CN109180131A - A kind of preparation method of gypsum based self-leveling mortar - Google Patents
A kind of preparation method of gypsum based self-leveling mortar Download PDFInfo
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- CN109180131A CN109180131A CN201811401011.5A CN201811401011A CN109180131A CN 109180131 A CN109180131 A CN 109180131A CN 201811401011 A CN201811401011 A CN 201811401011A CN 109180131 A CN109180131 A CN 109180131A
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- based self
- leveling mortar
- gypsum
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- 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
- C04B28/14—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 calcium sulfate cements
- C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
- C04B28/146—Calcium sulfate hemi-hydrate with a specific crystal form alpha-hemihydrate
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/60—Flooring materials
- C04B2111/62—Self-levelling compositions
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation method of gypsum based self-leveling mortar, includes the following steps: 1) to dry carbide slag, then grind, obtain A product;2) first phosphoric acid is placed in reactor, then A product is put into reactor, temperature reaction, after being separated by filtration, filtrate is B product;3) sulfuric acid solution is taken, is slowly added in B product that the reaction was continued, filters, separate after reaction, and washing and drying is to get α high strength gypsum powder;4) α high strength gypsum powder made from step 3) is mixed with dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent, antiprecipitant and retarder to get gypsum based self-leveling mortar.The present invention has gypsum based self-leveling mortar manufacturing cost low, and physical and mechanical property is good, meanwhile, the characteristics of carbide slag is turned waste into wealth, carbide slag resource utilization is realized.
Description
Technical field
The present invention relates to a kind of preparation process of gravity flowing levelling mortar, especially a kind of preparation side of gypsum based self-leveling mortar
Method.
Background technique
Gypsum based self-leveling mortar, also known as Self-leveling gypsum.It is to be added by gypsum material, extraordinary aggregate and various architectural chemistries
Add agent to be configured meticulously in factory, be uniformly mixed prepared by a kind of dry powder and mortar dedicated for floor leveling.
Self-leveling gypsum according to raw material be divided into alpha-semi water plaster stone type and II type admant paste type (by dihydrate gypsum through 650 DEG C~
750 DEG C are calcined and are obtained), it is all that a certain proportion of retarder (alpha-semi water plaster stone type) or exciting agent (II are added in corresponding raw material
Type admant paste type), then mix cement, water-reducing agent, water-retaining agent, fine aggregate (quartz sand), defoaming agent etc., it is uniformly mixed and is made.By
In the adding proportion very little of above-mentioned various additives, 1% hereinafter, and being all common chemical products, therefore, Self-leveling
The essence of gypsum production technology is exactly the production technology of alpha-semi water plaster stone or II type anhydrite.
Currently, the alpha-semi water plaster stone in China is because accordingly higher by high-quality natural gypsum low output and production cost, it is basic to use
In ceramic mold, Self-leveling gypsum volume of production and marketing is extremely small, and quality monitoring still belongs to blank.Due to being formulated in JC/T 1023-2007
Mechanics index of physics using the minimum of external respective standard, there are some manufacturers to originate from using building gypsum next life
Levelling gypsum makes the quality of Self-leveling gypsum close to the physics of JC/T 1023-2007 by the ratio for increasing chemical addition agent
Mechanical property.The Self-leveling gypsum price for causing current China's sale is high, it is difficult to the situation of popularization and application.
Carbide slag, calcium carbide hydrolysis obtain acetylene gas after with calcium hydroxide waste residue as main component.Its main component is
Ca(OH)2(80%-90%), while also containing SiO2、MgO、Al2O3And a small amount of CaCO3、Fe2O3, carbon slag and S, P etc. it is organic
Impurity.Carbide slag is in strong basicity, and pH value is up to 12 or more.1t calcium carbide adds water to produce more than 300 kg acetylene gas, generates simultaneously
The industrial wastes of 10t solid content about 12%, is commonly called as carbide slag slurries.Due to carbide slag substantial amounts, transportation cost is high, now main at present
The processing mode wanted still is stacked on the spot, but this can not only occupy limited land resource, but also pollute and stack near place
Water body and soil.
This researcher is by research, dense by control phosphoric acid using phosphoric acid and sulfuric acid as reaction medium using carbide slag raw material
Degree and temperature, make α type half-H 2 O calcium sulphate nucleated directly, need not move through calcium sulphate dihydrate to α type half-H 2 O calcium sulphate and turn brilliant process,
Meanwhile by control carbide slag and phosphoric acid quality ratio and sulfuric acid concentration, regulate and control the life of each crystal face of α type half-H 2 O calcium sulphate crystal
Long rate realizes short cylinder crystal controlling, to prepare α high strength gypsum, and prepares stone using α high strength gypsum as primary raw material
Cream base gravity flowing levelling mortar.The technology of preparing can not only reduce the production cost of gypsum based self-leveling mortar, at the same time it can also full
The physical and mechanical property of sufficient gypsum based self-leveling mortar;Also, so that carbide slag is turned waste into wealth, realize resource utilization.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of gypsum based self-leveling mortar.The present invention has gypsum base
Gravity flowing levelling mortar manufacturing cost is low, and physical and mechanical property is good, meanwhile, carbide slag is turned waste into wealth, carbide slag recycling is realized
The characteristics of utilization.
Technical solution of the present invention: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried, is then ground, obtain A product;
2) first phosphoric acid is placed in reactor, then A product is put into reactor, reacted 120~180min, be separated by filtration
Afterwards, filtrate is B product;
3) B product are heated to 85~95 DEG C, take sulfuric acid solution, be slowly added to react in B product, filter, separate, and wash
Drying is washed to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 1), after the carbide slag drying, free moisture is small
In 5%.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 1), after the carbide slag grinding, partial size 80-
120 mesh.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 2), phosphoric acid solution concentration is 25~35%.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 2), the weight ratio of phosphoric acid solution and carbide powder
For 2.0~8.0:1.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 2), the temperature of the reaction is 10~20 DEG C, instead
Answering environmental pressure is normal pressure.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 3), the concentration of sulfuric acid solution is 98%, after addition
Sulfate concentration is 1.02~1.25 times of calcium ion concentration in B product.
The preparation method of gypsum based self-leveling mortar above-mentioned, in step 3), the mode that is slowly added to of the sulfuric acid is drop
Add.
The preparation method of gypsum based self-leveling mortar above-mentioned, in the step 3), being added the time reacted after sulfuric acid is
60~300min is to wash and be dried to free moisture less than 2% with 80~95 DEG C of hot water.
The preparation method of gypsum based self-leveling mortar above-mentioned, in the step 4), the gypsum based self-leveling mortar is pressed
Parts by weight meter, by 40-60 parts of α high strength gypsum powder, 8-12 parts of dicalcium powder, 40-60 parts of quartz sand, 1-3 parts of rubber powder, polycarboxylic acids diminishing
0.1-0.3 parts of agent, 0.1-0.3 parts of defoaming agent, 0.5-1.5 parts of antiprecipitant and 0.05-0.15 parts of retarder mix.
Beneficial effects of the present invention
1, the primary raw material α high strength gypsum of the invention by using carbide slag as raw material, preparing gypsum based self-leveling mortar, by
It is very cheap on cost of material in inherently a kind of waste material for polluting environment of carbide slag, greatly reduce gypsum base gravity flow
The production cost of flat mortar;Meanwhile α high strength gypsum quality made from method of the invention is good, purity is high substantially increases gypsum
The physical and mechanical property of based self-leveling mortar;Furthermore the present invention is by preparing main gypsum by raw material of carbide slag, by itself
It is the carbide slag effective use of waste residue, is turned waste into wealth, realize resource utilization, there is important meaning to environment sustainable development
Justice.
2, the present invention is prepared by carbide slag in the preparation process of α high strength gypsum powder, does not generate dihydrate gypsum crystal, directly
Obtain αsemiwatergypsum, therefore, there is no need to steam pressure dewatering process, with it is traditional prepare the technique of αsemiwatergypsum compared with, save significantly
About energy consumption, also, technique is enormously simplified, improve production efficiency.
3, after reaction, filtrate is phosphoric acid and sulfuric acid mixed acid solution to the present invention, be can be used in addition after concentration is adjusted
In the production of the land plaster of batch, it can be recycled, further reduced production cost.
Metallic element in carbide slag of the present invention forms metal ion, to play to half water stone of a under the action of phosphoric acid
The crystalline form of cream regulates and controls, and promotes its oriented growth at short cylinder;By being detected to α high strength gypsum powder produced by the present invention,
Whiteness >=95, impurity content is few, gypsum content >=98% in α high strength gypsum, fullys meet the high-strength stone of α of now current high-quality
The rank of cream.
According to examination criteria JC/T 1023-2007 to the object of gypsum based self-leveling mortar made from 1-5 of the embodiment of the present invention
Reason mechanical property is detected, test result is as follows table:
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried to free moisture less than 5%, is then ground to 80 mesh, obtain A product;
2) first the phosphoric acid that concentration is 25% is placed in reactor, then A product is pressed to the weight of phosphoric acid solution and carbide powder
It is put into reactor than 8.0:1, reacts 120min under 10 DEG C of normal pressures, after being separated by filtration, filtrate is B product;
3) B product are heated to 85 DEG C, taking concentration is 98% sulfuric acid solution, it is slowly added dropwise into B product that the reaction was continued,
Sulfate concentration is 1.02 times of calcium ion concentration in B product after sulfuric acid solution is added, and reacts filtering, separation after 60min, and with 80
The washing of DEG C hot water is dried to free moisture less than 2% to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar;The gypsum based self-leveling mortar by weight, by α
40 parts of high strength gypsum powder, 40 parts of quartz sand, 1 part of rubber powder, 0.1 part of polycarboxylate water-reducer, 0.1 part of defoaming agent, resists 8 parts of dicalcium powder
0.5 part and 0.05 part of retarder of precipitating reagent mixes.
Embodiment 2: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried to free moisture less than 5%, is then ground to 90 mesh, obtain A product;
2) first the phosphoric acid that concentration is 28% is placed in reactor, then A product is pressed to the weight of phosphoric acid solution and carbide powder
It is put into reactor than 6.0:1, reacts 135min under 12 DEG C of normal pressures, after being separated by filtration, filtrate is B product;
3) B product are heated to 88 DEG C, taking concentration is 98% sulfuric acid solution, it is slowly added dropwise into B product that the reaction was continued,
Sulfate concentration is 1.1 times of calcium ion concentration in B product after sulfuric acid solution is added, and reacts filtering, separation after 120min, and with 85
The washing of DEG C hot water is dried to free moisture less than 2% to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar;The gypsum based self-leveling mortar by weight, by α
45 parts of high strength gypsum powder, 8 parts of dicalcium powder, 45 parts of quartz sand, 1.5 parts of rubber powder, 0.15 part of polycarboxylate water-reducer, defoaming agent 0.15
Part, 0.8 part of antiprecipitant and 0.08 part of retarder mix.
Embodiment 3: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried to free moisture less than 5%, is then ground to 100 mesh, obtain A product;
2) first the phosphoric acid that concentration is 30% is placed in reactor, then A product is pressed to the weight of phosphoric acid solution and carbide powder
It is put into reactor than 5.0:1, reacts 150min under 15 DEG C of normal pressures, after being separated by filtration, filtrate is B product;
3) B product are heated to 90 DEG C, taking concentration is 98% sulfuric acid solution, it is slowly added dropwise into B product that the reaction was continued,
Sulfate concentration is 1.15 times of calcium ion concentration in B product after sulfuric acid solution is added, and reacts filtering, separation after 170min, is used in combination
88 DEG C of hot water washings are dried to free moisture less than 2% to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar;The gypsum based self-leveling mortar by weight, by α
50 parts of high strength gypsum powder, 50 parts of quartz sand, 2 parts of rubber powder, 0.2 part of polycarboxylate water-reducer, 0.2 part of defoaming agent, resists 10 parts of dicalcium powder
1 part and 0.01 part of retarder of precipitating reagent mixes.
Embodiment 4: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried to free moisture less than 5%, is then ground to 110 mesh, obtain A product;
2) first the phosphoric acid that concentration is 33% is placed in reactor, then A product is pressed to the weight of phosphoric acid solution and carbide powder
It is put into reactor than 3.5:1, reacts 175min under 18 DEG C of normal pressures, after being separated by filtration, filtrate is B product;
3) B product are heated to 92 DEG C, taking concentration is 98% sulfuric acid solution, it is slowly added dropwise into B product that the reaction was continued,
Sulfate concentration is 1.20 times of calcium ion concentration in B product after sulfuric acid solution is added, and reacts filtering, separation after 250min, is used in combination
90 DEG C of hot water washings are dried to free moisture less than 2% to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar;The gypsum based self-leveling mortar by weight, by α
55 parts of high strength gypsum powder, 11 parts of dicalcium powder, 55 parts of quartz sand, 2.5 parts of rubber powder, 0.25 part of polycarboxylate water-reducer, defoaming agent 0.25
Part, 1.3 parts of antiprecipitant and 0.13 part of retarder mix.
Embodiment 5: a kind of preparation method of gypsum based self-leveling mortar includes the following steps:
1) carbide slag is dried to free moisture less than 5%, is then ground to 120 mesh, obtain A product;
2) first the phosphoric acid that concentration is 35% is placed in reactor, then A product is pressed to the weight of phosphoric acid solution and carbide powder
It is put into reactor than 2.0:1, reacts 180min under 20 DEG C of normal pressures, after being separated by filtration, filtrate is B product;
3) B product are heated to 95 DEG C, taking concentration is 98% sulfuric acid solution, it is slowly added dropwise into B product that the reaction was continued,
Sulfate concentration is 1.25 times of calcium ion concentration in B product after sulfuric acid solution is added, and reacts filtering, separation after 300min, is used in combination
95 DEG C of hot water washings are dried to free moisture less than 2% to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent,
Antiprecipitant and retarder mixing are to get gypsum based self-leveling mortar;The gypsum based self-leveling mortar by weight, by α
60 parts of high strength gypsum powder, 60 parts of quartz sand, 3 parts of rubber powder, 0.3 part of polycarboxylate water-reducer, 0.3 part of defoaming agent, resists 12 parts of dicalcium powder
1.5 parts and 0.15 part of retarder of precipitating reagent mix.
Claims (10)
1. a kind of preparation method of gypsum based self-leveling mortar, which comprises the steps of:
1) carbide slag is dried, is then ground, obtain A product;
2) first phosphoric acid is placed in reactor, then A product is put into reactor, react 120 ~ 180 min, after being separated by filtration, filter
Liquid is B product;
3) B product are heated to 85 ~ 95 DEG C, take sulfuric acid solution, be slowly added to react in B product, filter, separate, and wash baking
It does to get α high strength gypsum powder;
4) by α high strength gypsum powder made from step 3) and dicalcium powder, quartz sand, rubber powder, polycarboxylate water-reducer, defoaming agent, anti-heavy
Shallow lake agent and retarder mixing are to get gypsum based self-leveling mortar.
2. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 1)
After carbide slag drying, free moisture is less than 5%.
3. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 1)
After carbide slag grinding, partial size is 80-120 mesh.
4. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 2
Phosphoric acid solution concentration is 25 ~ 35%.
5. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 2
The weight ratio of phosphoric acid solution and carbide powder is 2.0 ~ 8.0:1.
6. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 2
The temperature of reaction is 10 ~ 20 DEG C, and reaction environment pressure is normal pressure.
7. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 3)
The concentration of sulfuric acid solution is 98%, and sulfate concentration is 1.02 ~ 1.25 times of calcium ion concentration in B product after addition.
8. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: described in step 3)
The mode that is slowly added to of sulfuric acid is to be added dropwise.
9. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: in the step 3),
It is 60 ~ 300 min that the time reacted after sulfuric acid, which is added, is to wash and be dried to free moisture less than 2% with 80 ~ 95 DEG C of hot water.
10. the preparation method of gypsum based self-leveling mortar according to claim 1, it is characterised in that: in the step 4),
The gypsum based self-leveling mortar by weight, by 40-60 parts of α high strength gypsum powder, 8-12 parts of dicalcium powder, quartz sand 40-60
Part, 1-3 parts of rubber powder, 0.1-0.3 parts of polycarboxylate water-reducer, 0.1-0.3 parts of defoaming agent, 0.5-1.5 parts of antiprecipitant and retarder
0.05-0.15 parts mix.
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CN110156423A (en) * | 2019-06-26 | 2019-08-23 | 贵州大学 | A kind of preparation method of half water ardealite gypsum-based phase change energy storage gravity flowing levelling mortar |
CN110218068A (en) * | 2019-06-26 | 2019-09-10 | 贵州大学 | The preparation method of half water ardealite cement base phase-change accumulation energy gravity flowing levelling mortar of ground |
CN111875273A (en) * | 2020-08-13 | 2020-11-03 | 江苏一夫科技股份有限公司 | High-strength gypsum cementing material based on anhydrite and desulfurized beta powder and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110156423A (en) * | 2019-06-26 | 2019-08-23 | 贵州大学 | A kind of preparation method of half water ardealite gypsum-based phase change energy storage gravity flowing levelling mortar |
CN110218068A (en) * | 2019-06-26 | 2019-09-10 | 贵州大学 | The preparation method of half water ardealite cement base phase-change accumulation energy gravity flowing levelling mortar of ground |
CN110218068B (en) * | 2019-06-26 | 2022-02-18 | 贵州大学 | Preparation method of semi-hydrated phosphogypsum cement-based phase-change energy-storage self-leveling mortar for ground |
CN111875273A (en) * | 2020-08-13 | 2020-11-03 | 江苏一夫科技股份有限公司 | High-strength gypsum cementing material based on anhydrite and desulfurized beta powder and preparation method thereof |
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