CN103626471B - A kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof - Google Patents

A kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof Download PDF

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CN103626471B
CN103626471B CN201310608006.2A CN201310608006A CN103626471B CN 103626471 B CN103626471 B CN 103626471B CN 201310608006 A CN201310608006 A CN 201310608006A CN 103626471 B CN103626471 B CN 103626471B
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phosphorus
gelling
mine tailing
slag
quality
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CN103626471A (en
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曹宏
薛俊
梁兴荣
王其林
石小勇
李先福
赖小莹
张晖
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YUNNAN LINHUA GROUP CORP Ltd
Wuhan Institute of Technology
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YUNNAN LINHUA GROUP CORP Ltd
Wuhan Institute of Technology
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Abstract

The invention belongs to material of construction preparing technical field, be specifically related to a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof.Steamed brick of the present invention, be made up of lean property base-material, gelling material, activator and water, described lean property base-material is made up of phosphorus mine tailing and sand, and described gelling material is made up of phosphorus slag and calcareous raw material, and the mass ratio of described lean property base-material and described gelling material is 8:2 ~ 5:5; The quality of described activator is 2% ~ 5% of phosphorus slag quality in described gelling material, and the quality of described water is 10% ~ 40% of described gelling material quality.Steamed brick ultimate compression strength of the present invention is high, good endurance, dimensional standard, and profile is complete, can meet the requirement of existing national standards JC/T422-2007 " non-sintered rubbish tailing-bricks "; And preparation method's technique is simple, mild condition, be easy to realize.

Description

A kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof
Technical field
The invention belongs to material of construction preparing technical field, be specifically related to a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof.
Background technology
Along with exploitation and the utilization of phosphorus ore, phosphate rock resource is dilution increasingly, and after being listed in 2010 by Ministry of Land and Resources, one of 20 kinds of mineral that can not meet national economic development demand, are classified as non-renewable strategic resource.China's phosphate rock resource enriches, but 80% be in, low-grade phosphate ore, the collophanite of high, the difficult choosing of most genus foreign matter content, in order to meet the specification of quality of phosphoric acid by wet process to raw ore, have to pass through cost-effective beneficiation enrichment and could meet phosphoric acid and high-concentration phosphate compound fertilizers Production requirement, produce a large amount of mine tailing thus.
From mining ore out, extract after useful matter through ore dressing, the overwhelming majority is accumulated all the year round and is deposited in tailing dam, not only takies tract, and may cause severe contamination and destruction to ecotope.Phosphorus mine tailing granularity is comparatively thin, piles up a place, washes away, easily cause Serious geological disasters, cause security incident if meet heavy rain.
In addition, in order to change China's building material industry medium-term and long-term with clay be raw material production vitrified brick this waste land resources in a large number, destroy the way of ploughing, China forbade producing, using and selling solid clay brick in 30 days June in 2003, and advocated research use industrial waste as building material.For this reason, the research and apply utilizing flyash, cinder, coal gangue, mine tailings, residue of chemical industry or natural sand, tidal land mud etc. (above raw material one or several) to prepare building material as main raw material is carried out fast, and reaps rich fruits.But because phosphorus mine tailing belongs to the thinner poor material of particle, it utilizes the following problem of ubiquity in process to need to improve in sundry item: (1) phosphorus mine tailing uses volume very low as fine aggregate; (2) cement cementitious material consumption is large; (3) due to complicacy and the ins and outs of phosphorus mine tailing composition, low strength when making that the cement consumption of phosphorus tailing baking-free brick is little, phosphorus mine tailing volume is large, in order to improve the ultimate compression strength of goods, normal needs add certain admixture (water reducer, exciting agent or retardant etc.), this adds increased production cost.
In view of above problem, not yet find a kind of High-Efficiency Utilization of Phosphorus mine tailing to produce the method for green structural material, this also aggravates phosphorus mine tailing further to the detrimentally affect of environment.
Phosphorus slag is the industrial residue discharged in producing yellow Phosphorus by electric oven process, is generally particulate matter in stokehold through Water Quenching, is generally canescence, in neutral, have vesicular structure, mostly be vitreum, have good pozzolanic activity.Its chemical composition is divided by SiO 2with CaO be main outside, also containing F, Al 2o 3, P 2o 5, MgO, Fe 2o 3and a small amount of K 2o, MnO, Na 2o etc.Often produce 1 ton of yellow phosphorus and approximately will discharge 8 ~ 10 tons of waste residues, according to incompletely statistics, the quantity discharged of phosphorus slag is 1078 ~ 1,300 ten thousand tons/year in the world, so large quantity discharged is major part all air storages except small portion regeneration, both tract was occupied, to environment, human health can be worked the mischief again.
For solving the pollution problem of phosphorus slag, people have researched and developed the multiple method utilizing phosphorus slag to produce material of construction.As the method utilizing phosphorus slag production vitrified brick, haydite, ceramic tile etc. to need high temperature sintering, for another example utilize punching press, the mode such as steam-cured prepares non-burning brick method, if number of patent application is the patent of invention " a kind of novel steamed brick utilizing using waste phosphorus slag to produce and preparation method thereof " of 201110208348.6.
Phosphorus mine tailing and phosphorus slag belong to the waste residue produced after phosphate rock resource utilizes, a lot of phosphorous chemical industry enterprise has this two kinds of industrial residues simultaneously, but at present in disclosed technical scheme, there is no the report both fully utilized together, particularly there is no a large amount of method utilizing thinner phosphorus mine tailing.
In addition, non-burning brick water tolerance prepared by prior art is poor, and particularly serious when especially lean property waste material doping is higher, this just causes a definite limitation to its application, and waterproofing work may be caused to drop into increase.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce and preparation method thereof.
In order to achieve the above object, technical scheme of the present invention is:
Utilize the steamed brick that phosphorus mine tailing and phosphorus slag are produced, be prepared from by lean property base-material, gelling material, activator and water, described lean property base-material is made up of phosphorus mine tailing and sand, and wherein phosphorus mine tailing accounts for the mass percent of lean property base-material is 20% ~ 90%, and all the other are sand; Described gelling material is made up of phosphorus slag and calcareous raw material, and wherein calcareous raw material accounts for the mass percent of gelling material is 5% ~ 30%, and all the other are phosphorus slag; Described calcareous raw material is one or both in lime, carbide slag; The mass ratio of described lean property base-material and described gelling material is 8:2 ~ 5:5; Described activator is one or more in sodium sulfate, sodium aluminate and water glass, and the quality of described activator is 2% ~ 5% of phosphorus slag quality in described gelling material; The quality of described water is 10% ~ 40% of described gelling material quality.
In such scheme, preferably, described calcareous raw material accounts for the mass percent of gelling material is 10% ~ 20%.
In such scheme, preferably, the quality of described activator is 3% of phosphorus slag quality in described gelling material.
In such scheme, granularity≤20 order of described phosphorus slag.
A preparation method for the steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, comprises the steps:
(1) take lean property base-material, gelling material, activator and water, described lean property base-material is made up of phosphorus mine tailing and sand, and wherein phosphorus mine tailing accounts for the mass percent of lean property base-material is 20% ~ 90%, and all the other are sand; Described gelling material is made up of phosphorus slag and calcareous raw material, and wherein calcareous raw material accounts for the mass percent of gelling material is 5% ~ 30%, and all the other are phosphorus slag; Described calcareous raw material is one or both in lime, carbide slag; The mass ratio of described lean property base-material and described gelling material is 8:2 ~ 5:5; Described activator is one or more in sodium sulfate, sodium aluminate and water glass, and the quality of described activator is 2% ~ 5% of phosphorus slag quality in described gelling material; The quality of described water is 10% ~ 40% of described gelling material quality;
(2) the lean property base-material, gelling material and the activator that step (1) are weighed up are dry mixed and stir, and then add load weighted water wet mixing and stir, after wet mixing stirs, then by the ageing of gained material;
(3) pour material good for step (2) ageing in mould impact briquetting, forming pressure 5MPa ~ 25MPa, the shaping rear demoulding, obtains adobe;
(4) by step (3) stamping forming adobe at 20 ~ 30 DEG C, maintenance under the condition of relative humidity >=80%;
(5) autoclave is put in adobe good for step (4) maintenance, be warming up to 150 DEG C ~ 190 DEG C, under autoclave pressure 0.5MPa ~ 1.25MPa, insulation 6 ~ 16h, takes out after naturally cooling, obtains the steamed brick finished product utilizing phosphorus mine tailing and phosphorus slag to produce.
In such scheme, preferably, the step of step (5) is: autoclave is put in adobe good for step (4) maintenance, first be warming up to 80 DEG C ~ 90 DEG C, be incubated after 10 minutes, then be warming up to 150 DEG C ~ 190 DEG C, under autoclave pressure 0.5MPa ~ 1.25MPa, insulation 6 ~ 16h, takes out after naturally cooling, obtains the steamed brick finished product utilizing phosphorus mine tailing and phosphorus slag to produce.
Beneficial effect of the present invention:
(1) steamed brick of the present invention with phosphorus mine tailing and phosphorus slag for main raw material, without the need to sintering, in a large number, integrally can consume phosphorus mine tailing and phosphorus slag, particularly can utilize thinner phosphorus mine tailing in a large number, having low cost, advantage that environmental protection intensity is high, is a kind of extremely promising renewal product that can replace conventional clay common brick;
(2) high, the good endurance of steamed brick ultimate compression strength of the present invention, dimensional standard, profile is complete, can meet the related request of MU25 level goods in existing national standards JC/T422-2007 " non-sintered rubbish tailing-bricks ";
(3) steamed brick prepared of the present invention, can also have good water tolerance, can be applied in wet environment and even water, the applied range of product;
(4) gelling material that steamed brick of the present invention is used is mainly phosphorus slag and calcareous raw material, and comparatively the gelling material such as cement has energy-saving and environmental protection, the advantages such as production cost is low;
(5) main raw material that the present invention prepares steamed brick can obtain near phosphorus ore, has more advantage especially, can save amount transport cost for the phosphorous chemical industry enterprise producing phosphorus slag and phosphorus mine tailing two kinds of waste materials simultaneously;
(6) simple, the mild condition of preparation method's technique of steamed brick of the present invention, be easy to realize.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce of the present invention.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, accompanying drawing and subordinate list, but content of the present invention is not only confined to the following examples.
In following examples, phosphorus mine tailing used takes from Jinning County of phosphatization group, Yunnan phosphorus ore wheatland tailing dam, phosphorus slag takes from the phosphorus slag that Yunnan phosphatization group Jinning County's Yellow Phosphorous Plant production yellow phosphorus produces, only phosphorus mine tailing and phosphorus slag source are described herein, do not form the present invention's restriction, this type of phosphorus ore waste material in other area also can realize the present invention.
In following examples, sand and lime are common building materials, and sand is common river sand, and lime is the building stone ashes meeting national standard.
In following examples, described phosphorus slag is granularity≤20 object phosphorus slag after crushing and screening, SiO free in phosphorus slag after broken 2and Al 2o 3amount increases, and the specific surface area of phosphorus slag increases, and more easily carries out hydration reaction, can reduce calcareous raw material and activator level, reduces production cost.
Embodiment 1 ~ 92
In embodiment 1 ~ 24, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 8:2, and each component proportion sees the following form 1.
Table 1
In embodiment 1 ~ 24, prepare the step of above-mentioned steamed brick:
(1) lean property base-material, gelling material, activator and water is taken according to the proportioning of each component of table 1;
(2) load weighted for step (1) lean property base-material, gelling material and activator are poured into stirrer be dry mixed and stir after (stirring 3 ~ 10min), add load weighted water wet mixing again to stir, (3 ~ 10min is stirred), by gained material ageing 24 hours after stirring;
(3) pour material good for step (2) ageing in mould impact briquetting, forming pressure 25MPa, after shaping, the demoulding immediately, obtains adobe;
(4) by step (3) stamping forming adobe at 20 DEG C, maintenance under the condition of relative humidity 90%, curing time is 24 hours;
(5) autoclave is put in adobe good for step (4) maintenance, be warming up to 174.5 DEG C, autoclave pressure is under 0.8MPa condition, and insulation 8h, takes out goods after naturally cooling, obtain steamed brick finished product.
Curing time in actual production in the digestion time of step (2) and step (4) can increase, and increases the above time can promote to some extent product performance, but can increase the production cycle, and above problem can be grasped flexibly according to practical condition.
In embodiment 25 ~ 48, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 7:3, and each component proportion sees the following form 2.
Table 2
In embodiment 25 ~ 48, the step preparing above-mentioned steamed brick is roughly the same with embodiment 1 ~ 24, and difference is: (1) this raw material does not need ageing; (2) the old material stirred is poured in mould, earthquake platform shook after 5 minutes, then with the forming pressure impact briquetting of 20MPa, after shaping, the demoulding immediately, obtains adobe; (3) stamping forming adobe is at 25 DEG C, maintenance 24h under the condition of relative humidity >=80%; (4) autoclave is put in the adobe that maintenance is good, is warming up to 180 DEG C, and under autoclave pressure 1.0MPa, insulation 6h, takes out after naturally cooling, obtains the steamed brick finished product utilizing phosphorus mine tailing and phosphorus slag to produce.
In embodiment 49 ~ 72, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 6:4, and each component proportion side sees the following form 3.In embodiment 49 ~ 72, in described phosphorus mine tailing, particle diameter < 80 object phosphorus mine tailing accounts for more than 99% of phosphorus mine tailing total mass, and the phosphorus mine tailing of this kind of fineness is comparatively thin because of it, is difficult to more greatly and more utilize to environmental hazard;
Table 3
In embodiment 49 ~ 72, the step preparing above-mentioned steamed brick is roughly the same with embodiment 1 ~ 24, difference is: pour in mould by material good for step (2) ageing, earthquake platform shakes after 3 minutes, again with the forming pressure impact briquetting of 25MPa, after shaping, the demoulding immediately, obtains adobe.
In embodiment 73 ~ 80, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 5:5, and each component proportion sees the following form 4.In embodiment 73 ~ 80, because gelling material addition is more, lean property base-material is sieved, set thick lean property base-material: thin lean property base-material=6:4, wherein thick lean property base-material particle diameter >=2mm, all the other are thin lean property base-material, because phosphorus mine tailing is thinner, for reducing material screening cost, in this series is implemented, chiltern raw material accounts for lean property base-material mass percent >=60%.
Table 4
In embodiment 73 ~ 80, the step preparing above-mentioned steamed brick is:
(1) lean property base-material, gelling material, activator and water is taken according to the proportioning of each component of table 1;
(2) load weighted for step (1) lean property base-material, gelling material and activator are poured into stirrer be dry mixed and stir after (stirring 3 ~ 10min), add load weighted water wet mixing again to stir, (3 ~ 10min is stirred), by gained material ageing 48 hours after stirring;
(3) pour in mould by material good for step (2) ageing, earthquake platform shook after 5 minutes, and with the forming pressure impact briquetting of 5MPa, the shaping rear demoulding, obtains adobe;
(4) by step (3) stamping forming adobe at 30 DEG C, maintenance under the condition of relative humidity 90%, curing time is 48 hours;
(5) autoclave is put in adobe good for step (4) maintenance, be first warming up to 80 DEG C ~ 90 DEG C, be incubated after 10 minutes, then be warming up to 190 DEG C, autoclave pressure is under 1.25MPa condition, and insulation 6h, takes out goods after naturally cooling, obtain steamed brick finished product.
In embodiment 81 ~ 85, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 6:4, and each component proportion sees the following form 5.In embodiment 81 ~ 85, wherein in gelling material, calcareous raw material accounts for 30% of total gelling material, and all the other are phosphorus slag.
Table 5
The method that embodiment 81 ~ 85 prepares above-mentioned steamed brick is roughly the same with embodiment 73 ~ 80, and difference is: the digestion time of (1) material is 24 hours; (2) autoclave is put in adobe good for step (4) maintenance, be first warming up to 80 DEG C, be incubated after 10 minutes, then be warming up to 150 DEG C, autoclave pressure is under 0.5MPa condition, and insulation 16h, takes out goods after naturally cooling, obtain steamed brick finished product.
In embodiment 86 ~ 92, a kind of steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, its lean property base-material and gelling material mass ratio are 6:4, and each component proportion sees the following form 6.In embodiment 86 ~ 92, the quality of activator accounts for the quality 3% of phosphorus slag quality.
Table 6
The method that embodiment 86 ~ 92 prepares above-mentioned steamed brick is roughly the same with embodiment 81 ~ 85, difference is: adobe good for step (4) maintenance is put into autoclave by (1), first be warming up to 80 DEG C ~ 90 DEG C, be incubated after 10 minutes, be warming up to 160 DEG C again, autoclave pressure is under 0.6MPa condition, insulation 10h, take out goods after naturally cooling, obtain steamed brick finished product.
Adopt the testing method of regulation in existing national standards JC/T422-2007 " non-sintered rubbish tailing-bricks ", the steamed brick goods that testing example 1 ~ 92 prepares ultimate compression strength, folding strength, water-intake rate.The ultimate compression strength that test result shows above-described embodiment 1 ~ 92 steamed brick goods is 26.78MPa ~ 75.12MPa, and folding strength is 5.64MPa ~ 11.53MPa, and water-intake rate is 8.65% ~ 14.24%.Above index all meets MU25 level goods related request in existing national standards JC/T422-2007 " non-sintered rubbish tailing-bricks ".
Simultaneously, test result statistical study is found, the ultimate compression strength > 45.0MPa of embodiment 30,31,34,35,38,39,41,42,43,54,55,57,58,59,62,63,66,67,74,78, folding strength > 7.0MPa, this is far longer than the steamed brick prepared by current standards and public technology, and shaping rear outward appearance and steam-cured rear outward appearance all better, brick body is smooth complete, without cracking, therefore in above embodiment, each component proportion is preferable range.
Choose embodiment 2,41,80,83,92 and test its water tolerance.Water tolerance refers to that material is not damaged under saturation water effect, the not significantly reduced character of its intensity, represents with the coefficient of softening K that characteristic strength reduces.
K=fw/f
In formula: the ultimate compression strength of fw---material under saturated-water phase, MPa.
F---material ultimate compression strength in the dry state, MPa.
Coefficient of softening K contains the increase of saturated water amount along with material and reduces, and usual K is more than or equal to 0.85 for water-resistant material, can be in for a long time in water or in wet environment and use.
Testing method is as follows: choose each 90 of the good goods of embodiment 2,41,80,83,92 maintenance respectively, dries after 24 hours for subsequent use at 110 DEG C.Each embodiment chooses 30 test ultimate compression strength and folding strength (after folding strength test, two bats cut off mouth and stack test ultimate compression strength on the contrary), and calculating mean value.Remaining goods submerge immersion 24 hours, wiped clean after taking out, and each embodiment chooses 30 test ultimate compression strength and folding strength (after folding strength test, two bats cut off mouths and stack test ultimate compression strength on the contrary) again, and calculating mean value.Residue goods were dried after 24 hours at 110 DEG C, submerge immersion 24 hours again, the ultimate compression strength often organized and folding strength (after folding strength test, two bats cut off mouth and stack test ultimate compression strength on the contrary) is tested after taking out wiped clean, and calculating mean value.Test result sees the following form 5.
Table 7
As can be seen from above data, after goods immersion, intensity is not lost substantially, coefficient of softening K is approximately 1, this illustrates that steamed brick goods prepared by the present invention program have good water tolerance, can be applied in wet environment and even water, this is the non-burning brick characteristic do not possessed of slag system prepared by current technology.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And therefore amplified apparent change or variation are still within the protection domain of the invention.

Claims (5)

1. the steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce, it is characterized in that, be prepared from by lean property base-material, gelling material, activator and water, described lean property base-material is made up of phosphorus mine tailing and sand, wherein phosphorus mine tailing accounts for the mass percent of lean property base-material is 20% ~ 90%, and all the other are sand; Described gelling material is made up of phosphorus slag and calcareous raw material, and wherein calcareous raw material accounts for the mass percent of gelling material is 5% ~ 30%, and all the other are phosphorus slag; Described calcareous raw material is one or both in lime, carbide slag; The mass ratio of described lean property base-material and described gelling material is 8:2 ~ 5:5; Described activator is one or more in sodium sulfate, sodium aluminate and water glass, and the quality of described activator is 2% ~ 5% of phosphorus slag quality in described gelling material; The quality of described water is 10% ~ 40% of described gelling material quality; Granularity≤20 order of described phosphorus slag.
2. utilize the steamed brick that phosphorus mine tailing and phosphorus slag are produced according to claim 1, it is characterized in that, the mass percent that described calcareous raw material accounts for gelling material is 10% ~ 20%.
3. utilize the steamed brick that phosphorus mine tailing and phosphorus slag are produced according to claim 1, it is characterized in that, the quality of described activator is 3% of phosphorus slag quality in described gelling material.
4. a preparation method for the steamed brick utilizing phosphorus mine tailing and phosphorus slag to produce as claimed in claim 1, is characterized in that, comprise the steps:
(1) take lean property base-material, gelling material, activator and water, described lean property base-material is made up of phosphorus mine tailing and sand, and wherein phosphorus mine tailing accounts for the mass percent of lean property base-material is 20% ~ 90%, and all the other are sand; Described gelling material is made up of phosphorus slag and calcareous raw material, and wherein calcareous raw material accounts for the mass percent of gelling material is 5% ~ 30%, and all the other are phosphorus slag; Described calcareous raw material is one or both in lime, carbide slag; The mass ratio of described lean property base-material and described gelling material is 8:2 ~ 5:5; Described activator is one or more in sodium sulfate, sodium aluminate and water glass, and the quality of described activator is 2% ~ 5% of phosphorus slag quality in described gelling material; The quality of described water is 10% ~ 40% of described gelling material quality;
(2) the lean property base-material, gelling material and the activator that step (1) are weighed up are dry mixed and stir, and then add load weighted water wet mixing and stir, after wet mixing stirs, then by the ageing of gained material;
(3) pour material good for step (2) ageing in mould impact briquetting, forming pressure 5MPa ~ 25MPa, the shaping rear demoulding, obtains adobe;
(4) by step (3) stamping forming adobe at 20 ~ 30 DEG C, maintenance under the condition of relative humidity >=80%;
(5) autoclave is put in adobe good for step (4) maintenance, be warming up to 150 DEG C ~ 190 DEG C, under autoclave pressure 0.5MPa ~ 1.25MPa, insulation 6 ~ 16h, take out after naturally cooling, obtain the steamed brick finished product utilizing phosphorus mine tailing and phosphorus slag to produce.
5. preparation method according to claim 4, it is characterized in that, described step (5) is: autoclave is put in adobe good for step (4) maintenance, first be warming up to 80 DEG C ~ 90 DEG C, be incubated after 10 minutes, then be warming up to 150 DEG C ~ 190 DEG C, under autoclave pressure 0.5MPa ~ 1.25MPa, insulation 6 ~ 16h, takes out after naturally cooling, obtains the steamed brick finished product utilizing phosphorus mine tailing and phosphorus slag to produce.
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