CN102515579A - Method for preparing geological polymeric material by using low-grade kaolin - Google Patents
Method for preparing geological polymeric material by using low-grade kaolin Download PDFInfo
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- CN102515579A CN102515579A CN2011104056303A CN201110405630A CN102515579A CN 102515579 A CN102515579 A CN 102515579A CN 2011104056303 A CN2011104056303 A CN 2011104056303A CN 201110405630 A CN201110405630 A CN 201110405630A CN 102515579 A CN102515579 A CN 102515579A
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Abstract
The invention discloses a method for preparing a geological polymeric material by using low-grade kaolin. The method comprises the following steps (1) uniformly mixing low-grade kaolin and an activator I in a certain proportion, wherein the mass ratio of particle size of solid phase in a mixture to material residue on sieve with 200 meshes is less than10%; (2)insulating calcining the mixture in the step (1) at high temperature of 750-950 DEG C for 2-4 hours, grinding the calcined product to obtain the clinker powder, the mass ratio of clinker powder particle size to material residue on sieve with 200 meshes is less than10%; (3) adding an water solution of an activator II in the clinker powder obtained in the step (2), uniformly mixing, vibrating and compacting, keeping the moisture and conserving at 60-90 DEG C for 2-4 days to obtain the geological polymer material; wherein, the water cement ratio of activator II water solution to clinker powder is 0.2 0.4, and the mass ratio of solid phase in activator II to calcined clinker powder is 0 0.07. The present invention has obvious significance for expanding the sources of raw materials, reducing the cost and improving the use convenience.
Description
Technical field
The invention belongs to the novel concrete field of materials, be specifically related to a kind of method of utilizing low-grade kaolin to prepare the geology polymeric materials.
Background technology
[0002] geology polymeric materials (abbreviating the ground polymers as) is also referred to as mineral polymeric material, native polywater mud, alkali-excited cement etc., is a kind of ecological environment-friendly type sal inorganic coagulation material that is expected to substitute portland cement that development in recent years is got up.It mainly is meant contains multiple amorphousness to the hemicrystalline type of three-dimensional aluminium silicate mineral polymkeric substance of zeolite.Its typical preparation procedure is: sal raw material → calcining activation → soluble alkali metal silico-aluminate dissolving excites → 20～120 ℃ of insulated curings.Ground polymers raw material sources are abundant, and carbon emission is low, and expansion-concentration rate is low; Rate of permeation is low, and early strength rises fast, and final strength is high; Acid resistance is strong, good heat resistance, and alkali-aggregate reaction is far below conventional portland cement; Endurance quality is good, is considered to progressively to replace that the energy consumption material consumption is high, carbon emission is high, environmental pollution is serious, the novel inorganic gelling material of the portland cement of acid resistance and poor durability.Davidovits uses kaolinite and calcined kaolinite to prepare geopolymer the earliest and applies for a patent.In recent years, as the product that has most application market to be worth, the research of flyash base polymers is concentrated relatively.At home, the real research of geology polymeric materials is started from this century and persistently overheating, more with the research that China University of Geosciences, China Mining University and Southeast China University deliver.
Patent CN1634795A provides a kind of preparation method of aluminium silicate mineral polymer materials, promptly uses the mixing solutions of alkalescence to excite clay class aluminum silicate raw material to prepare the method for polymer materials.Utilize common clay class aluminosilicate, i.e. kaolin perhaps contains the industrial waste raw materials such as flyash, slag of aluminosilicate, uses chemical activator, in the moulding of 5-10MPa pressure pressed, through the prepared in reaction mineral polymeric material.CN1882516 provides a kind of method that forms the geopolymer moulded parts; It comprises: the geopolymer concrete compsn that forms alkali metal containing or alkaline earth metal silicate component, basic metal or alkaline earth metal hydroxides, aggregate and water; Wherein the content of water is not enough to provide the concrete of slump, SiO
2With M
2The ratio of O is at least 0.8.Concrete casting is cast onto in the mould, make the concrete of moulding in mould, carry out fixed.Yet; The geology polymeric materials is used for substituting portland cement and still faces some subject matters: 1. raw material restriction; See from composition; The abundantest aluminum silicate raw material of content all can be used as ground polymers natural matter in the earth's crust, but practical study at most and can prepare sufficient intensity ground polymers still have only kaolin; The sal solid waste is then formed with textural difference big, is difficult to extensive utilization.2. preparation cost is higher, and during natural matter preparation ground polymers, the high grade kaolinite of calcining pretreatment and alkali silicate exciting agent all are the higher raw materials of cost; During with industrial solid wastes preparation ground polymers, though do not need precalcining, used exciting agent is identical with natural mineral raw, and its cost still need reduce.3. be that exciting agent and bicomponent system make its storage use inconvenience with water absorbability and hyperergic overbased salts, and environmental exposure is bigger.
Summary of the invention
The objective of the invention is to provides a kind of new low-grade kaolin that utilizes to prepare the method for geology polymeric materials to existing defective in the existing preparation geology polymeric materials technology.
The inventive method comprises the step of following order:
(1) low-grade kaolin and exciting agent I are mixed, the granularity of solid phase is Zhi Liang Bi ≦ 10% of 200 screen residues in its mixture; Contain CaO and Na in the exciting agent I
2The ratio of the mole number of O is n (CaO)/n (Na
2O) be 0-1.0; The volume of exciting agent I is pressed the Na in the exciting agent I
2The content of O converts, and satisfies Na
2O quality/kaolin quality is 0.07-0.20;
(2) with step (1) gained mixture 750 ℃-950 ℃ soak calcining after 2-4 hour again with the levigate again chamotte powder that obtains of calcinate, the chamotte powder granularity is Zhi Liang Bi ≦ 10% of 200 screen residues;
(3) in step (2) gained chamotte powder, mix the aqueous solution of exciting agent II, mix, obtained at 60-90 ℃ of moisture-keeping maintaining 2-4 days behind the vibratory compaction geology polymeric materials; Wherein, wc is that the aqueous solution of exciting agent II and the mass ratio of chamotte powder are 0.2-0.4, and solid phase is 0-0.07 with the mass ratio of calcining back chamotte powder in the exciting agent II.
Said exciting agent I or NaOH, or soda ash light NaCO
3, or soda ash light NaCO
3Add lime; Said exciting agent II or NaOH, or KOH.
The hybrid mode of said low-grade kaolin of step (1) and exciting agent I is for first kind: low-grade kaolin and exciting agent I solid phase mixing mix with the mode of grinding together; Second kind is: the kaolin powder after the grinding carries out solid-liquid with the exciting agent I in being dissolved in water to be mixed, and stirs to reach uniform mixing; Wherein, be preferably second kind of hybrid mode.
Low-grade kaolin according to the invention is meant that the content of kaolinite mineral is lower in the kaolin, contains the kaolin of more impurity, and usually in the kaolin impure maximum be quartzy, secondly be feldspar, mica and iron mineral etc.For the performance of improving the geology polymeric materials can also add various gathering materials and inertia enhancing material in the material of above-mentioned steps (3).
The present invention is through adjustment ground polymers preparation technology; Add the highly basic that should in subsequent technique, add at the raw material calcination stage and calcine (hereinafter referred is an alkali fusion) with raw material with other builder salts; To improve the geology polymerization activity of calcinate, solved the problem that exists in the existing ground polymers technology of preparing.Alkali fusion method of the present invention excites the meaning of low-grade kaolinic geology polymerization activity to be: 1. improved the strength property of the geology polymeric materials of low-grade kaolin preparation, thereby expanded the raw material range of geology polymeric materials.2. be expected to reduce ground polymers cost and energy consumption and make things convenient for its use.
Embodiment
Through concrete experiment embodiment the present invention is described in further detail below.Equipment used is a conventional equipment in the embodiment of the invention, and raw materials used is conventional raw material.
Used low-grade kaolinic chemical constitution is as shown in table 1 in the embodiment of the invention.Kaolin powder after the grinding shows that through X-ray diffraction analysis its thing phase composite is: alpha-quartz, kaolinite, potassium felspar sand and white mica.The quality percentage composition that goes out each mineral facies through the chemical constitution COMPREHENSIVE CALCULATING is respectively: alpha-quartz 37.05, kaolinite 33.05, potassium felspar sand 24.65 and white mica 3.85.
The contrast experiment is: 650-950 ℃ directly this kaolin powder of calcining (fineness is 200 screen residue mass ratioes 7%) after 3 hours ball milling to particle diameter be 200 screen residue mass ratioes 8%; Sodium silicate solution with the caustic soda modification is mixed into slurries then; Be poured into moulding in 40 * 40 * 40 the punching block, maintenance made the geology polymeric materials in 3 days under the humidity of vibratory compaction Hou Zai ≧ 90% and 80 ℃ the temperature.Through four factors such as calcining temperature, liquid-solid ratio, modulus of water glass and concentration of sodium silicate being carried out the maximum compressive strength that the optimization of two-wheeled orthogonal experiment obtains is 16.3MPa (seeing the contrast experiment of table 2).
Low-grade kaolinic chemical constitution of table 1 and mineral composition
The low-grade kaolin alkali fusion of table 2 excites the preparation technology parameter and the intensity table look-up of preparation geology polymeric materials instance
*The full water ultimate compression strength of measuring in soaked 1 day after the maintenance;
*Exciting agent is that modulus is 1.1 modification sodium silicate.
The embodiment of the invention is, adds suitable quantity of water with exciting agent I wiring solution-forming or suspension liquid (when in the exciting agent during limy), and the exciting agent I comprises the mixture of a kind of of caustic soda, soda ash light and lime or two kinds.Being 200 mesh screen residue material amounts with this exciting agent liquid slurry and ball milling to particle diameter is uniformly mixed into muddy than ≦ 10% above-mentioned kaolin powder; Obtained grog in 2-4 hour 750-950 ℃ of calcining; Be the chamotte powder of 200 mesh screen residue material amounts ratio ≦ 10% again with refrigerative chamotte powder ball milling to fineness; The solution of chamotte powder with the exciting agent II is mixed, and the dosage of water is the upper limit with the wc that just satisfies the slurries thixotropy respectively in each instance.In the cement paste stirrer, stir after 2-5 minute, be poured into moulding in 40 * 40 * 40 the punching block, made the geology polymeric materials under the humidity of vibratory compaction Hou Zai ≧ 90% and 60-90 ℃ the temperature in maintenance 2-4 days.The relevant prescription and the processing parameter of 22 instances see table 2 for details.
Can know by table 2; Under close conservation system; The ultimate compression strength majority of the geology polymeric materials that obtains with alkali fusion method processing low-grade kaolin is greater than the ultimate compression strength (seeing the contrast experiment) that excites the geology polymeric materials that obtains behind the direct calcined kaolin with modified water glass; The former maximum compressive strength reaches 63MPa, near 4 times of the latter, explains that the alkali fusion method has positive effect to the intensity that improves the geology polymeric materials for preparing with low-grade kaolin.The present invention prepares geopolymer, when aquation, only adds water and does not add the geopolymer that other alkali-activator such as modified water glass can also make sufficient intensity, improves the convenience that uses clear meaning is all arranged reducing preparation cost.
Claims (3)
1. method of utilizing low-grade kaolin to prepare the geology polymeric materials is characterized in that comprising the step of following order:
(1) low-grade kaolin and exciting agent I are mixed, the granularity of solid phase is Zhi Liang Bi ≦ 10% of 200 screen residues in its mixture; Contain CaO and Na in the exciting agent I
2The ratio of the mole number of O is n (CaO)/n (Na
2O) be 0-1.0; The volume of exciting agent I is pressed the Na in the exciting agent I
2The content of O converts, and satisfies Na
2O quality/kaolin quality is 0.07-0.20;
(2) with step (1) gained mixture 750 ℃-950 ℃ soak calcining after 2-4 hour again with the levigate again chamotte powder that obtains of calcinate, the chamotte powder granularity is Zhi Liang Bi ≦ 10% of 200 screen residues;
(3) in step (2) gained chamotte powder, mix the aqueous solution of exciting agent II, mix, obtained at 60-90 ℃ of moisture-keeping maintaining 2-4 days behind the vibratory compaction geology polymeric materials; Wherein, wc is that the mass ratio of the exciting agent II aqueous solution and chamotte powder is 0.2-0.4, and solid phase is 0-0.07 with the mass ratio of calcining back chamotte powder in the exciting agent II.
2. the method for utilizing low-grade kaolin to prepare the geology polymeric materials according to claim 1 is characterized in that: said exciting agent I or NaOH, or soda ash light NaCO
3, or soda ash light NaCO
3Add lime; Said exciting agent II or NaOH, or KOH.
3. the method for utilizing low-grade kaolin to prepare the geology polymeric materials according to claim 1 and 2; It is characterized in that: the hybrid mode of said low-grade kaolin of step (1) and exciting agent I is for first kind: low-grade kaolin and exciting agent I solid phase mixing mix with the mode of grinding together; Second kind is: the kaolin powder after the grinding carries out solid-liquid with the exciting agent I in being dissolved in water to be mixed, and stirs to reach uniform mixing; Wherein, be preferably second kind of hybrid mode.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730996A (en) * | 2012-07-11 | 2012-10-17 | 湖南科技大学 | Preparation of single-component alkali-activated cement and application method thereof |
| CN103613296A (en) * | 2013-12-04 | 2014-03-05 | 重庆大学 | Method for preparing alkali-activated gel material by use of low-temperature calcined intercalated kaolin |
| CN105324346A (en) * | 2013-05-23 | 2016-02-10 | 蒂森克虏伯工业解决方案股份公司 | Method for producing a cement clinker substitute |
| CN108863127A (en) * | 2018-07-05 | 2018-11-23 | 浙江大学 | A kind of micro-nano fiber composite toughening enhancing geopolymer and preparation method thereof based on hole optimization |
| CN112250332A (en) * | 2020-09-15 | 2021-01-22 | 山东和光新材料有限公司 | High-temperature-resistant cementing material prepared from flint clay serving as raw material |
| CN112592148A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Method for preparing structural material by utilizing brick-concrete building solid waste reclaimed sand powder with high doping amount |
| CN112592077A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Brick-concrete building waste residue cold-recycling cementing material and use method thereof |
| CN112592147A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Preparation and construction method of brick-concrete building waste residue regenerated road base inorganic mixture |
| CN113003968A (en) * | 2021-05-07 | 2021-06-22 | 中国矿业大学 | Geopolymer dry powder material and preparation method thereof |
-
2011
- 2011-12-08 CN CN2011104056303A patent/CN102515579B/en not_active Expired - Fee Related
Non-Patent Citations (1)
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| 冷达等: "《激发剂对土聚水泥力学性能影响的研究》", 《水泥》 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730996A (en) * | 2012-07-11 | 2012-10-17 | 湖南科技大学 | Preparation of single-component alkali-activated cement and application method thereof |
| CN102730996B (en) * | 2012-07-11 | 2014-06-18 | 湖南科技大学 | Preparation of single-component alkali-activated cement and application method thereof |
| CN105324346A (en) * | 2013-05-23 | 2016-02-10 | 蒂森克虏伯工业解决方案股份公司 | Method for producing a cement clinker substitute |
| RU2672271C2 (en) * | 2013-05-23 | 2018-11-13 | Тюссенкрупп Индастриал Солюшнс Аг | Method for producing cement clinker substitute |
| CN103613296A (en) * | 2013-12-04 | 2014-03-05 | 重庆大学 | Method for preparing alkali-activated gel material by use of low-temperature calcined intercalated kaolin |
| CN103613296B (en) * | 2013-12-04 | 2015-09-09 | 重庆大学 | A kind of low temperature calcination intercalation kaolin soil prepares the method for alkali-activated carbonatite gelling material |
| CN108863127A (en) * | 2018-07-05 | 2018-11-23 | 浙江大学 | A kind of micro-nano fiber composite toughening enhancing geopolymer and preparation method thereof based on hole optimization |
| CN108863127B (en) * | 2018-07-05 | 2020-06-19 | 浙江大学 | Micro-nano fiber composite toughening and reinforcing geopolymer based on pore optimization and preparation method thereof |
| CN112250332A (en) * | 2020-09-15 | 2021-01-22 | 山东和光新材料有限公司 | High-temperature-resistant cementing material prepared from flint clay serving as raw material |
| CN112592148A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Method for preparing structural material by utilizing brick-concrete building solid waste reclaimed sand powder with high doping amount |
| CN112592077A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Brick-concrete building waste residue cold-recycling cementing material and use method thereof |
| CN112592147A (en) * | 2021-01-24 | 2021-04-02 | 湖南科技大学 | Preparation and construction method of brick-concrete building waste residue regenerated road base inorganic mixture |
| CN112592147B (en) * | 2021-01-24 | 2022-06-24 | 湖南科技大学 | Preparation and construction method of brick-concrete building waste residue regenerated road base inorganic mixture |
| CN112592148B (en) * | 2021-01-24 | 2022-06-28 | 湖南科技大学 | Method for preparing structural material by utilizing brick-concrete building solid waste reclaimed sand powder with high doping amount |
| CN112592077B (en) * | 2021-01-24 | 2022-06-28 | 湖南科技大学 | Brick-concrete building waste residue cold-recycling cementing material and use method thereof |
| CN113003968A (en) * | 2021-05-07 | 2021-06-22 | 中国矿业大学 | Geopolymer dry powder material and preparation method thereof |
| CN113003968B (en) * | 2021-05-07 | 2023-02-28 | 中国矿业大学 | Geopolymer dry powder material and preparation method thereof |
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| CN102515579B (en) | 2013-11-13 |
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