CN115043619A - Preparation method of self-gelling fiber composite material - Google Patents
Preparation method of self-gelling fiber composite material Download PDFInfo
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- CN115043619A CN115043619A CN202210706603.8A CN202210706603A CN115043619A CN 115043619 A CN115043619 A CN 115043619A CN 202210706603 A CN202210706603 A CN 202210706603A CN 115043619 A CN115043619 A CN 115043619A
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- filter cake
- self
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- phosphogypsum
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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
- 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
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
- C04B14/383—Whiskers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Processing Of Solid Wastes (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a preparation method of a self-gelling fiber composite material, which comprises the following steps of 1) adding phosphogypsum serving as a raw material into an acid solution, stirring for reaction, and filtering a product while the product is hot after the reaction is finished to obtain a filter cake A and a filtrate A; 2) cooling and crystallizing the filtrate A, and then filtering to obtain a filter cake B and a filtrate B; 3) washing and drying the filter cake A and the filter cake B; 4) and uniformly mixing the dried filter cake A and the dried filter cake B to obtain the self-gelling fiber composite material. The phosphogypsum is used as a raw material to prepare the self-gelling fiber composite material, so that the problem of a bonding interface between fibers and a cement matrix in the traditional fiber cement-based composite material is effectively solved, the adhesion between cement and the fibers is enhanced, the toughness and the strength of the cement material are obviously improved, the problem of stacking of the phosphogypsum can be solved, and the waste is favorably recycled.
Description
Technical Field
The invention belongs to the field of building materials, particularly relates to a self-gelling fiber composite material, and more particularly relates to a preparation method of the self-gelling fiber composite material.
Background
Cement, the most widely used building material in the world, has a major limitation in its brittleness, which is mainly attributed to its poor crack resistance and low flexural strength.
A great deal of research shows that the adding of the fiber material into the cement material obviously improves the brittleness problem of the cement material and improves the crack resistance and the toughness of the cement material by preventing the interaction of the growth, the expansion and the fracture of microcracks. The nanometer fiber and the superfine fiber are used as the cement matrix composite additive, and the strength and the toughness of the nanometer fiber and the superfine fiber are enhanced, so that the research focus of the current cement matrix composite material is formed. CaSO 4 The whisker is an inorganic single crystal with the diameter of 1-4 μm, the aspect ratio of 40-80, the performances of tensile modulus, tensile strength and the like exceeding 170GPa and 20GPa respectively, and the excellent performances make the whisker ideal for cement composite materials. An article named as the mechanical property and the strengthening mechanism of calcium sulfate whisker cement mortar of Liwenbo and the like proves that the calcium sulfate whiskers have effective strengthening and toughening effects on the cement mortar from the research of the adaptability of the calcium sulfate whiskers in the cement mortar and the analysis from a microscopic angle. The phosphogypsum is solid waste residue generated when phosphorite is treated by sulfuric acid in the production of phosphoric acid, the phosphogypsum is a main byproduct in the production of wet-process phosphoric acid, and 4.5 tons of phosphogypsum residue are generated when 1 ton of wet-process phosphoric acid is produced. Because most of the phosphogypsum is treated in a stacking mode, the phosphogypsum not only occupies the land and causes water eutrophication, but also causes resource waste, so that the production of the gypsum whisker with high performance and high added value by using the industrial phosphogypsum is significant. CN103074667B discloses a method for preparing calcium sulfate whiskers by recrystallization: the raw material with the main component of calcium sulfate is added into a sulfuric acid solution to complete reaction and aging at the speed of temperature programming and cooling.
The general fiber cement-based composite material has the problems of inappropriate interface bonding strength between fibers and a cement matrix, uneven dispersion and the like. A paper named 'the mechanical properties and microstructure of calcium sulfate whisker modified cement-based composite material doped with silica fume' of panqing et al indicates that silica fume is used as an excellent cementing filling material and can promote the formation of C-S-H gel in cement to show thatThe microstructure and interface bonding strength of whisker-cement are improved remarkably. It is well known that phosphogypsum contains SiO in addition to a large amount of calcium sulphate dihydrate 2 If it can be used to form SiO therein 2 Effectively utilizes the phosphogypsum more fully.
Based on the self-gelling fiber composite material and the preparation method thereof, the self-gelling fiber composite material with high length-diameter ratio and strong adhesion can be prepared by adopting the phosphogypsum as the raw material, the strength and toughness of a cement material can be increased by the existence of fibers, the bonding strength of the fibers and the cement-based material can be effectively improved, and the phosphogypsum can be fully utilized.
Disclosure of Invention
The invention aims to provide a self-gelling fiber composite material which is added into a cement material, on one hand, the strength and the toughness of the cement material are obviously improved, on the other hand, phosphogypsum is fully utilized, and the green development requirement of enterprises is met.
To achieve the above purpose, the method is mainly implemented by the following scheme:
the preparation method of the self-gelling fiber composite material is characterized by comprising the following steps of:
(1) adding a crystallization promoter into phosphogypsum serving as a raw material, adding the phosphogypsum into an acid solution, stirring and reacting at a certain temperature of 80-90 ℃ for 3-4h, and filtering the product while the product is hot after the reaction is finished to obtain a filter cake A and a filtrate A;
the crystallization aid is citric acid or polyacrylic acid, and the mass ratio of the phosphogypsum to the crystallization aid is 1: 50-200.
The acid solution is hydrochloric acid solution or nitric acid solution, wherein the solid-to-liquid ratio of the phosphogypsum to the acid solution is 0.03-0.1, and the concentration of the acid solution is controlled to be 6-8%.
A tackifier is also added in the step (1), and the tackifier is preferably waterborne polyurethane. The concentration of the tackifier is 50-500g/L, and preferably concentrated to 100-150 g/L.
(2) Cooling and crystallizing the filtrate A, and filtering to obtain a filter cake B and a filtrate B;
(3) washing and drying the filter cake A and the filter cake B;
(4) and uniformly mixing the dried filter cake A and the dried filter cake B to obtain the self-gelling fiber composite material.
In the technical scheme of the invention, the phosphogypsum is used as a raw material in the step (1), the crystallization assistant is added, the mixture is added into an acid solution, the mixture is stirred and reacted at a certain temperature, the reaction temperature is 80-90 ℃, the reaction time is 3-4 hours, the product is filtered when the reaction is finished, and a filter cake A and a filtrate A are obtained
CaSO 4 ·2H 2 O (granule) + HCl ═ Ca 2+ +Cl - +SO 4 2- +2H 2 O (1)
2) Cooling and crystallizing the filtrate A, and then filtering to obtain a filter cake B and a filtrate B, wherein the main reaction is
Ca 2+ +SO 4 2- +2H 2 O＝＝CaSO 4 ·2H 2 O (fiber) (2)
3) Washing and drying the filter cake A and the filter cake B; the drying temperature is 45 ℃.
4) And uniformly mixing the dried filter cake A and the dried filter cake B to obtain the self-gelling fiber cement-based composite material, wherein the filter cake B is the microfiber calcium sulfate dihydrate whisker, and the filter cake A is siliceous slag.
Filtering the obtained filtrate B, and returning to the step 1) for circularly dissolving the phosphogypsum.
The self-gelling calcium sulfate fiber composite material can achieve the effects of strengthening and toughening cement by the existence of calcium sulfate fibers.
The self-gelling fiber composite material contains silica fume which can spontaneously consume hydration products Ca (OH) after meeting water 2 The adhesive property between the microfiber calcium sulfate whisker and a cement matrix is obviously improved, and the interface bonding strength of the microfiber calcium sulfate whisker and the cement matrix is enhanced, so that the number of pores in the cement material is reduced, and the toughness and strength of the cement material are improved.
The technical scheme of the invention adopts phosphogypsum as a raw material, uses an acid solution dissolution recrystallization method and uses organic acid as a crystallization promoter to prepare the calcium sulfate whisker containing siliceous ash and slag with a length-diameter ratio, and the calcium sulfate whisker is mixed and added into a cement material, so that the microfiber calcium sulfate whisker improves the strength and toughness of the cement.
The existence of the waterborne polyurethane and the whole preparation process lead the obtained silica fume to have strong adhesion, the silica fume slag optimizes the dispersibility of the calcium sulfate whisker in the cement matrix and consumes Ca (OH) generated by cement hydration 2 The self-gelling function is generated, so that cracks existing between fibers and cement are effectively reduced, and the strength and the toughness of the cement are further improved.
Realizes the reutilization of wastes and effectively relieves the problem of phosphogypsum stockpiling.
The chemical reagent is recycled, and the process production cost is saved.
The whole production process is simple to operate.
Detailed Description
According to the self-gelling fiber composite material and the preparation method thereof, the phosphogypsum is treated by adopting a chemical reagent recycling process to prepare the calcium sulfate whisker and the filter residue containing the siliceous dust, and the calcium sulfate whisker and the siliceous filter residue are mixed and added into the cement material, so that the strength and toughness of the cement are remarkably improved, and the problem of stacking the phosphogypsum is solved.
To better illustrate the above embodiments, the following examples are given, without limiting the scope of the invention to the examples given, and the phosphogypsum used in the examples is produced by Hakko chemical Co., Ltd, the ingredients are listed below:
table 1: phosphogypsum components:
example 1
1) Weighing 350g of phosphogypsum and 7g of citric acid, uniformly mixing, adding into a reaction kettle, pouring 8750ml of solution with the solid-to-liquid ratio of 0.04, wherein the solution contains 6.0% of hydrochloric acid, adding water polyurethane to ensure that the concentration of the water polyurethane in the mixed solution is 100g/L, reacting for 3h at 80 ℃, and filtering while hot to obtain a filtrate A and a filter cake A.
2) And cooling and crystallizing the filtrate A at room temperature for 12 hours, then filtering to obtain filtrate B and a filter cake B, and returning the filtrate B to the previous step for recycling.
3) And respectively washing and filtering the filter cake A and the filter cake B, and drying at 45 ℃, wherein the filter cake A is siliceous ash, and the filter cake B is microfiber calcium sulfate dihydrate whisker.
4) The siliceous clinker and the microfibrous calcium sulfate dihydrate whisker are mixed to prepare the self-gelling fiber composite material-1 which is named as A-1, wherein the length-diameter ratio of the microfibrous calcium sulfate dihydrate whisker in the A-1 is 68.7, and the viscosity of the siliceous clinker is 43.1 mpa.s.
Example 2
1) Weighing 350g of phosphogypsum and 70000g of citric acid, uniformly mixing, adding into a reaction kettle, pouring 7000ml of solution with a solid-to-liquid ratio of 0.05, adding water polyurethane into the solution until the concentration of the hydrochloric acid is 7.0 percent, reacting for 3h at 80 ℃ until the concentration of the water polyurethane in the mixed solution is 150g/L, and filtering while the solution is hot to obtain filtrate A and filter cake A.
2) And cooling and crystallizing the filtrate A at room temperature for 12 hours, then filtering to obtain filtrate B and a filter cake B, and returning the filtrate B to the previous step for recycling.
3) Washing and filtering the filter cake A and the filter cake B, and drying at 45 ℃, wherein the filter cake A is clinker-containing slag, and the filter cake B is microfiber calcium sulfate dihydrate whisker.
4) The siliceous clinker and the microfibrous calcium sulfate dihydrate whisker are mixed to prepare the self-gelling fiber composite material-2 which is named as A-2, wherein the length-diameter ratio of the microfibrous calcium sulfate dihydrate whisker in the A-2 is 68.1, and the viscosity of the siliceous clinker is 45.5 mpa.s.
Example 3
1) Weighing 350g of phosphogypsum and 3.5g of citric acid, uniformly mixing, adding into a reaction kettle, pouring 5000ml of solution with the solid-to-liquid ratio of 0.07, wherein the solution contains 7.3% of hydrochloric acid, adding water polyurethane to ensure that the concentration of the water polyurethane in the mixed solution is 200g/L, reacting for 4 hours at 90 ℃, and filtering while hot to obtain filtrate A and filter cake A.
2) And cooling and crystallizing the filtrate A at room temperature for 24 hours, then filtering to obtain filtrate B and a filter cake B, and returning the filtrate B to the previous step for recycling.
3) And washing and filtering the filter cake A and the filter cake B, and drying at 45 ℃, wherein the filter cake A is siliceous ash and the filter cake B is microfiber calcium sulfate dihydrate whisker.
4) The siliceous slag and the microfibrous calcium sulfate dihydrate whisker are mixed to prepare the self-gelling fiber composite material-3 which is named as A-3, wherein the length-diameter ratio of the microfibrous calcium sulfate dihydrate whisker in the A-3 is 73.4, and the viscosity of the siliceous slag is 46.6 mpa.s.
Example 4
1) Weighing 350g of phosphogypsum and 3.5g of polyacrylic acid, uniformly mixing, adding into a reaction kettle, pouring 3500ml of solution with the solid-to-liquid ratio of 0.1, wherein the solution contains 8.0% of hydrochloric acid, adding water polyurethane to ensure that the concentration of the water polyurethane in the mixed solution is 300g/L, reacting for 4 hours at 90 ℃, and filtering while hot to obtain filtrate A and filter cake A.
2) And cooling and crystallizing the filtrate A at room temperature for 24 hours, then filtering to obtain filtrate B and a filter cake B, and returning the filtrate B to the previous step for recycling.
3) And washing and filtering the filter cake A and the filter cake B, and drying at 45 ℃, wherein the filter cake A is siliceous ash and the filter cake B is microfiber calcium sulfate dihydrate whisker. The microfiber calcium sulfate dihydrate whisker had a property of 64.3.
4) The siliceous slag and the microfibrous calcium sulfate dihydrate whisker are mixed to prepare the self-gelling fiber composite material-4 which is named as A-4, wherein the length-diameter ratio of the microfibrous calcium sulfate dihydrate whisker in the A-4 is 64.3, and the viscosity of the siliceous slag is 47.6 mpa.s.
Example 5
The method and the steps are the same as the example 1, only sulfuric acid is used as an acid solution, anhydrous polyurethane is added, the property of the microfiber calcium sulfate dihydrate whisker is 7.2, and the viscosity of silica fume is 3.3 mpa.s.
Example 6
The method and the steps are the same as the example 1, only polyurethane is added to the concentration of 20g/L, the property of the microfiber calcium sulfate dihydrate whisker is 61.1, and the viscosity of the silica fume is 38.2 mpa.s.
Example 7
The method and the steps are the same as the example 1, only polyurethane is added until the concentration is 50g/L, the property of the microfiber calcium sulfate dihydrate whisker is 63.3, and the viscosity of the silica fume slag is 41.4 mpa.s.
Example 8
The method and the steps are the same as the example 1, only polyurethane is added to the concentration of 400g/L, the property of the microfiber calcium sulfate dihydrate whisker is 64.7, and the viscosity of the silica fume slag is 55.8 mpa.s.
Example 9
The method and the steps are the same as the example 1, only polyurethane is added to the concentration of 500g/L, the property of the microfiber calcium sulfate dihydrate whisker is 63.1, and the viscosity of the silica fume slag is 58.1 mpa.s.
Example 10
The method and the steps are the same as the example 1, only polyurethane is added to the concentration of 600g/L, the property of the microfiber calcium sulfate dihydrate whisker is 64.2, and the viscosity of the silica fume slag is 59.9 mpa.s.
The self-gelling fiber composite materials 1-10 prepared by the scheme are mixed according to the mass ratio of 10% and respectively added into cement P.O42.5, molding mortar test blocks according to the proportion specified in the national standard cement mortar strength test method (ISO method) and maintaining for 28 days, and the porosity, the compressive strength and the bending strength of the molded mortar test blocks are tested, wherein the performance test results are shown in Table 2:
table 2: results of Performance testing
| Examples | Resistance to compression (MPa) | Anti-fracture (MPa) | Porosity (%) |
| Example 1 | 68.7 | 11.8 | 16.5 |
| Example 2 | 69.5 | 11.9 | 15.2 |
| Example 3 | 65.7 | 12.1 | 14.1 |
| Example 4 | 61.8 | 12.4 | 13.7 |
| Example 5 | 51.4 | 8.4 | 36.6 |
| Example 6 | 65.3 | 10.9 | 27.1 |
| Example 7 | 66.7 | 11.3 | 24.0 |
| Example 8 | 53.4 | 11.6 | 12.8 |
| Example 9 | 50.9 | 10.8 | 10.4 |
| Example 10 | 49.7 | 10.5 | 6.2 |
Claims (6)
1. The preparation method of the self-gelling fiber composite material is characterized by comprising the following steps of:
(1) adding a crystallization promoter into phosphogypsum serving as a raw material, adding the phosphogypsum into an acid solution, stirring and reacting at a certain temperature, and filtering a product while the product is hot after the reaction is finished to obtain a filter cake A and a filtrate A;
(2) cooling and crystallizing the filtrate A, and filtering to obtain a filter cake B and a filtrate B;
(3) washing and drying the filter cake A and the filter cake B;
(4) and uniformly mixing the dried filter cake A and the dried filter cake B to obtain the self-gelling fiber composite material.
2. The preparation method of the self-gelling fiber composite material according to claim 1, wherein the crystallization promoter in the step (1) is citric acid or polyacrylic acid, and the mass ratio of the phosphogypsum to the crystallization promoter is 1: 50-200.
3. The method for preparing self-gelling fiber composite material according to claim 1, wherein the acid solution in step (1) is hydrochloric acid solution or nitric acid solution, wherein the solid-to-liquid ratio of phosphogypsum to the acid solution is 0.03-0.1, and the concentration of the acid solution is controlled to be 6% -8%.
4. The method for preparing the self-gelling fiber composite material according to claim 1, wherein the stirring reaction temperature in the step (1) is 80-90 ℃ and the reaction time is 3-4 hours.
5. The method for preparing the self-gelling fiber composite material according to claim 1, wherein a tackifier is further added in the step (1), and the tackifier is polyurethane.
6. The method of preparing a self-gelling fiber composite according to claim 1, wherein the concentration of the tackifier is 50 to 500 g/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115432986A (en) * | 2022-09-28 | 2022-12-06 | 宜都兴发化工有限公司 | Preparation method of high-strength water-permeable composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115432986A (en) * | 2022-09-28 | 2022-12-06 | 宜都兴发化工有限公司 | Preparation method of high-strength water-permeable composite material |
| CN115432986B (en) * | 2022-09-28 | 2023-10-24 | 宜都兴发化工有限公司 | Preparation method of high-strength water-permeable composite material |
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Inventor after: Zhu He Inventor after: Zheng Guangming Inventor after: Li Fang Inventor after: Wang Fengling Inventor after: Sun Hualin Inventor after: Zhao Chunyang Inventor before: Zhu He Inventor before: Zheng Guangming Inventor before: Li Fang Inventor before: Wang Fengling Inventor before: Sun Hualin Inventor before: Zhao Chunyang |
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