CN104909602A - 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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- CN104909602A CN104909602A CN201510290353.4A CN201510290353A CN104909602A CN 104909602 A CN104909602 A CN 104909602A CN 201510290353 A CN201510290353 A CN 201510290353A CN 104909602 A CN104909602 A CN 104909602A
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- benzene emulsion
- correcting agent
- properties
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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, be specifically related to a kind of properties-correcting agent for magnesia oxychloride cement and its production and use.
Background technology
Magnesium oxychloride cementing material (magnesium oxychloride cement, MOC) MgO-MgCl
2-H
2the important inorganic gel system of O composition, because material strength losses is large after its poor water resistance, water suction, makes it be very limited in engineer applied.Actual from current research, although there has been proposed many active measures and obtain good effect, magnesium oxychloride cementing material water resistance problem is solved not yet at all; Phosphoric acid and soluble phosphate are current for improving the mainly material modified of magnesium oxychloride cementing material water repelling property, but phosphoric acid is huge to cement retardative effect, can cause cement early strength degradation; Investigator is had to attempt in magnesia oxychloride cement hardenite, to form waterresistant polymeric protective membrane by mixing emulsion polymerization; cover aquation its surface; fill hardenite hole, thus improve the water resistance of magnesium oxychloride cementing material, but test proving effect is not good mostly.The author, in the emulsion modified magnesia oxychloride cement water resistant test of the use multiple polymers such as phenylpropyl alcohol, butylbenzene, finds that most of high molecular polymer does not almost have modified effect, even reduces the original water-fast and mechanical property of system.
The present invention intends on the basis of the single modification of the polymkeric substance such as phosphoric acid and phenylpropyl alcohol, adopts phosphoric acid and benzene emulsion to carry out compound water resistance modified test to magnesia oxychloride cement, and research phosphoric acid/polymkeric substance compound improves the effect of magnesia oxychloride cement water resistance.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art part, the present invention is by the basis of phosphoric acid, the single study on the modification of benzene emulsion difference, employing phosphoric acid, benzene emulsion carry out composite modified to magnesia oxychloride cement, maximize favourable factors and minimize unfavourable ones, to playing the best effects of properties-correcting agent of the present invention, find out the optimal path improving water resistance, the New Building Materials that final acquisition is good.
First object of the present invention is to provide a kind of properties-correcting agent for magnesia oxychloride cement;
Second object of the present invention is to provide a kind of above-mentioned properties-correcting agent and is preparing the purposes in modified magnesium oxychloride cement;
3rd object of the present invention is to provide a kind of modified magnesium oxychloride cement;
4th 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:
For a properties-correcting agent for magnesia oxychloride cement, described properties-correcting agent comprises H
3pO
4and/or benzene emulsion; Preferably, described properties-correcting agent is by H
3pO
4form with benzene emulsion; More preferably, described H
3pO
4for liquid.
Described properties-correcting agent is by H
3pO
4with benzene emulsion composition, wherein, count by weight, H in described properties-correcting agent
3pO
40.5 ~ 2 part, benzene emulsion 0.5 ~ 5 part; Preferably, H in described properties-correcting agent
3pO
4it is 0.5 part or 1 part; Preferably, described benzene emulsion is 1 part or 4 parts.
Described properties-correcting agent is by H
3pO
4with benzene emulsion composition, wherein, count by weight, H in described properties-correcting agent
3pO
40.5 part, benzene emulsion 1 part.
The purposes in modified magnesium oxychloride cement prepared by properties-correcting agent of the present invention.
A kind of modified magnesium oxychloride cement, described cement adopts properties-correcting agent of the present invention and MgO, MgCl
2be prepared.
The raw material packet of described cement is containing MgO 90 ~ 110 parts, MgCl
235.5 ~ 43.5 parts, H
3pO
40.5 ~ 2 part, benzene emulsion 0.5 ~ 5 part; Preferably, count by weight, described cement raw material comprises MgO 100 parts, MgCl
2, 39.5 parts, H
3pO
40.5 part, benzene emulsion 1 part.
Described preparation method comprises the following steps: be uniformly mixed in proportion by each raw material of described modified magnesium oxychloride cement, shaping;
Preferably, described preparation method comprises the following steps:
(1) by MgCl
2make the solution that degree Beaume is 24 ~ 26 ° of B é, then with H
3pO
4, benzene emulsion mixing;
(2) MgO is added to the mixture that step (1) obtains, after forming even slurry, shaping, maintenance;
Preferably, described modified magnesium oxychloride cement shaping after maintenance in air; More preferably, maintenance is the demoulding afterwards in 24 hours;
Preferably, described preparation method is further comprising the steps of:
(4) maintenance at least 7 days is continued after the demoulding.
The present invention is described as follows:
In order to verify that in properties-correcting agent provided by the invention, each component is to the effect of magnesia oxychloride cement water tolerance, carry out following research.
1, H is tested
3
pO
4
with benzene emulsion respectively as single properties-correcting agent to magnesia oxychloride cement water tolerance
the impact of energy
Starting material and reagent:
The light-burning magnesium powder in Yingkou, Liaoning, Yancheng Xiangshui County halogen sheet, industrial phosphoric acid liquid, benzene emulsion.
Plant and instrument:
SJD-30 type concrete mixer, SHBY-40A type cement standard maintaining box, 101A-3B type electric drying oven with forced convection, electronic balance, YAW-300B type pressure testing machine, QANTA-200 type scanning electronic microscope.
Test method:
The preparation of magnesia oxychloride cement matrix: the benchmark proportioning adopted in process of the test is MgO: MgCl
2=6: 1 (mol ratio), MgCl
2adopt solution form to prepare cement matrix, the degree Beaume (° B é) of this solution should control 24 ~ 26.By the light-burned MgO powder, the MgCl that weigh in advance and prepare
2solution and properties-correcting agent to be tested are poured in concrete mixer and are stirred (liquid modifier and MgCl
2solution mixes, add MgO again), after forming even slurry, pour 100mm × 100mm × 100mm die for molding into, the demoulding after natural curing 24h in atmosphere, respectively maintenance 3 days and 7 days, after 7 days soaked 7 days, test its ultimate compression strength respectively in these three cases, the method specified according to GB/T17671-1999 " Test method for strength of hydraulic cement mortar (ISO method) " standard is tested.
Sample after resistance to compression is used for SEM and XRD analysis.
Coefficient of softening all carries out with reference to measuring method in JG/T 1169-2005 " light lath for building partition wall ".Coefficient of softening I=R1/R0, in formula: R1 is maintenance ultimate compression strength mean value of soaked 7 days again after 7 days, and R0 is the ultimate compression strength mean value of maintenance after 7 days under absolute dry condition.
Blank testing sample simultaneously, for not adding the magnesia oxychloride cement of properties-correcting agent of the present invention.
Ultimate compression strength and the coefficient of softening result of different larval instar, different addition quantity (mass percent of properties-correcting agent and MgO powder) modified magnesium oxychloride cement are as follows:
(1) H of magnesia oxychloride cement
3pO
4modified effect is tested
The phosphoric acid choosing 0.5%, 1%, 1.5%, 2% volume respectively carries out modification to magnesia oxychloride cement, and the modified effect of different addition quantity is as shown in table 1.
Table 1: phosphoric acid is to the modified effect of magnesia oxychloride cement
As can be seen from Table 1, along with the increase of phosphoric acid volume, the coefficient of softening of magnesia oxychloride cement improves thereupon, and water tolerance significantly strengthens, but the early anti pressured intension of cement declines rapidly thereupon, shows that phosphoric acid is to MgO-MgCl
2-H
2o system gelling material has obvious delayed coagulation.When volume phosphoric acid is 2%, the coefficient of softening of cement reaches 0.81, but 3 days ultimate compression strength is only 42.3MPa, and more blank sample have dropped 29.3Mpa.
The water tolerance that phosphoric acid can improve magnesia oxychloride cement system is because phosphoric acid and hydrated product react, and defines fine and close indissoluble trimagnesium phosphate protective membrane on hydrated product surface; Phosphoric acid add the surface topography that simultaneously have also been changed hydrated product crystalline phase, make sturdy 5Mg (OH)
2mgCl
28H
2o phase styloid becomes elongated and round and smooth bar-shaped, thus causes cement strength to decline, and phosphoric acid mixes the SEM figure of front and back magnesia oxychloride cement sample respectively as shown in Fig. 1 (a) He (b).
(2) the Modification of Styrene-Acrylate Emulsion measure of merit of magnesia oxychloride cement
The benzene emulsion choosing 0.5%, 1%, 2%, 3%, 5% volume respectively carries out modification to magnesia oxychloride cement, and the modified effect of different addition quantity is as shown in table 2.
Table 2: benzene emulsion is to the modified effect of magnesia oxychloride cement
As shown in table 2, benzene emulsion does not almost have modified effect, even reduces the original water-fast and mechanical property of system.Analyze its major cause, polymkeric substance and the poor binding property of hydrated product cause it can not form the water-fast protective membrane of effectively densification on hydrated product crystalline phase surface, can not be formed and disperse preferably and sprawl in hydrated product structural system.
2, H is tested
3
pO
4
with the combination of benzene emulsion on the impact of magnesia oxychloride cement water resistance
Adopt 0.5% phosphoric acid and 1% benzene emulsion, 1% phosphoric acid and 1% benzene emulsion, 1% phosphoric acid and 4% benzene emulsion to carry out composite modified to magnesia oxychloride cement respectively, modified effect is as shown in table 3.
Table 3: phosphoric acid and benzene emulsion are to the modified effect of magnesia oxychloride cement
From table 3, the compound of appropriate phosphoric acid and benzene emulsion is not only better than independent admixture benzene emulsion to the modified effect of magnesia oxychloride cement water tolerance, and being much better than independent admixture phosphoric acid, coefficient of softening close to 1, and overcomes the defect of phosphoric acid modification slow setting and early strength decline.But under the existence of appropriate phosphoric acid, the consumption increasing benzene emulsion is not The more the better; Water tolerance when admixture 0.5% phosphoric acid and 1% benzene emulsion carry out composite modified is best.Phosphoric acid and benzene emulsion compound make magnesia oxychloride cement have better water resistance to show; the interaction of phosphoric acid and benzene emulsion changes the bonding properties on benzene emulsion and hydrated product surface; facilitate the adhesion of polymeric film on hydrated product surface and covering, this is because define the water-fast protective layer of compound on the basis of original phosphatize phosphate coat.
Conclusion
(1) single phosphoric acid can improve the water resistance of magnesia oxychloride cement system, but has obvious delayed coagulation to cement, and the early anti pressured intension of cement is declined.
(2) water resistance of single phenylpropyl alcohol emulsion polymerization to magnesia oxychloride cement does not have obvious modified effect, even reduces the original water-fast and mechanical property of cement.
(3) appropriate benzene emulsion and phosphoric acid compound, be not only better than singly mixing polymer emulsion to magnesia oxychloride cement water tolerance modified effect, and be much better than singly to mix phosphoric acid, and overcome the defect of phosphoric acid slow setting and early strength decline.According to the specific embodiment of the present invention, properties-correcting agent for the preparation of modified magnesium oxychloride cement provided by the invention can make the water tolerance of cement and early strength be significantly increased, the early strength of maintenance after 3 days and 7 days can reach 64.1Mpa and 75.8Mpa respectively, and coefficient of softening reaches 0.99, maintenance after 7 days the more soaked intensity of soaked 7 days up to 68.9MPa.
Accompanying drawing explanation
The cross-section morphology SEM that Fig. 1 (a) is magnesia oxychloride cement blank sample schemes;
The modified magnesium oxychloride cement matrix sample section pattern SEM that Fig. 1 (b) is the phosphoric acid of 1% for volume schemes.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, the embodiment provided only in order to illustrate the present invention, instead of in order to limit the scope of the invention.
Experimental technique in following embodiment, if no special instructions, is ordinary method.Test materials used in following embodiment, if no special instructions, is and purchases available from routine biochemistry reagent shop.
Be below each embodiment starting material and test method:
Starting material and reagent:
The light-burning magnesium powder in Yingkou, Liaoning, Yancheng Xiangshui County halogen sheet, industrial phosphoric acid liquid, benzene emulsion.
Plant and instrument:
SJD-30 type concrete mixer, SHBY-40A type cement standard maintaining box, 101A-3B type electric drying oven with forced convection, electronic balance, YAW-300B type pressure testing machine, QANTA-200 type scanning electronic microscope.
The method that ultimate compression strength specifies according to GB/T17671-1999 " Test method for strength of hydraulic cement mortar (ISO method) " standard is tested.Coefficient of softening all carries out with reference to measuring method in JG/T 1169-2005 " light lath for building partition wall ".Coefficient of softening I=R1/R0, in formula: R1 is maintenance ultimate compression strength mean value of soaked 7 days again after 7 days, and R0 is the ultimate compression strength mean value of maintenance after 7 days under absolute dry condition.
embodiment 1: the preparation of modified magnesium oxychloride cement of the present invention
Raw material: count by weight, H
3pO
40.5 part, benzene emulsion 0.5 part, MgO powder 90 parts, MgCl
235.5 parts.
Preparation and test: by MgCl
2make the solution that degree Beaume is 24 ~ 26 ° of B é, then with H
3pO
4, benzene emulsion mixing; MgO and this mixture are poured in concrete mixer and stirs, formed after even slurry, pour 100mm × 100mm × 100mm die for molding into, in atmosphere the natural curing 24h demoulding, respectively maintenance 3 days and 7 days, after 7 days soaked 7 days.Test 3 days, 7 days and ultimate compression strength again after soaked 7 days, and test coefficient of softening.
embodiment 2: the preparation of modified magnesium oxychloride cement of the present invention
Raw material: count by weight, H
3pO
42 parts, benzene emulsion 5 parts, MgO powder 110 parts, MgCl
243.5 parts.
Preparation and test are with embodiment 1.
embodiment 3: the preparation of modified magnesium oxychloride cement of the present invention
Raw material: count by weight, H
3pO
40.5 part, benzene emulsion 1 part, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
embodiment 4: the preparation of modified magnesium oxychloride cement of the present invention
Raw material: count by weight, H
3pO
41 part, benzene emulsion 4 parts, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
embodiment 5: the preparation of modified magnesium oxychloride cement of the present invention
Raw material: count by weight, H
3pO
41 part, benzene emulsion 1 part, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
comparative example 1: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
40.3 part, benzene emulsion 0.3 part, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
comparative example 2: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
40.1 part, benzene emulsion 0.2 part, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
comparative example 3: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
43 parts, benzene emulsion 6 parts, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
comparative example 4: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
45 parts, benzene emulsion 8 parts, MgO powder 100 parts, MgCl
239.5 parts.
Preparation and test are with embodiment 1.
comparative example 5: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
42 parts, 50 parts, flyash, benzene emulsion 13 parts, MgO powder 100 parts, NF high efficiency water reducing agent 1 part, degree Beaume is the MgCl of 25
2solution 40 parts, 50 parts, water.
Modified magnesium oxychloride cement is prepared according to the method for patent application CN201210216756.0 embodiment 4.
comparative example 6: the preparation of modified magnesium oxychloride cement
Raw material: count by weight, H
3pO
42.8 parts, 52 parts, flyash, benzene emulsion 14.1 parts, MgO powder 100 parts, NF high efficiency water reducing agent 1.5 parts, degree Beaume is the MgCl of 30
2solution 39.1 parts, 45.7 parts, water.
Modified magnesium oxychloride cement is prepared according to the method for patent application CN201210216756.0 embodiment 4.
The modified magnesium oxychloride cement water resistance contrast that in the present invention prepared by each embodiment and comparative example sees the following form 4.
Table 4: modified magnesium oxychloride cement water resistance contrast (with weight parts) prepared by various embodiments of the present invention
Conclusion: phosphoric acid and benzene emulsion have very large lifting to the composite modified effect of magnesia oxychloride cement, properties-correcting agent of the present invention, and it is counted by weight, works as H
3pO
40.5 part, benzene emulsion 1 part time composite modified most pronounced effects.
Claims (7)
1., for a properties-correcting agent for magnesia oxychloride cement, described properties-correcting agent comprises H
3pO
4and/or benzene emulsion; Preferably, described properties-correcting agent is by H
3pO
4form with benzene emulsion; More preferably, described H
3pO
4for liquid.
2. properties-correcting agent according to claim 1, is characterized in that, described properties-correcting agent is by H
3pO
4with benzene emulsion composition, wherein, count by weight, H in described properties-correcting agent
3pO
40.5 ~ 2 part, benzene emulsion 0.5 ~ 5 part; Preferably, H in described properties-correcting agent
3pO
4it is 0.5 part or 1 part; Preferably, described benzene emulsion is 1 part or 4 parts.
3. properties-correcting agent according to claim 1 and 2, is characterized in that, described properties-correcting agent is by H
3pO
4with benzene emulsion composition, wherein, count by weight, H in described properties-correcting agent
3pO
40.5 part, benzene emulsion 1 part.
4. the purposes in modified magnesium oxychloride cement prepared by properties-correcting agent as claimed any one in claims 1 to 3.
5. a modified magnesium oxychloride cement, is characterized in that, described cement adopts properties-correcting agent as claimed any one in claims 1 to 3 and MgO, MgCl
2be prepared.
6. modified magnesium oxychloride cement according to claim 5, is characterized in that, the raw material packet of described cement is containing MgO 90 ~ 110 parts, MgCl
235.5 ~ 43.5 parts, H
3pO
40.5 ~ 2 part, benzene emulsion 0.5 ~ 5 part; Preferably, count by weight, described cement raw material comprises MgO 100 parts, MgCl
239.5 parts, H
3pO
40.5 part, benzene emulsion 1 part.
7. the preparation method of the modified magnesium oxychloride cement according to any one of claim 5 to 6, described preparation method comprises the following steps: be uniformly mixed in proportion by each raw material of described modified magnesium oxychloride cement, shaping;
Preferably, described preparation method comprises the following steps:
(1) by MgCl
2make the solution that degree Beaume is 24 ~ 26 ° of B é, then with H
3pO
4, benzene emulsion mixing;
(2) MgO is added to the mixture that step (1) obtains, after forming even slurry, shaping, maintenance;
Preferably, described modified magnesium oxychloride cement shaping after maintenance in air; More preferably, maintenance is the demoulding afterwards in 24 hours;
Preferably, described preparation method is further comprising the steps of:
(4) maintenance at least 7 days is continued after the demoulding.
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|---|---|---|---|
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|---|---|---|---|
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| CN107434398A (en) * | 2017-07-28 | 2017-12-05 | 中国科学院过程工程研究所 | A kind of cyanidation tailings curing agent and its application |
| 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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| CN104909602B (en) | 2017-05-03 |
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