CN104844106A - A3.5 B05 grade autoclaved aerated concrete block made of quartz weathered sand, and making method thereof - Google Patents
A3.5 B05 grade autoclaved aerated concrete block made of quartz weathered sand, and making method thereof Download PDFInfo
- Publication number
- CN104844106A CN104844106A CN201510156468.4A CN201510156468A CN104844106A CN 104844106 A CN104844106 A CN 104844106A CN 201510156468 A CN201510156468 A CN 201510156468A CN 104844106 A CN104844106 A CN 104844106A
- Authority
- CN
- China
- Prior art keywords
- autoclave
- water
- base substrate
- cement
- weathered sand
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/10—Lime cements or magnesium oxide cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/02—Selection of the hardening environment
- C04B40/024—Steam hardening, e.g. in an autoclave
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides an A3.5 B05 grade autoclaved aerated concrete block made of quartz weathered sand. The high-performance A3.5 B05 grade autoclaved aerated concrete block is made by using the quartz weathered sand, cement, quicklime, industrial waste phosphogypsum, aluminum powder paste and water as raw materials. The dry density of the block is 509kg/m<3>, the average cubic compressive strength of the block is 3.6MPa, the single component minimum of the block is 3.2Mpa, the split-to-compression ratio is 0.20, the mass loss after freezing is 2.8%, the strength after freezing is 3.1Mpa, the heat conduction coefficient (dry state) is 0.1251W/(m.K), the drying shrinkage value (standard process) is 0.32mm/m, and the qualified rate is greater than 98%. The method has the advantages of reasonable treatment of raw materials, scientific formula calculation, concise production flow, recycling of production wastes. The block is a novel energy saving and environmental protection wall material, and can be industrially produced.
Description
Technical field
The present invention relates to A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand and preparation method thereof, belong to novel energy-saving environment-friendly materials for wall field.
Background technology
Quartz Weathered Sand, be that natural quartz is formed after weathering in millions upon millions of years, its former crystal habit transforms, and becomes tiny crystal grain, and portions turn is noncrystal, and major ingredient is silicon-dioxide (SiO
2), containing small amounts aluminium (Al
2o
3), potassium oxide (K
2o), ferric oxide (Fe
2o
3) and calcium oxide (CaO).Quartz Weathered Sand is to provide SiO at autoclave aerated concrete building block production process Main Function
2, its mineral constituent is complicated, and what content was maximum is quartz, is secondly feldspar, is also mingled with mica, carbonate, clay etc., the Na wherein also containing some amount
2o and K
2o, they generate solubility Na
2sO
4and K
2sO
4.
The clay impurity contained in quartz Weathered Sand is very large on the impact of autoclave aerated concrete building block performance: on the one hand, because clay is a kind of high dispersive material, water-absorbent is strong, during too high levels, phosphoric acid can be made to increase, if the viscosity that guarantee is certain and increase water consumption, then extend again base substrate setting time; On the other hand, a certain amount of Al is contained in clay
2o
3, it promotes the generation of steam-pressing aero-concrete hydrated product tobermorite (tobermorite) phase.
Tobermorite is the laminate structure that silicon-oxy tetrahedron strand and calcium oxide polyhedron are formed, and containing moisture between laminate structure, middle water is unstable, and very easily dehydration causes volumetric shrinkage to be out of shape.In order to obtain the excellent aerated concrete products of stable performance, must be controlled tobermorite.
At present, along with the fast development of steam pressure sand aerated concrete block industry Technology and equipment, the ability producing B06, B07 level autoclaved aerated building block in enormous quantities has become ripe.But can suit measures to local conditions, produce A2.0 B04 in conjunction with local physical condition qualification rate in enormous quantities, high, the building block of A3.5 B05 level steam pressurized coagulation, the building materials enterprise of thin piece are little.The Major Difficulties of production A2.0 B04, A3.5 B05 level autoclave aerated concrete building block is, while reduction product unit weight, ensures product strength again.The quality of B04, B05 level steam pressurized foam concrete quality directly affects the cold-heat bridge position isothermal holding such as self heat insulation wall and beams of concrete, post and shear wall.
Summary of the invention
The object of this invention is to provide the quartzy Weathered Sand of a kind of employing and prepare A3.5 B05 level steam pressure sand aerated concrete block.By strictly controlling each raw material quality, adjustment proportioning and accurate measurement, improve processing method, improve the stability of base substrate, ensure that steam pressure sand aerated concrete block air hole structure is good, unit weight is low, intensity is high, thermal conductivity and drying shrinkage value is low, frost resistance is good.
For achieving the above object, the present invention adopts following technical scheme:
A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand, this concrete segment comprises the dry material composition of following weight part: quartzy Weathered Sand 55-70 part, cement 12-30 part, unslaked lime 10-28 part, aluminium powder cream 0.10-0.13 part, phosphogypsum 3-6 part; Wherein, the dry material component of this concrete segment also comprises water, and the mass ratio of water and dry material is 0.67-0.72:1.
The dry material of above-mentioned concrete segment more preferably comprises the dry material composition of following weight part: quartzy Weathered Sand 62.4 parts, cement 19.5 parts, unslaked lime 13.6 parts, aluminium powder cream 0.12 part, phosphogypsum 4.38 parts; Wherein, the dry material component of this concrete segment also comprises water, and the mass ratio of water and dry material is 0.68:1.
The present invention also provides a kind of quartzy Weathered Sand to prepare the method for A3.5 B05 level autoclave aerated concrete building block, comprises following preparation process:
1) by quartzy Weathered Sand and phosphogypsum by weight after mix, being delivered to ball mill, is that 7:1 adds ball mill by water, useless slurry with throughput ratio, mix grinding 10-30min, obtains that fineness is 25-28%, mass percent concentration is the slip of 58-65%; Pulverize and ball milling unslaked lime, obtain the calcium lime powder that fineness is 10%-13%; Be that 8-10:1 mix with aluminium powder cream with mass ratio by water, stir and obtain aluminium paste;
2) by cement, calcium lime powder, slip, water adds in stirred pot, mixing, stir 25-35s, employing 0.3-0.4MPa is steam heated to 30-35 DEG C, stop heating, aluminium paste is added in stirred pot, after continuing to stir 35-40s, slip in stirred pot is discharged into framed in, and be quiet in the precuring of 48-52 DEG C stopping by framed room temperature of sending to, slip is in framed interior expansion, stable base substrate is formed after 40-48min, base substrate is without sinking, subside, the phenomenon such as bubbling and bleeding, continue to rest after 170-190min and cut, remove the scrap stock after base substrate cutting, base substrate is sent in autoclave,
3) by distribution system, steam press maintenance is carried out to the base substrate in still, base substrate in autoclave successively through vacuumizing, boosting, obtain A3.5 B05 level autoclave aerated concrete building block after constant voltage and step-down.
In described step 1), described fineness for dry material through 180 order standard inspection sieves screen over-size shared by mass percent.
In described step 1), described useless slurry is step 2) in base substrate cutting after scrap stock enter recirculated water after, through stir formed density be 1.2-1.3g/cm
3mixture, the main component of this mixture comprises calcium hydroxide, the hydrated calcium silicate that in silicon-dioxide, lime and the cement that water, quartzy Weathered Sand and cement provides, calcium oxide hydration reaction is formed.
Described step 2) in, cement, calcium lime powder, slip, water adds in stirred pot, mixing, stir 30s, employing 0.35MPa is steam heated to 31 DEG C, stop heating, aluminium paste is added in stirred pot, after continuing to stir 40s, slip in stirred pot is discharged into framed in, be quiet in the precuring of 50 DEG C stopping by framed room temperature of sending to, slip is got angry in framed expansion, stable base substrate is formed after 45min, base substrate is without sinking, subside, the wild effect such as bubbling and bleeding, continue to rest after 185min and cut, remove the scrap stock after base substrate cutting, base substrate is sent in autoclave.
In described step 3), after vacuumizing in autoclave, autoclave internal pressure is-0.03MPa; Again to delivering vapor in autoclave, in 10-15min, rise to 0MPa; Continue boosting, in 50-70min, rise to 0.45MPa; Further boosting, rises to 0.8MPa in 25-35min; Again boost, in 25-35min, rise to 1.32MPa; In autoclave, supplement steam in time, keep still internal pressure to be 1.31-1.33MPa, maintain 6-7h; Then be vented step-down, in 25-35min, be depressurized to 1.0MPa; Further exhaust step-down, is depressurized to 0.65MPa in 25-35min; Continue exhaust step-down, autoclave internal pressure is down to normal pressure.
Above-mentioned middle cement is PO 42.5 ordinary Portland cement, this silicate cement reacts rapidly mainly meet water in the preparation of concrete segment after, produce a large amount of hydrated calcium silicate gels, phosphoric acid increases guarantee pouring stability rapidly, base substrate is formed afterwards and accelerates the sclerosis of base substrate, is conducive to cutting.Cement is also the supplier of CaO simultaneously.
The digestion rate of unslaked lime is 8-15min/ DEG C, digestion temperature is 75-85 DEG C, the massfraction of A (CaO+MgO) is 68-80%, and this unslaked lime mainly provides effective CaO and heat in the preparation of concrete segment, plays an important role to the early strength of slip thickening and base substrate.The heat that effective CaO hydration reaction produces, promotes that aluminium cream is got angry.
Phosphogypsum, the content of its terra alba is 70-78%, this phosphogypsum in the preparation of concrete segment mainly to the suppression that unslaked lime is cleared up, extend the slip thickening time, slurry temperature is made to increase mild, aluminium cream is got angry evenly, is conducive to base substrate and forms good air hole structure, can provide product strength within the specific limits.Also participate in hydrothermal synthesis reaction and improve product strength, reduce shrinkage value, improve frost resistance.When consumption is too much, easily cause slip multiviscosisty cross slow and cause bubbling and sinking, even collapse mould.
In quartz Weathered Sand, the content of silicon-dioxide is 80-90%, and this quartzy Weathered Sand mainly plays in the preparation of concrete segment provides siliceous material and skeletal support effect, SiO
2react with the CaO in lime and cement, under steam press maintenance condition, produce new hydrated product, make autoclave aerated concrete building block reach requirement of strength.
Aluminium powder cream plays foaming agent in the preparation of concrete segment.Metallic aluminium in aluminium cream and water react and produce hydrogen under alkaline environment, and hydrogen forms nuclei of bubbles on aluminium cream fine particle surface, and bubble parameters promotes slip and expands, and forms the base substrate of certain volume.
Water carries out hydrothermal synthesis reaction and aluminium powder cream to get angry the important component of reaction, is also the necessary medium each starting material being mixed and carries out complex chemical reaction.Appropriate ratio of water to material makes slip have suitable denseness and mobility, and make to get angry smooth and easy, base substrate obtains good air hole structure.
The autoclave aerated concrete building block dry density < 525kg/m prepared by above-mentioned steps
3, cubic compressive strength mean value > 3.5MPa, single group minimum value > 2.8Mpa, split pressure ratio > 0.16, freeze rear mass loss < 5.0%, freeze rear intensity > 2.8Mpa, thermal conductivity (dry state) < 0.14W/ (mK), drying shrinkage value (standard law) < 0. 50mm/m, reach the requirement of GB GB11968-2006 " autoclave aerated concrete building block " A3.5 B05 level autoclave aerated concrete building block.Qualification rate > 98%.
technical scheme of the present invention is adopted to have following beneficial effect
The present invention in enormous quantities, high qualification rate can produce A3.5 B05 level autoclave aerated concrete building block.Compared with existing process for producing aerated concrete, there is following remarkable advantage.
1. the present invention adds the industrial waste phosphogypsum of suitable proportion and useless slurry mix grinding in wet-milling slurrying.Add the digestion reaction that trade waste phosphogypsum effectively can suppress unslaked lime, not only solve production unslaked lime and cause because digestion rate is fast, digestion temperature is high unstable problem of getting angry, also alleviate a difficult problem for trade waste comprehensive utilization to a certain extent.Useless slurry mix and adopt mix grinding technique, overcome the active low and problem that pulp viscosities is poor of quartzy Weathered Sand.
Useless slurry is that waste material after Aerated concrete blank cutting and water stir and formed, and density domination is at 1.2 ~ 1.3 g/cm
3, useless slurry is transported to useless slurry tank for mix grinding slurrying by Pulp pump.Because have higher basicity in useless slurry, and after long time stored, each material has tentatively carried out hydration reaction, and number of gels is more.Mix grinding technique then makes partial material antedating response, is conducive to base substrate sclerosis, shortens the precuring time.
2. the present invention suitably improves the fineness of slip in mix grinding slurrying.The quartzy Weathered Sand SiO that the present invention uses
2content is up to 88.9%, and 180 mesh sieve margins only 50 ~ 55%, silt content reaches 12%.Because self fine aggregate content before making quartzy Weathered Sand ball milling is many, specific surface area is large, SiO
2content is high, can ensure SiO
2with the abundant reaction of CaO.If slip fineness is lower, stickiness or the denseness of slip are excessive, and mobility is deteriorated, and getting angry, it is smooth and easy not to expand.
3. the present invention increases ratio of water to material in compounding links, reduces teeming temperature.A3.5 B05 level autoclave aerated concrete building block is lower relative to B06, B07 level building block dry density, and the dry material of unit volume is less, will ensure that goods meet the requirements of intensity simultaneously, suitably should increase calcium silicon ratio, generates more silico-calcium hydrated product.The increase of lime or cement cementitious material ratio, the heat that effective CaO hydration reaction produces increases, and slip bodying velocity is accelerated, and need reduce warm-up time, reduces teeming temperature, reduces aluminium cream raising rate.Need to increase ratio of water to material simultaneously, suppress the multiviscosisty of slip.Finally make slip get angry in expansion process, raising rate and bodying velocity, setting rate are harmonious, and slip expand into default volume, the mould that do not occur collapsing, shrink lower floor or bubbling boiling phenomenon.
The present invention can significantly reduce product dry density, reduce thermal conductivity, improve intensity, strengthen frost resistance, reduce drying shrinkage value, key is that production process determines the source material mixture ratio of applicable quartzy Weathered Sand, through accurate measurement, control Heating temperature and churning time, ensure the stability of getting angry that slurry is good, and expand into the volume of setting, under the steam press maintenance condition formulated, generate hydrated calcium silicate and the aquation calcium aluminosilicate crystallizable mineral of some amount and form.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that quartzy Weathered Sand prepares A3.5 B05 level autoclave aerated concrete building block.
Fig. 2,3,4 is the scanned copy that quartzy Weathered Sand prepares the examining report book of A2.0 B04 level autoclave aerated concrete building block.
Embodiment
Quartz Weathered Sand prepares A3.5 B05 level autoclave aerated concrete building block, each raw-material weight per-cent in total dry material: cement 12 ~ 30%, unslaked lime 10 ~ 28%, quartzy Weathered Sand 55 ~ 70%, aluminium powder cream 0.10 ~ 0.13%, phosphogypsum 3% ~ 6%.Total water (comprise slip is moisture, external adding water, aluminium paste are moisture, steam of heating moisture) and total dry material ratio (ratio of water to material) are 0.67 ~ 0.72.Above-mentioned starting material stir by operation steps, heat after, cast progressive die frame, precuring are shaping, cutting marshalling, steam press maintenance, go out still and pack, and make A3.5 B05 level steam pressure sand aerated concrete block.Product dry density < 525kg/m
3, cubic compressive strength mean value > 3.5MPa, single group minimum value > 2.8Mpa, split pressure ratio > 0.16, freeze rear mass loss < 5.0%, freeze rear intensity > 2.8Mpa, thermal conductivity (dry state) < 0.14W/ (mK), drying shrinkage value (standard law) < 0.50mm/m, qualification rate > 98%.
When the framed volume of precuring is 3.44m
3time, feed composition and formula thereof are: cement 310 ~ 340kg, lime 205 ~ 235 kg, quartzy Weathered Sand 1000 ~ 1100kg, phosphogypsum 62 ~ 78kg, aqueous liquid aluminium powder cream 1.86 ~ 1.96kg, total water 1050 ~ 1150 kg, wherein external adding water 330 ~ 420kg.
Described cement is PO 42.5 ordinary Portland cement, and quicklime slaking speed 8 ~ 15min, digestion temperature 75 ~ 85 DEG C, A (CaO+MgO) massfraction 68 ~ 80%, phosphogypsum is trade waste, terra alba (CaSO
42H
2o) massfraction 70 ~ 78%, sand is quartzy Weathered Sand, silicon-dioxide (SiO
2) massfraction 80 ~ 90%.Foaming agent is GLS-65 water aqua type aluminium powder cream.
Prepare the process flow sheet of A3.5 B05 level autoclave aerated concrete building block as can be seen from the quartzy Weathered Sand of Fig. 1, lime sends into lime powder bin after fragmentation and ball milling, cement bin sent into by bulk cement; Quartz Weathered Sand, phosphogypsum, water, useless slurry send into ball mill mix grinding, send into slurry tank after wearing into slip; Aluminium powder cream and water send into aluminium paste tank through measuring, after mix and blend; Simultaneously send into steam toward cast building stirred pot, by above-mentioned compound through measuring, pouring into a mould, get angry, precuring, the demoulding, cutting, organize into groups, enter still, go out still, torpedo, packing obtain product.In this process, pour into a mould in process of heating and need to pass into steam, quiet stopping needs in precuring process to pass into steam maintenance room temperature, needs to pass into steam steam press maintenance after entering still.Side plate after framed and cutting upset after the demoulding, after cleaning and assembling, is sent into casting process by track, is recycled.Scrap stock after cutting are recycled water and pour useless stock tank, through fully stirring the useless slurry of the certain density of formation, send into useless slurry storage tank for subsequent use, and slip process processed will give up slurry feeding ball mill with quartzy Weathered Sand, phosphogypsum and water mix grinding.
embodiment 1
By quartzy Weathered Sand and phosphogypsum in mass ratio 100:6.2 use belt scale metering respectively, be transported to feed inlet of globe mill, the slurry that adds water and give up (throughput ratio of water and useless slurry is 7:1) mix grinding, obtain that fineness is 26%, mass percent concentration is the slip of 62.0%; Broken unslaked lime, ball milling prepares calcium lime powder, and fineness is 12%, digestion time 9min, digestion temperature 81 DEG C, A (CaO+MgO) massfraction 78%; By water and aluminium powder cream in mass ratio 9:1 to stir formation aluminium paste.Fineness for dry material through 180 order standard inspection sieves screen over-size shared by mass percent.Described useless slurry be following in leftover bits enter recirculated water after, through stir formed density be 1.28g/cm
3mixture, the main component of this mixture comprises calcium hydroxide, the hydrated calcium silicate that in silicon-dioxide, lime and the cement that water, quartzy Weathered Sand and cement provides, calcium oxide hydration reaction is formed.
Feed proportioning system adopts PLC automatically to control, measure slip 1733kg respectively, external adding water 468kg, cement 320kg, lime 220kg, start stirrer discharging successively, stir 30s, use 0.35MPa steam heating, metering aluminium paste 19.4kg, in tank to be mixed, temperature rises to 31 DEG C (outdoor environment temperature is 14 ~ 16 DEG C) stopping heating, when in tank, temperature rises to 32 DEG C automatically, the aluminium paste measured is discharged in stirred pot, stir 38s, open casting valve, in stirred pot slurry be all discharged into framed in, be rest between the precuring of 48 ~ 52 DEG C by the framed temperature that is delivered into, slurry goes up and highly reaches 34.2cm in 42min, billet surface is smooth, without sinking, subside and the phenomenon such as bubbling, cut after 185min.Remove the tailing of billet surface, organize into groups into still.
Carry out steam press maintenance to entering the base substrate after still by distribution system, the pressure that wherein each link is corresponding and time requirement complete by the method: 1. close autoclave door, vacuumize, make still internal pressure reach-0.03Mpa;
2. boosting heats up, uninterrupted through the temperature-rise period :-0.03Mpa that boosts as follows-0Mpa (in 15 minutes, still internal pressure being boosted to 0MPa from-0.03MPa) successively; 0Mpa-0.45Mpa (in 60 minutes, still internal pressure being boosted to 0.45MPa from 0MPa); 0.45Mpa-0.8Mpa (in 30 minutes, still internal pressure being boosted to 0.8MPa from 0.45MPa); 0.8Mpa-1.32Mpa (in 30 minutes, still internal pressure being boosted to 1.32MPa from 0.8MPa);
3. constant voltage constant temperature: supplement steam in time, keeps still internal pressure 1.32Mpa (maintaining 6.5 hours);
4. step-down cooling, uninterrupted through following step-down temperature-fall period successively: 1.32-1.0Mpa is (in 30 minutes, still internal pressure is depressurized to 1.0MPa from 1.32MPa), 1.0-0.65Mpa is (in 30 minutes, still internal pressure is depressurized to 0.65MPa from 1.0MPa), 0.65Mpa-normal pressure.
Pressure and temperature in this step is by autoclave delivering vapor or gas exhaust inspecting, through supplying gas or being vented, forms boosting intensification, constant voltage constant temperature or step-down cooling in still.
After going out still, conforming product rate is 98.9%.After testing, by autoclave aerated concrete building block dry density 518kg/m prepared by above-mentioned steps
3cubic compressive strength mean value 3.5MPa, single group minimum value 2.9Mpa, freeze rear mass loss 4.2%, freeze rear intensity 2.9Mpa, thermal conductivity (dry state) 0.127W/ (mK), drying shrinkage value (standard law) 0.39mm/m, meets the requirement of GB11968-2006 " autoclave aerated concrete building block " A3.5 B05 level autoclave aerated concrete building block.
embodiment 2
By quartzy Weathered Sand and phosphogypsum in mass ratio 100:6.5 use belt scale metering respectively, the slurry that adds water and give up (throughput ratio of water and useless slurry is 7.2:1) mix grinding, obtain that fineness is 25%, mass percent concentration is the slip of 62.3%; Broken unslaked lime, ball milling prepares calcium lime powder, and fineness is 12%, digestion time 12min, digestion temperature 82 DEG C, A (CaO+MgO) massfraction 76%; By water and aluminium powder cream in mass ratio 9:1 to stir formation aluminium paste.Fineness for dry material through 180 order standard inspection sieves screen over-size shared by mass percent.Described useless slurry be following in scrap stock enter recirculated water after, through stir formed density be 1.25g/cm
3mixture, the main component of this mixture comprises calcium hydroxide, the hydrated calcium silicate that in silicon-dioxide, lime and the cement that water, quartzy Weathered Sand and cement provides, calcium oxide hydration reaction is formed.
Feed proportioning system adopts PLC automatically to control, measure slip 1710kg respectively, external adding water 485kg, cement 325kg, lime 225kg, start stirrer discharging successively, stir 30s, use 0.35MPa steam heating, metering aluminium paste 19.2kg, in tank to be mixed, temperature rises to 30.8 DEG C (outdoor environment temperature is 10 ~ 12 DEG C) stopping heating, when in tank, temperature rises to 31.8 DEG C automatically, the aluminium paste measured is discharged in stirred pot, stir 38s, open casting valve, in stirred pot slurry be all discharged into framed in, be rest between the precuring of 48 ~ 52 DEG C by the framed temperature that is delivered into, slurry goes up and highly reaches 34.6cm in 44min, billet surface is smooth, without sinking, subside and the phenomenon such as bubbling, cut after 190min.Remove the tailing of billet surface, organize into groups into still.
Carry out steam press maintenance according to distribution system in embodiment 1, wherein constant pressure and constant thermophase, keep still internal pressure 1.32Mpa, maintain 7.0 hours, other pressure and time controling process are with embodiment 1.
After going out still, conforming product rate is 98.7%.After testing, by autoclave aerated concrete building block dry density 514kg/m prepared by above-mentioned steps
3cubic compressive strength mean value 3.6MPa, single group minimum value 3.0Mpa, freeze rear mass loss 3.6%, freeze rear intensity 3.0Mpa, thermal conductivity (dry state) 0.126W/ (mK), drying shrinkage value (standard law) 0.35mm/m, meets the requirement of GB11968-2006 " autoclave aerated concrete building block " A3.5 B05 level autoclave aerated concrete building block.
embodiment 3
By quartzy Weathered Sand and phosphogypsum in mass ratio 100:7 use belt scale metering respectively, be transported to feed inlet of globe mill, the slurry that adds water and give up (throughput ratio of water and useless slurry is 7.5:1) mix grinding, obtain that fineness is 27%, mass percent concentration is the slip of 62.2%; Broken unslaked lime, ball milling prepares calcium lime powder, and fineness is 11%, digestion time 12min, digestion temperature 81 DEG C, A (CaO+MgO) massfraction 80%; By water and aluminium powder cream in mass ratio 9:1 to stir formation aluminium paste.Fineness for dry material through 180 order standard inspection sieves screen over-size shared by mass percent.Described useless slurry be following in scrap stock enter recirculated water after, through stir formed density be 1.26g/cm
3mixture, the main component of this mixture comprises calcium hydroxide, the hydrated calcium silicate that in silicon-dioxide, lime and the cement that water, quartzy Weathered Sand and cement provides, calcium oxide hydration reaction is formed.
Feed proportioning system adopts PLC automatically to control, measure slip 1702kg respectively, external adding water 490kg, cement 330kg, lime 230kg, start stirrer discharging successively, stir 30s, use 0.35MPa steam heating, metering aluminium paste 19.5kg, in tank to be mixed, temperature rises to 31 DEG C (outdoor environment temperature is 12 ~ 14 DEG C) stopping heating, when in tank, temperature rises to 32 DEG C automatically, the aluminium paste measured is discharged in stirred pot, stir 40s, open casting valve, in stirred pot slurry be all discharged into framed in, be rest between the precuring of 48-52 DEG C by the framed temperature that is delivered into, slurry goes up and highly reaches 35.4cm in 45min, billet surface is smooth, without sinking, subside and the phenomenon such as bubbling, cut after 185min.Remove the tailing of billet surface, organize into groups into still.
Carry out steam press maintenance to entering the base substrate after still by distribution system, the pressure that wherein each link is corresponding and time requirement complete by the method: 1. close autoclave door, vacuumize, make still internal pressure reach-0.03Mpa;
2. boosting heats up, uninterrupted through the temperature-rise period :-0.03Mpa that boosts as follows-0Mpa (in 15 minutes, still internal pressure being boosted to 0MPa from-0.03MPa) successively; 0Mpa-0.45Mpa (in 65 minutes, still internal pressure being boosted to 0.45MPa from 0MPa); 0.45Mpa-0.8Mpa (in 35 minutes, still internal pressure being boosted to 0.8MPa from 0.45MPa); 0.8Mpa-1.32Mpa (in 35 minutes, still internal pressure being boosted to 1.32MPa from 0.8MPa);
3. constant voltage constant temperature: supplement steam in time, keeps still internal pressure 1.32Mpa (maintaining 6.5 hours);
4. step-down cooling, uninterrupted through following step-down temperature-fall period successively: 1.32-1.0Mpa is (in 35 minutes, still internal pressure is depressurized to 1.0MPa from 1.32MPa), 1.0-0.65Mpa is (in 35 minutes, still internal pressure is depressurized to 0.65MPa from 1.0MPa), 0.65Mpa-normal pressure.
Pressure and temperature in this step is by autoclave delivering vapor and gas exhaust inspecting, through supplying gas or being vented, forms boosting intensification, constant voltage constant temperature, step-down cooling or normal temperature and pressure in still.
After going out still, conforming product rate is 99.0%.After testing, by autoclave aerated concrete building block dry density 509kg/m prepared by above-mentioned steps
3cubic compressive strength mean value 3.6MPa, single group minimum value 3.2Mpa, split pressure ratio 0.20, freeze rear mass loss 2.8%, freeze rear intensity 3.1Mpa, thermal conductivity (dry state) 0.1251W/ (mK), drying shrinkage value (standard law) 0.32mm/m, meet the requirement of GB11968-2006 " autoclave aerated concrete building block " A3.5 B05 level autoclave aerated concrete building block.
Claims (8)
1. the A3.5 B05 level autoclave aerated concrete building block prepared of quartzy Weathered Sand, is characterized in that, this concrete segment comprises the dry material composition of following weight part: quartzy Weathered Sand 55-70 part, cement 12-30 part, unslaked lime 10-28 part, aluminium powder cream 0.10-0.13 part, phosphogypsum 3-6 part; Wherein, the dry material component of this concrete segment also comprises water, and the mass ratio of water and dry material is 0.67-0.72:1.
2. the A3.5 B05 level autoclave aerated concrete building block prepared of quartzy Weathered Sand according to claim 1, it is characterized in that, this concrete segment comprises the dry material composition of following weight part: quartzy Weathered Sand 62.4 parts, cement 19.5 parts, unslaked lime 13.6 parts, aluminium powder cream 0.12 part, phosphogypsum 4.38 parts; Wherein, the dry material component of this concrete segment also comprises water, and the mass ratio of water and dry material is 0.68:1.
3. the A3.5 B05 level autoclave aerated concrete building block prepared of quartzy Weathered Sand according to claim 1 and 2, it is characterized in that, cement is PO 42.5 ordinary Portland cement; The digestion rate of unslaked lime is 8-15min/ DEG C, and digestion temperature is the massfraction of 75-85 DEG C, A (CaO+MgO) is 68-80%; Phosphogypsum, the content of its terra alba is 70-78%; In quartz Weathered Sand, the content of silicon-dioxide is 80-90%.
4. quartzy Weathered Sand prepares a method for A3.5 B05 level autoclave aerated concrete building block, it is characterized in that, comprises following preparation process:
By quartzy Weathered Sand and phosphogypsum by weight after mix, being delivered to ball mill, is that 7:1 adds ball mill by water, useless slurry with throughput ratio, mix grinding 10-30min, obtains that fineness is 25-28%, mass percent concentration is the slip of 58-65%; Pulverize and ball milling unslaked lime, obtain the calcium lime powder that fineness is 10%-13%; Be that 8-10:1 mix with aluminium powder cream with mass ratio by water, stir and obtain aluminium paste;
By cement, calcium lime powder, slip, water adds in stirred pot, mixing, stir 25-35s, employing 0.3-0.4MPa is steam heated to 30-35 DEG C, stop heating, aluminium paste is added in stirred pot, after continuing to stir 35-40s, slip in stirred pot is discharged into framed in, and be quiet in the precuring of 48-52 DEG C stopping by framed room temperature of sending to, slip is in framed interior expansion, stable base substrate is formed after 40-48min, base substrate is without sinking, subside, the phenomenon such as bubbling and bleeding, continue to rest after 170-190min and cut, remove the scrap stock after base substrate cutting, base substrate is sent in autoclave,
By distribution system, steam press maintenance is carried out to the base substrate in autoclave, base substrate in autoclave successively through vacuumizing, boosting, obtain A3.5 B05 level autoclave aerated concrete building block after constant voltage and step-down.
5. method according to claim 4, is characterized in that, in step 1), described fineness for dry material through 180 order standard inspection sieves screen over-size shared by mass percent.
6. method according to claim 4, is characterized in that, in step 1), described useless slurry is step 2) in base substrate cutting after scrap stock enter recirculated water after, through stir formed density be 1.2-1.3g/cm
3mixture, the main component of this mixture comprises calcium hydroxide, the hydrated calcium silicate that in silicon-dioxide, lime and the cement that water, quartzy Weathered Sand and cement provides, calcium oxide hydration reaction is formed.
7. method according to claim 4, it is characterized in that, step 2) middle cement, calcium lime powder, slip, water adds in stirred pot, mixing, stir 30s second, employing 0.35MPa is steam heated to 31 DEG C, stop heating, in-tank mixing thing temperature to be mixed rises to 32 DEG C, aluminium paste is added in stirred pot, after continuing to stir 40s, slip in stirred pot is discharged into framed in, be quiet in the precuring of 48-52 DEG C stopping by framed room temperature of sending to, slip is got angry in framed expansion, stable base substrate is formed after 45min, base substrate is without sinking, subside, the wild effect such as bubbling and bleeding, continue to rest after 185min and cut, remove the scrap stock after base substrate cutting, base substrate is sent in autoclave.
8. method according to claim 4, is characterized in that, in described step 3), after vacuumizing in autoclave, autoclave internal pressure is-0.02--0.03MPa; Again to delivering vapor in autoclave, in 12-18min, rise to 0MPa; Continue boosting, in 50-70min, rise to 0.45MPa; Further boosting, rises to 0.8MPa in 25-35min; Again boost, in 25-35min, rise to 1.32MPa; In autoclave, supplement steam in time, keep still internal pressure to be 1.31-1.33MPa, maintain 6-7h; Then be vented step-down, in 25-35min, be depressurized to 1.0MPa; Further exhaust step-down, is depressurized to 0.65MPa in 25-35min; Continue exhaust step-down, autoclave internal pressure is down to normal pressure.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610058148.XA CN105753420B (en) | 2015-04-03 | 2015-04-03 | A3.5 B05 levels autoclave aerated concrete building blocks and its application on wall prepared by a kind of quartzy Weathered Sand |
| CN201610057522.4A CN105693178B (en) | 2015-04-03 | 2015-04-03 | Quartzy Weathered Sand prepares the method for A3.5B05 level autoclave aerated concrete building blocks and its application on wall |
| CN201510156468.4A CN104844106B (en) | 2015-04-03 | 2015-04-03 | A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand and method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510156468.4A CN104844106B (en) | 2015-04-03 | 2015-04-03 | A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand and method thereof |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610057522.4A Division CN105693178B (en) | 2015-04-03 | 2015-04-03 | Quartzy Weathered Sand prepares the method for A3.5B05 level autoclave aerated concrete building blocks and its application on wall |
| CN201610058148.XA Division CN105753420B (en) | 2015-04-03 | 2015-04-03 | A3.5 B05 levels autoclave aerated concrete building blocks and its application on wall prepared by a kind of quartzy Weathered Sand |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104844106A true CN104844106A (en) | 2015-08-19 |
| CN104844106B CN104844106B (en) | 2016-02-24 |
Family
ID=53844153
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610057522.4A Active CN105693178B (en) | 2015-04-03 | 2015-04-03 | Quartzy Weathered Sand prepares the method for A3.5B05 level autoclave aerated concrete building blocks and its application on wall |
| CN201510156468.4A Active CN104844106B (en) | 2015-04-03 | 2015-04-03 | A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand and method thereof |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610057522.4A Active CN105693178B (en) | 2015-04-03 | 2015-04-03 | Quartzy Weathered Sand prepares the method for A3.5B05 level autoclave aerated concrete building blocks and its application on wall |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN105693178B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693178A (en) * | 2015-04-03 | 2016-06-22 | 湖北益通建设股份有限公司 | Method for preparing A3.5B05-grade autoclaved aerated concrete block by quartz weathered sand and application thereof to wall |
| CN106316251A (en) * | 2016-02-02 | 2017-01-11 | 聊城市黄河工程局 | Frost crack prevention pavement construction material and application thereof |
| CN106699218A (en) * | 2017-02-13 | 2017-05-24 | 石河子大学 | Desert sand autoclaved aerated concrete block and processing method thereof |
| CN106699093A (en) * | 2016-12-06 | 2017-05-24 | 常州工学院 | Autolaved aerated concrete block and preparation method thereof |
| CN112125630A (en) * | 2020-06-17 | 2020-12-25 | 湖北益通建设股份有限公司 | High-content phosphogypsum-based stabilizing material and application thereof in road base |
| CN117209242A (en) * | 2023-09-18 | 2023-12-12 | 武汉鑫祥旺实业有限责任公司 | Short-curing high-durability autoclaved aerated concrete and preparation method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753420B (en) * | 2015-04-03 | 2017-11-14 | 湖北益通建设股份有限公司 | A3.5 B05 levels autoclave aerated concrete building blocks and its application on wall prepared by a kind of quartzy Weathered Sand |
| CN112919484A (en) * | 2021-04-25 | 2021-06-08 | 西南科技大学 | Magnesium silicate prepared by taking quartz sand as siliceous raw material and method thereof |
| CN116587409B (en) * | 2023-06-15 | 2024-05-17 | 江苏宇航板业有限公司 | Autoclaved curing method for calcium silicate slab |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000220247A (en) * | 1999-01-29 | 2000-08-08 | Hidenori Matsushita | Light weight brick |
| CN101265072B (en) * | 2008-04-02 | 2011-08-17 | 曹磊 | Coal ash autoclaved sintering-free load bearing section bar and preparation method thereof |
| CN102295438A (en) * | 2010-06-22 | 2011-12-28 | 陈英辉 | Sulfuric acid flyash brick and production process thereof |
| CN102206095B (en) * | 2011-04-12 | 2013-06-05 | 俞华贵 | Aerated concrete building block and preparation technology thereof |
| CN103964781A (en) * | 2014-05-04 | 2014-08-06 | 抚州市恒顺环保建材有限公司 | Autoclaved aerated concrete block and manufacturing process thereof |
| CN104163651A (en) * | 2014-07-18 | 2014-11-26 | 景泰富海阳光建材有限责任公司 | Autoclaved aeolian sand aerated concrete building block and wallboard |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102627468A (en) * | 2012-04-12 | 2012-08-08 | 金立虎 | Waste foundry sand aerated concrete building block and production process thereof |
| CN102850012A (en) * | 2012-05-31 | 2013-01-02 | 贵州省建筑材料科学研究设计院 | Manufacturing method of high-calcium solid sulfur ash aerated concrete building blocks |
| KR101525034B1 (en) * | 2013-06-19 | 2015-06-09 | 주식회사 씨엠디기술단 | Environment-conscious embankment material using high-volume industrial waste by hydration reaction of phosphogypsum-slag |
| CN105693178B (en) * | 2015-04-03 | 2017-11-10 | 湖北益通建设股份有限公司 | Quartzy Weathered Sand prepares the method for A3.5B05 level autoclave aerated concrete building blocks and its application on wall |
-
2015
- 2015-04-03 CN CN201610057522.4A patent/CN105693178B/en active Active
- 2015-04-03 CN CN201510156468.4A patent/CN104844106B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000220247A (en) * | 1999-01-29 | 2000-08-08 | Hidenori Matsushita | Light weight brick |
| CN101265072B (en) * | 2008-04-02 | 2011-08-17 | 曹磊 | Coal ash autoclaved sintering-free load bearing section bar and preparation method thereof |
| CN102295438A (en) * | 2010-06-22 | 2011-12-28 | 陈英辉 | Sulfuric acid flyash brick and production process thereof |
| CN102206095B (en) * | 2011-04-12 | 2013-06-05 | 俞华贵 | Aerated concrete building block and preparation technology thereof |
| CN103964781A (en) * | 2014-05-04 | 2014-08-06 | 抚州市恒顺环保建材有限公司 | Autoclaved aerated concrete block and manufacturing process thereof |
| CN104163651A (en) * | 2014-07-18 | 2014-11-26 | 景泰富海阳光建材有限责任公司 | Autoclaved aeolian sand aerated concrete building block and wallboard |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693178A (en) * | 2015-04-03 | 2016-06-22 | 湖北益通建设股份有限公司 | Method for preparing A3.5B05-grade autoclaved aerated concrete block by quartz weathered sand and application thereof to wall |
| CN106316251A (en) * | 2016-02-02 | 2017-01-11 | 聊城市黄河工程局 | Frost crack prevention pavement construction material and application thereof |
| CN106380157A (en) * | 2016-02-02 | 2017-02-08 | 聊城市黄河工程局 | A method of preparing a frost-crack-preventing pavement construction material and an application of the material |
| CN106699093A (en) * | 2016-12-06 | 2017-05-24 | 常州工学院 | Autolaved aerated concrete block and preparation method thereof |
| CN106699093B (en) * | 2016-12-06 | 2019-04-12 | 常州工学院 | A kind of sand aerated concrete block and preparation method thereof |
| CN106699218A (en) * | 2017-02-13 | 2017-05-24 | 石河子大学 | Desert sand autoclaved aerated concrete block and processing method thereof |
| CN112125630A (en) * | 2020-06-17 | 2020-12-25 | 湖北益通建设股份有限公司 | High-content phosphogypsum-based stabilizing material and application thereof in road base |
| CN112125630B (en) * | 2020-06-17 | 2022-12-06 | 湖北益通建设股份有限公司 | High-content phosphogypsum-based stabilizing material and application thereof in road base |
| CN117209242A (en) * | 2023-09-18 | 2023-12-12 | 武汉鑫祥旺实业有限责任公司 | Short-curing high-durability autoclaved aerated concrete and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104844106B (en) | 2016-02-24 |
| CN105693178A (en) | 2016-06-22 |
| CN105693178B (en) | 2017-11-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104844106B (en) | A3.5 B05 level autoclave aerated concrete building block prepared by a kind of quartzy Weathered Sand and method thereof | |
| CN104774031B (en) | A2.0 B04 grade autoclaved aerated concrete block prepared from quartz eroded sand and preparation method thereof | |
| CN104557107B (en) | Light-weight autoclaved aerated concrete and preparation process thereof | |
| CN101948331B (en) | Autoclaved aerated concrete building block and preparation method thereof | |
| CN101891499A (en) | Method for producing autoclaved aerated concrete from double siliceous raw materials | |
| CN108821671B (en) | Full-industrial solid waste high-strength ready-to-use foamed concrete material and preparation method thereof | |
| CN101289332A (en) | Low-temperature ceramic foam material and production method thereof | |
| CN104591563B (en) | A kind of Binder Materials with flyash as raw material and preparation method thereof | |
| CN103193447A (en) | Autoclaved aerated concrete brick prepared by utilizing pulverized fuel ash and preparation method thereof | |
| CN105110811B (en) | A kind of waste material of stone air entrained concrete and preparation method thereof | |
| CN108558324A (en) | A kind of impervious regeneration concrete | |
| CN103723988A (en) | Light and high strength aerated concrete prepared with glass powder and preparation method thereof | |
| CN101564866A (en) | Production technology for concrete building block of autoclaving and air entraining of circulating fluid bed fly ash | |
| CN111807858A (en) | Industrial solid waste autoclaved aerated concrete block and preparation method thereof | |
| CN102964095A (en) | Aerated concrete building block and manufacturing method thereof | |
| CN102627468A (en) | Waste foundry sand aerated concrete building block and production process thereof | |
| CN107522453A (en) | Air entrained concrete and preparation method thereof | |
| CN103979878A (en) | Waste residue aerated concrete block and production technology thereof | |
| CN105175003A (en) | Non-lime fly ash autoclaved aerated concrete and preparation method thereof | |
| CN110156492A (en) | The method and product of air entrained concrete are prepared based on microwave precuring technology of getting angry | |
| CN102295441A (en) | Aerated concrete brick produced by using tailing slags | |
| CN105016769B (en) | A kind of recycling method of caused solid waste in steam pressure sand aerated concrete block production | |
| CN114573361A (en) | Production method and system of environment-friendly carbon-fixing aerated brick | |
| CN114605121B (en) | Tungsten tailing autoclaved aerated concrete and preparation method thereof | |
| CN105753420B (en) | A3.5 B05 levels autoclave aerated concrete building blocks and its application on wall prepared by a kind of quartzy Weathered Sand |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |