emulsion carries out composite modified is optimal.Phosphoric acid is compound with styrene-acrylic emulsion to be caused
There is magnesia oxychloride cement more preferable water resistance to show, phosphoric acid changes styrene-acrylic emulsion and aquation with the interaction of styrene-acrylic emulsion
The binding ability of its surface, promotes adhesion and covering of the polymeric film on hydrated product surface, this is because in original phosphorus
Compound water-fast protective layer is defined on the basis of changing film.
Conclusion
(1) single phosphoric acid can improve the water resistance of magnesia oxychloride cement system, but have obvious deferred action to cement,
So that the early anti pressured intension of cement declines.
(2) single phenylpropyl alcohol emulsion polymerization does not have obvious modified effect to the water resistance of magnesia oxychloride cement,
The original water-fast and mechanical property of cement is reduced even.
(3) appropriate styrene-acrylic emulsion is combined with phosphoric acid, and magnesia oxychloride cement resistance to water modified effect is not only better than singly mixing poly-
Compound emulsion, and it is much better than single p-doped acid, and overcome the defect that phosphoric acid slow setting and early strength decline.It is of the invention
Specific embodiment, the modifying agent provided by the present invention for preparing modified magnesium oxychloride cement can cause the resistance to water of cement and
Early strength is significantly increased, and the early strength after conserving 3 days and 7 days can reach 64.1Mpa and 75.8Mpa respectively, and soft
Change coefficient and reach 0.99, the soaked intensity of soaked 7 days is up to 68.9MPa again after conserving 7 days.
Description of the drawings
Fig. 1 (a) is schemed for the cross-section morphology SEM of magnesia oxychloride cement blank sample；
Fig. 1 (b) is schemed for the modified magnesium oxychloride cement matrix sample section pattern SEM of the phosphoric acid that volume is 1%.
Specific embodiment
The present invention is further described in detail with reference to specific embodiment, the embodiment for being given is only for explaining
The bright present invention, rather than in order to limit the scope of the present invention.
Experimental technique in following embodiments, if no special instructions, is conventional method.Examination used in following embodiments
Material is tested, if no special instructions, is from routine biochemistry reagent shop what is be commercially available.
It is below each embodiment raw material and test method：
Raw material and reagent：
The light-burning magnesium powder in Liaoning Yingkou, Yancheng Xiangshui County halogen piece, industrial phosphoric acid liquid, styrene-acrylic emulsion.
Instrument and equipment：
SJD-30 type concrete mixers, SHBY-40A type cement standard curing boxes, 101A-3B type electric heating forced air dryings
Case, electronic balance, YAW-300B type pressure testing machines, QANTA-200 type scanning electron microscopes.
Comprcssive strength is according to GB/T17671-1999《Test method for strength of hydraulic cement mortar (ISO methods)》The method that standard specifies
Tested.Coefficient of softing is with reference to JG/T 1169-2005《Light lath for building partition wall》Middle assay method is carried out.Soften
Coefficient I=R1/R0, in formula：R1 be conserve 7 days after the comprcssive strength meansigma methodss of soaked 7 days again, R0 is over dry shape after maintenance 7 days
Comprcssive strength meansigma methodss under state.
Embodiment 1：The preparation of modified magnesium oxychloride cement of the present invention
Raw material：Count by weight, H3PO40.5 part, 0.5 part of styrene-acrylic emulsion, 90 parts of MgO powder body, MgCl235.5 parts.
Prepare and test：By MgCl2The solution that Baume degrees are 24～26 ° of B é is made, then with H3PO4, styrene-acrylic emulsion mix
Close；MgO and the mixture are poured in concrete mixer and are stirred, after forming even slurry, pour into 100mm × 100mm ×
100mm die for molding, in atmosphere the natural curing 24h demouldings are conserved 3 days and 7 days, soaked 7 days after 7 days respectively.Test 3
My god, the comprcssive strength after 7 days and again soaked 7 days, and test coefficient of softing.
Embodiment 2：The preparation of modified magnesium oxychloride cement of the present invention
Raw material：Count by weight, H3PO42 parts, 5 parts of styrene-acrylic emulsion, 110 parts of MgO powder body, MgCl243.5 parts.
Prepare and test with embodiment 1.
Embodiment 3：The preparation of modified magnesium oxychloride cement of the present invention
Raw material：Count by weight, H3PO40.5 part, 1 part of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Embodiment 4：The preparation of modified magnesium oxychloride cement of the present invention
Raw material：Count by weight, H3PO41 part, 4 parts of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Embodiment 5：The preparation of modified magnesium oxychloride cement of the present invention
Raw material：Count by weight, H3PO41 part, 1 part of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Comparative example 1：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO40.3 part, 0.3 part of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Comparative example 2：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO40.1 part, 0.2 part of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Comparative example 3：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO43 parts, 6 parts of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Comparative example 4：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO45 parts, 8 parts of styrene-acrylic emulsion, 100 parts of MgO powder body, MgCl239.5 parts.
Prepare and test with embodiment 1.
Comparative example 5：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO42 parts, 50 parts of flyash, 13 parts of styrene-acrylic emulsion, 100 parts of MgO powder body, NF is high
1 part of water reducer of effect, Baume degrees are 25 MgCl240 parts of solution, 50 parts of water.
Method according to patent application CN201210216756.0 embodiments 4 prepares modified magnesium oxychloride cement.
Comparative example 6：The preparation of modified magnesium oxychloride cement
Raw material：Count by weight, H3PO42.8 parts, 52 parts of flyash, 14.1 parts of styrene-acrylic emulsion, 100 parts of MgO powder body,
1.5 parts of NF high efficiency water reducing agents, Baume degrees are 30 MgCl239.1 parts of solution, 45.7 parts of water.
Method according to patent application CN201210216756.0 embodiments 4 prepares modified magnesium oxychloride cement.
The modified magnesium oxychloride cement water resistance contrast that in the present invention prepared by each embodiment and comparative example see the table below 4.
Table 4：Modified magnesium oxychloride cement water resistance prepared by various embodiments of the present invention is contrasted (in terms of parts by weight)
Conclusion：Phosphoric acid has very big lifting with styrene-acrylic emulsion to the composite modified effect of magnesia oxychloride cement, of the present invention modified
Agent, which is counted by weight, works as H3PO40.5 part, 1 part of styrene-acrylic emulsion when composite modified most pronounced effects.
Claims (14)
1. a kind of modifying agent for magnesia oxychloride cement, the modifying agent is by H3PO4Constitute with styrene-acrylic emulsion, wherein, by weight
Number meter, H in the modifying agent3PO40.5～2 part, 0.5～5 part of styrene-acrylic emulsion.
2. modifying agent according to claim 1, it is characterised in that the H3PO4For liquid.
3. modifying agent according to claim 1 and 2, it is characterised in that H in the modifying agent3PO4For 0.5 part or 1 part.
4. modifying agent according to claim 1 and 2, it is characterised in that styrene-acrylic emulsion is 1 part or 4 parts in the modifying agent.
5. modifying agent according to claim 1 and 2, it is characterised in that H in the modifying agent3PO40.5 part, styrene-acrylic emulsion
1 part.
6. purposes of the modifying agent as any one of claim 1 to 5 in modified magnesium oxychloride cement is prepared.
7. a kind of modified magnesium oxychloride cement, it is characterised in that the cement is adopted as any one of claim 1 to 5
Modifying agent and MgO, MgCl2It is prepared.
8. modified magnesium oxychloride cement according to claim 7, it is characterised in that the raw material of the cement comprising MgO 90～
110 parts, MgCl235.5～43.5 parts, H3PO40.5～2 part, 0.5～5 part of styrene-acrylic emulsion.
9. the modified magnesium oxychloride cement according to claim 7 or 8, it is characterised in that count by weight, the cement raw
Material includes 100 parts of MgO, MgCl239.5 parts, H3PO40.5 part, 1 part of styrene-acrylic emulsion.
10. the preparation method of the modified magnesium oxychloride cement as any one of claim 7 to 9, the preparation method include
Following steps：Each raw material of the modified magnesium oxychloride cement is stirred into mixing, molding in proportion.
11. preparation methoies according to claim 10, it is characterised in that the preparation method is comprised the following steps：
(1) by MgCl2The solution that Baume degrees are 24～26 ° of B é is made, then with H3PO4, styrene-acrylic emulsion mixing；
(2) MgO is added to step (1) mixture for obtaining, after forming even slurry, molding, maintenance.
12. preparation methoies according to claim 11, it is characterised in that the modified magnesium oxychloride cement molding is after air
Middle maintenance.
13. preparation methoies according to claim 10 or 11, it is characterised in that the maintenance demoulding afterwards in 24 hours.
14. preparation methoies according to claim 13, it is characterised in that the preparation method is further comprising the steps of：
(3) continue maintenance at least 7 days after the demoulding.
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| CN107434398B (en) * | 2017-07-28 | 2020-07-28 | 中国科学院过程工程研究所 | Cyaniding tailing curing agent and application thereof |
| CN108129044A (en) * | 2018-02-06 | 2018-06-08 | 河北科技大学 | A kind of method for improving magnesia oxychloride cement water resistance |
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| CN1164517A (en) * | 1996-05-02 | 1997-11-12 | 汕头德宝新型建材有限公司 | Magnesium oxychloride cement modified fibre-reinforced material and its process and products |
| CN1178873C (en) * | 2001-01-23 | 2004-12-08 | 董月 | Building decoration material and preparation method thereof |
| CN101822991B (en) * | 2010-03-12 | 2012-05-23 | 山东理工大学 | Preparation process of magnesium-oxy-chloride floating ball loading nanometer Fe<3+>-TiO2 film |
| CN102049812B (en) * | 2010-10-20 | 2012-06-20 | 南昌大学 | Preparation method of high-water resistance magnesite composite material greenhouse supporting frame |
| CN102795803B (en) * | 2012-06-28 | 2014-09-17 | 盐城工学院 | Composite modifier used in magnesium-chlorine cement and application thereof |
| CN103482953B (en) * | 2013-09-27 | 2015-07-15 | 佛山市东鹏陶瓷有限公司 | Artificial synthetic stone and manufacturing method thereof |
| CN104891939B (en) * | 2014-03-03 | 2017-11-28 | 河南理工大学 | A kind of mine timber alternative materials and preparation method |
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