CN103332960B - Method for controlling setting and hardening processes of magnesium phosphate cement - Google Patents
Method for controlling setting and hardening processes of magnesium phosphate cement Download PDFInfo
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- CN103332960B CN103332960B CN201310295608.7A CN201310295608A CN103332960B CN 103332960 B CN103332960 B CN 103332960B CN 201310295608 A CN201310295608 A CN 201310295608A CN 103332960 B CN103332960 B CN 103332960B
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- magnesium phosphate
- phosphate cement
- borax
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- 239000004568 cement Substances 0.000 title claims abstract description 119
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 title claims abstract description 87
- 239000004137 magnesium phosphate Substances 0.000 title claims abstract description 86
- 229910000157 magnesium phosphate Inorganic materials 0.000 title claims abstract description 86
- 229960002261 magnesium phosphate Drugs 0.000 title claims abstract description 86
- 235000010994 magnesium phosphates Nutrition 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000002002 slurry Substances 0.000 claims abstract description 56
- 229910021538 borax Inorganic materials 0.000 claims abstract description 45
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 45
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 79
- 239000000395 magnesium oxide Substances 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000002360 preparation method Methods 0.000 claims description 20
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 239000001095 magnesium carbonate Substances 0.000 claims description 9
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 9
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 9
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims 1
- 235000019796 monopotassium phosphate Nutrition 0.000 claims 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims 1
- 235000019799 monosodium phosphate Nutrition 0.000 claims 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 44
- 230000015271 coagulation Effects 0.000 abstract description 23
- 238000005345 coagulation Methods 0.000 abstract description 23
- 238000011161 development Methods 0.000 abstract description 4
- 238000012423 maintenance Methods 0.000 description 24
- 238000010276 construction Methods 0.000 description 11
- 239000003317 industrial substance Substances 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 230000002940 repellent Effects 0.000 description 6
- 239000005871 repellent Substances 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 3
- 238000010669 acid-base reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000003016 phosphoric acids Chemical class 0.000 description 2
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910000400 magnesium phosphate tribasic Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940045641 monobasic sodium phosphate Drugs 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229940093916 potassium phosphate Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
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Abstract
本发明涉及一种控制磷酸镁水泥凝结和硬化过程的方法。本方法通过提高硼砂缓凝剂的加入量以降低磷酸镁水泥的放热速度，从而延缓磷酸镁水泥浆体的凝结时间，有效调节浆体的凝结时间在20~150分钟范围内；然后，通过提高浆体早期的环境温度加速浆体与环境之间的传热过程和浆体自身的凝结硬化过程，使早期强度得以快速形成，1小时强度达到20～30MPa。该方法一定程度上解决了磷酸镁水泥作为快速修补材料应用于修补工程时凝结时间不够长和硼砂缓凝剂掺量较大造成磷酸镁水泥体系早期强度发展缓慢等问题。已有测试结果表明，该方法能方便、有效地控制磷酸镁水泥凝结和硬化过程。The invention relates to a method for controlling the setting and hardening process of magnesium phosphate cement. This method reduces the exothermic speed of magnesium phosphate cement by increasing the addition of borax retarder, thereby delaying the setting time of magnesium phosphate cement slurry, effectively adjusting the setting time of slurry within the range of 20 to 150 minutes; then, by Raising the early ambient temperature of the slurry accelerates the heat transfer process between the slurry and the environment and the coagulation and hardening process of the slurry itself, so that the early strength can be formed rapidly, and the strength can reach 20-30MPa in one hour. To a certain extent, this method solves the problems that the setting time of magnesium phosphate cement is not long enough and the amount of borax retarder is too large when the magnesium phosphate cement is used as a rapid repair material in the repair project, which leads to the slow development of the early strength of the magnesium phosphate cement system. Existing test results show that this method can conveniently and effectively control the setting and hardening process of magnesium phosphate cement.
Description
Technical field
The present invention relates to magnesium phosphate cement field, especially a kind of control condensed in magnesium phosphate cement construction and the method for process of setting.
Background technology
The features such as magnesium phosphate cement has soon firmly, morning is strong, are particularly suitable for the isostructural Rapid-Repair of concrete road surface and industrial premises.Because magnesium phosphate cement condenses very soon, in order to meet the required operating time of different construction conditions, in the trimagnesium phosphate system of being everlasting, mix retardant, as borax, boric acid etc.; But when retardant volume is few, retarding effect is limited, and while being no more than 5% as retardant borax volume, the presetting period of magnesium phosphate cement slurry is no more than at most 15 minutes; And retardant volume is when large, magnesium phosphate cement slurry early strength slower development, as after retardant borax volume exceedes 10%, magnesium phosphate cement did not almost have intensity at 1 hour, and 3 hours intensity is about 10MPa, and even later strength also has certain reduction.Magnesium phosphate cement, as a kind of patching material, will inevitably be faced with the impact of varying environment factor, and wherein ambient temperature effect is the most extensive.Current status quo shows, the setting and harden of magnesium phosphate cement slurry is subject to the impact of envrionment temperature (or slurry internal temperature) remarkable.If constant retardant borax volume is 5%, in the time that envrionment temperature is 5 DEG C, magnesium phosphate cement slurry is greater than 15 minutes time of coagulation, but 3 hours undercapacity 5MPa; In the time that envrionment temperature is increased to 35 DEG C, although 1 hour intensity can reach 40MPa, magnesium phosphate cement slurry presetting period less than 5 minutes.In addition, the factor such as magnesian activity and fineness, phosphoric acid salt and magnesian mass ratio all largely affects the setting and harden characteristic of magnesium phosphate cement system.
In actual quick fix engineering, the presetting period of the repairing general requirement magnesium phosphate cement of small area is not early than 15 minutes, if slightly large-area repairing magnesium phosphate cement can be controlled at 20 minutes time of coagulation, more satisfactory, it is longer that more the repairing of big area or volume may need the magnesium phosphate cement presetting period.Apparently, due to low retardant volume magnesium phosphate cement system condense very fast, be difficult to meet practice of construction require.Although develop some new retardant and adopted the technological method such as cooling mixing water, very unobvious to delaying the effect of magnesium phosphate cement slurry time of coagulation.
The most outstanding advantage of magnesium phosphate cement is the high strength of having constructed and even having reached in shorter time for latter initial 1 hour, and general 1 hour ultimate compression strength of repairing work should be able to reach 20MPa, even exceedes 25MPa, and within 3 hours, intensity is not less than 40MPa.In the time that construction process adopts raising retardant volume under cold condition or in order to provide suitable setup time to construction process, magnesium phosphate cement system early strength will decline to a great extent, thereby cannot meet the requirement of repairing work to intensity.
Existing technical measures can ensure that magnesium phosphate cement system can merely meet the requirement of required setup time of construction or hour intensity, but for the contradiction of how coordinating between time of coagulation and the early strength of magnesium phosphate cement system in quick fix engineering, also there is not relevant effective technology method at present.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the technical problem to be solved in the present invention is: be provided a kind of time of coagulation that can extend magnesium phosphate cement, do not reduce the method for early strength simultaneously, to meet the requirement of quick fix engineering; The present invention can make the time of coagulation of magnesium phosphate cement system in wider modification scope, and within 1 hour, intensity forms fast, and later strength is without obvious retraction simultaneously.
In order to solve above-mentioned technical problem, the present invention adopts following technical scheme:
Control that magnesium phosphate cement condenses and the method for process of setting, comprise the steps:
A. the preparation of magnesium phosphate cement slurry
At 15～40 DEG C, the ratio that is 2:1～5:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, add again the borax retardant of dead burned magnesia quality 5～30%, after mixing, add again 10～18% water of above-mentioned three kinds of pulverulent material total masses to stir, obtain magnesium phosphate cement slurry;
B. build
At 15～40 DEG C, the magnesium phosphate cement slurry that step a is made is built, and vibration compacting obtains cement and waters building body, maintenance 5～60 minutes at this temperature;
C. High Temperature Curing
Carry out High Temperature Curing watering building body through step b cement after treatment, adopt the method such as hot compress or irradiation control cement to water building body maintenance 10～60 minutes within the scope of 40～60 DEG C, or maintenance 5～30 minutes within the scope of 60～85 DEG C, maintenance is completed after cement water building body top temperature and reach 50～85 DEG C;
D. natural curing
Remove hot compress or the irradiation thermal source of c step, the cement after c step High Temperature Curing is watered to building body and be placed under natural temperature and continue maintenance.
In described step a, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, add again the borax retardant of dead burned magnesia quality 10～15%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, the better performances of the magnesium phosphate cement slurry obtaining.
In described step a, phosphoric acid salt is the one in potassiumphosphate, primary ammonium phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate; Adopt primary ammonium phosphate as preferably phosphate, this material has the features such as high acidity, low cost, excellent performance.
In described step a, dead burned magnesia is being greater than under 1500 DEG C of conditions after calcining by magnesite, and crushing and grinding is crossed 180～250 eye mesh screens and obtained, and its density is greater than 3.00g/cm
3, specific surface area is greater than 200m
2/ kg; As preferably, after dead burned magnesia is calcined under 1500 DEG C of conditions by magnesite, crushing and grinding is crossed 200 eye mesh screens and is obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg, performance the best; The activity of this dead burned magnesia is lower, can effectively control the condensing process of prepared magnesium phosphate cement, does not affect the mechanical property of magnesium phosphate cement simultaneously.
In described step a, borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 180～250 eye mesh screens when both use; As preferably, when using, borax and primary ammonium phosphate cross 200 screen clothes.
In described step a, when envrionment temperature is within the scope of 15～30 DEG C, the volume of borax is 5～20% of dead burned magnesia quality; When envrionment temperature is within the scope of 30～40 DEG C, the volume of borax is 15～30% of dead burned magnesia quality.As preferred, in the time that envrionment temperature is 15 DEG C, the volume of borax is 10% of dead burned magnesia quality; As preferred, in the time that envrionment temperature is 25 DEG C, the volume of borax is 15% of dead burned magnesia quality.Increase borax volume, make borax effectively cover the surface of dead burned magnesia particle, cause OH in solution
?and Mg
2+concentration significantly reduces, and in system solution, acid-base reaction slows down, and the amount of hydrated product and hydration heat be corresponding minimizing also, and the speed that forms spacial framework slows down, thereby is extended time of coagulation.
In described step c, described hot compress is to adopt the hot-water bottle of 40～85 DEG C to cover cement to build surface; Described irradiation is to adopt incandescence to irradiate cement to build surface.As preferably, the present invention adopts the mode of hot compress to carry out High Temperature Curing, and its equipment is simple and easy to get, processing ease, successful.High Temperature Curing process can impel magnesium phosphate cement to water building body and environmental system generation heat exchange, make its temperature after High Temperature Curing reach 50～85 DEG C, significantly to excite the reactive behavior of the reactants such as dead burned magnesia, simultaneously because the hydration reaction of magnesium phosphate cement is an acid-base neutralisation reaction, in reaction process, can emit a large amount of heat, so High Temperature Curing can be accelerated the hydration reaction speed of magnesium phosphate cement system, early strength is developed rapidly.
The present invention is 5～30% of magnesium oxide quality by the add-on of controlling borax retardant in magnesium phosphate cement, make the time of coagulation of cement within the scope of 20～150 minutes, after completing construction or repairing, carry out High Temperature Curing, the method control cement slurry that adopts hot compress or irradiation maintenance 10～60 minutes at 40～60 DEG C, or curing time was at 5～30 minutes at 60～85 DEG C, make the top temperature of cement slurry after High Temperature Curing reach 50～85 DEG C, impel magnesium phosphate cement slurry and environmental system generation heat exchange, promote the early hydration of magnesium phosphate cement, ensure that cement intensity after 1 hour reaches 20～30MPa, after 3 hours, intensity is higher than 40MPa, and later strength does not significantly decrease, reach magnesium phosphate cement slurry and can ensure that enough construction operable times can meet again the requirement of Rapid-Repair early-strong-fast-hard.
Compared with prior art, the invention has the beneficial effects as follows:
1. at 15 ~ 40 DEG C, improve the consumption of retardant borax to delay the time of coagulation of magnesium phosphate cement system, be 5～30% by the consumption of controlling retardant borax, make the time of coagulation of magnesium phosphate cement slurry in the scope of 20 ~ 150 minutes, solved the problems such as the too fast and preparation of construction deficiency of time of magnesium phosphate cement setting and harden.
2. pass through High Temperature Curing, adopt the mode of hot compress or irradiation to improve the internal temperature of the magnesium phosphate cement after building, effectively promote the sclerosis of magnesium phosphate cement slurry and the formation of early strength, the acid-base reaction of slurry inside was carried out in a large number in the short period of time, thereby form in early days abundant hydrated product and enough large hour intensity, solved magnesium phosphate cement because retardant volume is excessive or curing temperature is difficult to compared with the low early strength that causes the problem developing.
3. the curing temperature by raising borax consumption and after building, effectively control time of coagulation and the process of setting of magnesium phosphate cement, to obtain the time of coagulation and the early strength that meet construction requirement, the longterm strength of magnesium phosphate cement is not had to significant adverse impact simultaneously.
Brief description of the drawings
Fig. 1 is the temperature rise curve of 1# in embodiment, 3# and 5# test specimen.Wherein, the order up and down of test specimen label and label index wire crossing temperature rise curve is sequentially corresponding up and down successively.
Fig. 2 is the temperature rise curve of 2# in embodiment, 4# and 6# time.Wherein, the order up and down of test specimen label and label index wire crossing temperature rise curve is sequentially corresponding up and down successively.
From Fig. 1 and Fig. 2,1# and the temperature of 2# test specimen after High Temperature Curing are greater than 50 DEG C; 3# and 4# test specimen have improved borax volume, and the temperature rise of test specimen is slow, and extend time of coagulation; The borax volume of 5# and 6# test specimen is less, and time-temperature is higher, and time of coagulation is shorter.
Embodiment
In order to verify the experiment effect of this invention, applicant has carried out specific embodiment and has verified beneficial effect of the present invention.When checking, adopt method of the present invention and pedestal method to prepare 6 test specimens.
For 1# and 2# test specimen, adopt method preparation of the present invention, be after cement slurry is built, first be placed under normal temperature maintenance after 40 minutes, move to again at 50 DEG C maintenance 30 minutes, form removal after final set, then be placed in maintenance under normal temperature environment, and the ultimate compression strength of test test specimen 1.5 hours, 3 hours, 1 day, 7 days and 90 days; For 3# and 4# test specimen, wherein the volume of borax retardant is respectively 10% and 15% of magnesium oxide quality, adopts pedestal method preparation, after cement slurry is built, maintenance at normal temperatures again, and the ultimate compression strength of test test specimen 1.5 hours, 3 hours, 1 day, 7 days and 90 days; For 5# and 6# test specimen, wherein the volume of borax retardant is respectively 3% and 5% of magnesium oxide quality, adopts pedestal method preparation, after cement slurry is built, maintenance at normal temperatures again, and the ultimate compression strength of test test specimen 1.5 hours, 3 hours, 1 day, 7 days and 90 days.
the preparation of test specimen 1#
The preparation of test specimen 1# comprises the steps:
A. the preparation of magnesium phosphate cement slurry
At 15 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 10%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. build
At 15 DEG C, prepared step a magnesium phosphate cement slurry to be built, vibration compacting, obtains cement and waters building body, then inserts thermocouple thermometer therein and record temperature, maintenance 40 minutes at this temperature;
C. High Temperature Curing
Carry out High Temperature Curing watering building body through step b cement after treatment, adopt the hot-water bottle of 50 DEG C to cover cement and build surface maintenance 30 minutes, after maintenance completes, cement waters building body top temperature and is greater than 50 DEG C;
D. natural curing
Remove the hot compress thermal source of c step, the cement after c step High Temperature Curing is watered to building body and be placed under natural temperature and continue maintenance 90 days, obtain test specimen 1#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 200 mesh sieves when use.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
the preparation of test specimen 2#
The preparation of test specimen 2# comprises the steps:
A. the preparation of magnesium phosphate cement slurry
At 25 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 15%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. build
At 25 DEG C, prepared step a magnesium phosphate cement slurry to be built, vibration compacting, obtains cement and waters building body, then inserts thermocouple thermometer therein and record slurry temperature, maintenance 40 minutes at this temperature;
C. High Temperature Curing
Carry out High Temperature Curing watering building body through step b cement after treatment, adopt the hot-water bottle of 50 DEG C to cover cement and build surface maintenance 30 minutes, after maintenance completes, cement waters building body top temperature and is greater than 50 DEG C;
D. natural curing
Remove the hot compress thermal source of c step, the cement after c step High Temperature Curing is watered to building body and be placed under natural temperature and continue maintenance 90 days, obtain test specimen 2#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 200 mesh sieves when use.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
the preparation of test specimen 3#
The preparation of test specimen 3# comprises the steps:
A. at 15 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 10%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. after the magnesium phosphate cement slurry of being prepared by step a is built, then be placed under normal temperature maintenance 90 days, obtain test specimen 3#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Levigate mistake 200 mesh sieves when borax and primary ammonium phosphate are the two use of technical grade industrial chemicals.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
the preparation of test specimen 4#
The preparation of test specimen 4# comprises the steps:
A. at 25 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 15%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. after the magnesium phosphate cement slurry of being prepared by step a is built, then be placed under normal temperature maintenance 90 days, obtain test specimen 4#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 200 mesh sieves when the two uses.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
the preparation of test specimen 5#
The preparation of test specimen 5# comprises the steps:
A. at 15 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 3%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. after the magnesium phosphate cement slurry of being prepared by step a is built, then be placed under normal temperature maintenance 90 days, obtain test specimen 5#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 200 mesh sieves when use.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
the preparation of test specimen 6#
The preparation of test specimen 6# comprises the steps:
A. at 25 DEG C, the ratio that is 4:1 according to dead burned magnesia and phosphatic mass ratio is prepared burden, then adds the borax retardant of dead burned magnesia quality 5%, after mixing, add again 13% water of above-mentioned three kinds of pulverulent material total masses to stir, make magnesium phosphate cement slurry;
B. after the magnesium phosphate cement slurry of being prepared by step a is built, then be placed under normal temperature maintenance 90 days, make test specimen 6#.
In described step a, the dead burned magnesia in batching is by magnesite after 1500 DEG C of calcinings, and crushing and grinding is crossed 200 eye mesh screens and obtained, and its density is 3.42g/cm
3, specific surface area is 230m
2/ kg; Borax and primary ammonium phosphate are technical grade industrial chemicals, levigate mistake 200 mesh sieves when the two uses.
In described step b, adopt 25mm*25mm*25mm steel die while building, its bottom and surrounding have been done WATER REPELLENT.
experimental result
Because magnesium phosphate cement slurry is first, final setting time interval is little, therefore using the time of coagulation of presetting period as magnesium phosphate cement slurry.Due to the needs of contrast, pour into a mould and after 40 minutes, improve again temperature maintenance and exceeded 1 hour in 30 minutes, the therefore unified intensity of having measured 1.5 hours of test specimen 1#, 2#, other test specimens are measured 1 hour intensity, do not affect like this 3 hours strength ratios before.Because temperature is remarkable on experimental result impact, therefore measure the internal temperature of magnesium phosphate cement slurry before 5 hours, to control experimentation.The mensuration of time of coagulation is measured with reference to " cement normal consistency water consumption, time of coagulation, the stability method of inspection " (GB/T 1346-2011), and test result is as shown in table 1; Intensity (GB/T17671-1999) is measured according to " cement strength testing method ", and test result is as shown in table 1.
Table 1
From table 1, Fig. 1 and Fig. 2, for 1# and 2# test specimen, adopt method of the present invention, increase borax volume, make the time of coagulation of magnesium phosphate cement slurry in 20～150 minutes, adopt again the temperature of High Temperature Curing control magnesium phosphate cement slurry to reach more than 55 DEG C, make the development of magnesium phosphate cement slurry early strength very fast, 1.5 hours and 3 hours intensity respectively can 30MPa and more than 40MPa, later strength does not have obvious retraction, avoid the disadvantageous effect of high volume borax retardant to system intensity, can meet the requirement of quick fix engineering; For 3# and 4# test specimen, improve the volume of borax retardant, the temperature rise of magnesium phosphate cement slurry is slow, extend the time of coagulation of magnesium phosphate cement slurry, but early strength significantly reduces, within 3 hours, intensity is only 11.7MPa, and even later strength also has certain decline, can not meet the requirement of quick fix engineering; For 5# and 6# test specimen, borax volume is lower, the temperature of magnesium phosphate cement slurry is higher, all show higher intensity each length of time, early strength is particularly evident, and 1 hour and 3 hours intensity can reach respectively 30MPa and 70MPa, but the time of coagulation of magnesium phosphate cement slurry is too short, improve enough setup times cannot to the construction of Practical Project, can not meet the requirement of quick fix engineering.
In sum, temperature and retardant have important impact to the time of coagulation of magnesium phosphate cement, and temperature is higher, and slurry condenses faster, and raising retardant volume can delay the hydration process of magnesium phosphate cement system; Raising precuring temperature can effectively promote the development of the early strength of magnesium phosphate cement system, can largely make up the negative impact that high volume retardant causes system intensity.The present invention effectively controls time of coagulation and the process of setting of magnesium phosphate cement by improving retardant volume and precuring temperature, make it meet the requirement of quick fix engineering.
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| US20160304396A1 (en) * | 2015-04-16 | 2016-10-20 | Premier Magnesia, Llc | Magnesium-based cements and slurry precursors for the same |
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| FR3105215B1 (en) * | 2019-12-20 | 2022-01-14 | Orano Cycle | Thiosulphates for use as set retarders in phosphomagnesium cement pastes |
| CN111056757B (en) * | 2019-12-30 | 2021-12-07 | 杭州修路人科技股份有限公司 | Quick-hardening cement prepared from waste residues and preparation method thereof |
| CN111592328B (en) * | 2020-06-15 | 2022-03-08 | 重庆安淮科技有限公司 | Double-liquid magnesium phosphate material and preparation method thereof |
| CN111847936B (en) * | 2020-06-30 | 2022-03-18 | 重庆纽镁特科技有限公司 | Phosphate cement and preparation method thereof |
| CN112062537B (en) * | 2020-07-17 | 2022-06-03 | 武汉理工大学 | A kind of fast-setting impact-resistant composite sheet and preparation method thereof |
| CN113213884B (en) * | 2021-05-26 | 2023-01-13 | 天应(深圳)生态建材科技有限公司 | Green magnesium-based cement additive for 3D printing and application thereof |
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