CN113278306A - Microwave wet-method modified artificial granite waste residue and recycling process method thereof - Google Patents
Microwave wet-method modified artificial granite waste residue and recycling process method thereof Download PDFInfo
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- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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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
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a recycling process method for modifying artificial granite waste residues by a microwave wet method, which comprises the following steps: step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 1-12 parts by mass of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate; step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, and adding a composite modifier to fully grind for 10-15 min; carrying out auxiliary modification on the slurry for 15-30 min by microwaves with the frequency of 915MHZ and the power of 0.5-1 kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder. The invention can efficiently realize the resource utilization of the artificial granite waste residue.
Description
Technical Field
The invention relates to the technical field of recycling of building material wastes, in particular to microwave/wet modified artificial granite waste residue and a recycling process method thereof.
Background
The artificial granite mainly takes calcium carbonate ore powder and unsaturated polyester resin as main raw materials, and is formed into a final product through the steps of stirring, mixing, pressing, curing, forming, cutting, polishing and the like, wherein the unsaturated polyester resin is mainly prepared by polycondensation of dibasic acid (or anhydride) and dihydric alcohol under the action of an initiator and an accelerator. The waste artificial granite slag is produced through precipitation and press filtering of a great amount of waste slurry produced in cutting and polishing. The solid content of the artificial granite waste residue after filter pressing is about 80%, and the solid content comprises 90-92 parts of calcium carbonate and 7-9 parts of thermosetting unsaturated resin. In view of the complex structure of the artificial granite waste residue, a low-cost and large-batch resource utilization method is still lacking at present. Nowadays, enterprises generally adopt simple landfill and open-air stacking, a large amount of precious land resources are occupied, and meanwhile, generated volatile organic compounds and powder are scattered, so that secondary pollution is caused to the environment, the key factor which troubles the sustainable development of the enterprises is achieved, and meanwhile, the resources are also huge waste.
Chinese patent CN 201910343506.5 discloses a polymer composite filled with artificial granite waste residue and a preparation method thereof, wherein the artificial granite waste residue after drying and crushing is directly subjected to composite modification with one of polyvinyl alcohol, polyurethane, polyamide and the like. The method is applied to production enterprises, and still has the problems that the artificial granite waste residue can be treated only by additionally setting separate devices such as drying and crushing, the artificial granite waste residue is not modified, and the compatibility between the artificial granite waste residue and an organic compound is poor.
Chinese patent CN 201910592897.4 discloses a plastic product based on artificial marble waste residue filler and a preparation method thereof, wherein the method utilizes coupling agents such as aluminate, borate, titanate, phosphate and the like to modify the artificial marble waste residue, and then the modified artificial marble waste residue is blended with resin to prepare the plastic product. The method also does not consider the problem of drying and crushing the artificial granite waste residue in the early stage, and the coating of the calcium carbonate particles by the existing thermosetting unsaturated resin in the artificial granite waste residue can directly influence the modification treatment effect in the dry modification process.
In the prior art, the treatment of the artificial granite waste residue is carried out by drying and then modifying, while the solid content of the artificial granite waste residue after pressure filtration is about 80 percent, the traditional method needs to consume a large amount of manpower and material resources for evaporation and drying, and then the artificial granite waste residue can be used only by further crushing and grading, and the dry modification uniformity is lower than that of the wet modification.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a microwave wet-method modified artificial granite waste residue and a recycling process method thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: a method for modifying artificial granite waste residue by microwave/wet method comprises the following steps:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 1-12 parts of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, and adding a composite modifier to fully grind for 10-15 min; carrying out auxiliary modification on the slurry for 15-30 min by passing the slurry through a microwave with the frequency of 915MHZ and the power of 0.5-1 kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
Microwave has selective effect on substances, only polar molecules can be polarized by microwave to generate heat effect, the microwave can accelerate mass transfer speed in a medium, influence of internal diffusion is eliminated, heat efficiency and heating speed are greatly improved, and necessary reaction environment is provided for modification. The microwave excites the molecules in the substance to perform ultrahigh frequency vibration and friction, so that the 'violent stirring' on the molecular level is realized to generate the 'excitation effect', the surface activation of the powder is promoted to be combined with the modifier more effectively, and the aim of microwave-assisted modification is fulfilled. The ester bond of the unsaturated polyester part of the granite waste residue can be broken and opened under the action of microwave to realize activation, and the polyester can realize crosslinking with hydroxyl on the surface of calcium carbonate, water-soluble titanate coupling agent molecules and water-soluble titanate chelate molecules, so that the polyester is favorable for quick bonding and modification.
Further, the drying treatment is to dry the modified slurry by microwaves with the frequency of 915MHZ and the power of 1.5-1.8 kw and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
Further, the artificial granite waste residue comprises the following components: 88-93 parts by mass of calcium carbonate and 7-12 parts by mass of thermosetting unsaturated resin.
Further, the composite modifier comprises the following components: 0.5-2 parts of water-soluble titanate coupling agent, 0.05-1 part of silane coupling agent, 0.5-1.5 parts of water-based titanate chelate, 0.05-0.3 part of fatty alcohol-polyoxyethylene ether, 0.75-3 parts of stearic acid and 0.5-2 parts of polyethylene wax.
The invention has the advantages that: the wet modification is carried out by microwave assistance, the waste residue modification effect is enhanced, the microwave equipment can complete the two-step processes of modification and drying to improve the utilization rate and efficiency, modified waste residue slurry or modified waste residue powder can be produced without additionally adding equipment, the manpower and material resources are saved, the modified waste residue slurry can be used in the industries of inorganic artificial stones, coatings and the like, the modified waste residue powder can be applied to fillers of plastics, rubber and the like, and the resource utilization of the artificial granite waste residue is efficiently realized.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
Embodiment 1. a method for modifying artificial granite waste residue by microwave/wet method, the manufacturing process comprises:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 1 part by mass of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, and adding a composite modifier to fully grind for 10 min; carrying out auxiliary modification on the slurry for 15min by microwaves with the frequency of 915MHZ and the power of 1kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In this embodiment, the drying process is to dry the modified slurry with microwaves of frequency 915MHZ and power 1.5kw, and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
In this embodiment, the temperature during modification is controlled to be 75-95 ℃, and the temperature during drying is controlled to be 100-135 ℃.
In this embodiment, the artificial granite waste residue comprises the following components: 88 parts by mass of calcium carbonate and 7 parts by mass of a thermosetting unsaturated resin.
In this embodiment, the composite modifier comprises the following components: 0.5 part of water-soluble titanate coupling agent, 0.05 part of silane coupling agent, 0.5 part of aqueous titanate chelate, 0.05 part of fatty alcohol-polyoxyethylene ether, 0.75 part of stearic acid and 0.5 part of polyethylene wax.
Comparative example 1, the manufacturing process of the artificial granite waste residue modified by the common wet method comprises the following steps:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 1 part by mass of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, adding a composite modifier, and fully grinding for 10min to modify the slurry to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In this comparative example, the artificial granite waste residue comprises the following components: 88 parts by mass of calcium carbonate and 7 parts by mass of a thermosetting unsaturated resin.
In this comparative example, the composite modifier components were: 0.5 part of water-soluble titanate coupling agent, 0.05 part of silane coupling agent, 0.5 part of aqueous titanate chelate, 0.05 part of fatty alcohol-polyoxyethylene ether, 0.75 part of stearic acid and 0.5 part of polyethylene wax.
The modified artificial granite waste residue powders prepared in the above example 1 and comparative example 1 were subjected to oil absorption value measurement.
The reagent for measuring the oil absorption value is dioctyl phthalate DOP.
Weighing about 5g of powder sample, accurately measuring to 0.01g, placing on a glass plate or a glazed porcelain plate, and dripping DOP into a dropping bottle which is wiped by a known substance and contains DOP. During the dropping, the sample is continuously stirred and ground by using the adjustable knife, the sample is dispersed at first, and then the sample is gradually agglomerated until the sample is completely wetted by DOP, and the end point is formed.
The oil absorption value is expressed as the mass (g) of DOP absorbed per 100g of calcium carbonate
| Waste residue of granite (Dry) | Common wet modification | Microwave-assisted wet modification | |
| Oil absorption number | 37.28g | 26.34g | 22.81g |
After modification treatment, the oil absorption value of the granite waste residue is obviously reduced, and under the same formula condition, the oil absorption value of the modified powder body by microwave assistance is superior to that of the common wet modification.
Testing HDPE standard sample strip prepared by filling 30 parts of powder, and comparing tensile strength
The method has the advantages that the direct filling of plastic by untreated granite waste residues can affect the tensile property, the granite waste residues cannot be directly used, the granite waste residues can be used as a filler to be applied to plastic products only by modification treatment, and the microwave auxiliary effect is better after the granite waste residues are treated by the modifier with the same formula.
Embodiment 2. a method for preparing microwave/wet modified artificial granite waste residue, the preparation process comprises:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 12 parts of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, and adding a composite modifier to fully grind for 15 min; carrying out auxiliary modification on the slurry for 30min by microwaves with the frequency of 915MHZ and the power of 0.5kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In this embodiment, the drying process is to dry the modified slurry with microwaves at a frequency of 915MHZ and a power of 1.7kw, and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
In this embodiment, the temperature during modification is controlled to be 75-95 ℃, and the temperature during drying is controlled to be 100-135 ℃.
In this embodiment, the artificial granite waste residue comprises the following components: 93 parts by mass of calcium carbonate and 12 parts by mass of a thermosetting unsaturated resin.
In this embodiment, the composite modifier comprises the following components: 2 parts of water-soluble titanate coupling agent, 1 part of silane coupling agent, 1.5 parts of water-based titanate chelate, 0.3 part of fatty alcohol-polyoxyethylene ether, 3 parts of stearic acid and 2 parts of polyethylene wax.
Comparative example 2. a method for preparing microwave/wet modified artificial granite waste residue, the preparation process comprises:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 12 parts of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, adding a composite modifier, and fully grinding for 15min for modification to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In the comparative example, the drying treatment is to dry the modified slurry by microwave equipment and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
In a comparative example, the artificial granite waste residue comprises the following components: 93 parts by mass of calcium carbonate and 12 parts by mass of a thermosetting unsaturated resin.
In the comparative example, the composite modifier components were: 2 parts of water-soluble titanate coupling agent, 1 part of silane coupling agent, 1.5 parts of water-based titanate chelate, 0.3 part of fatty alcohol-polyoxyethylene ether, 3 parts of stearic acid and 2 parts of polyethylene wax.
The modified artificial granite waste residue powders prepared in the above example 2 and comparative example 2 were subjected to oil absorption value measurement.
The reagent for measuring the oil absorption value is dioctyl phthalate DOP.
Weighing about 5g of powder sample, accurately measuring to 0.01g, placing on a glass plate or a glazed porcelain plate, and dripping DOP into a dropping bottle which is wiped by a known substance and contains DOP. During the dropping, the sample is continuously stirred and ground by using the adjustable knife, the sample is dispersed at first, and then the sample is gradually agglomerated until the sample is completely wetted by DOP, and the end point is formed.
The oil absorption value is expressed as the mass (g) of DOP absorbed per 100g of calcium carbonate
| Waste residue of granite (Dry) | Common wet modification | Microwave-assisted wet modification | |
| Oil absorption number | 37.28g | 26.34g | 22.52g |
After modification treatment, the oil absorption value of the granite waste residue is obviously reduced, and under the same formula condition, the oil absorption value of the modified powder body by microwave assistance is superior to that of the common wet modification.
Testing HDPE standard sample strip prepared by filling 30 parts of powder, and comparing tensile strength
The method has the advantages that the direct filling of plastic by untreated granite waste residues can affect the tensile property, the granite waste residues cannot be directly used, the granite waste residues can be used as a filler to be applied to plastic products only by modification treatment, and the microwave auxiliary effect is better after the granite waste residues are treated by the modifier with the same formula.
Embodiment 3. a method for modifying artificial granite waste residue by microwave/wet method, the manufacturing process comprises:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 7 parts of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, and adding a composite modifier to fully grind for 13 min; carrying out auxiliary modification on the slurry for 25min by microwaves with the frequency of 915MHZ and the power of 0.8kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In this embodiment, the drying process is to dry the modified slurry with microwaves at a frequency of 915MHZ and a power of 1.8kw, and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
In this embodiment, the temperature during modification is controlled to be 75-95 ℃, and the temperature during drying is controlled to be 100-135 ℃.
In this embodiment, the artificial granite waste residue comprises the following components: 88 parts by mass of calcium carbonate and 7 parts by mass of a thermosetting unsaturated resin.
In this embodiment, the composite modifier comprises the following components: 1.5 parts of water-soluble titanate coupling agent, 0.6 part of silane coupling agent, 1.2 parts of aqueous titanate chelate, 0.15 part of fatty alcohol-polyoxyethylene ether, 2.1 parts of stearic acid and 1.4 parts of polyethylene wax.
Comparative example 3. A method for modifying artificial granite waste residue by microwave/wet method comprises the following steps:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 7 parts of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by a colloid mill to form slurry with the solid content of 50%, adding a composite modifier, and fully grinding for 13min for modification to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
In the comparative example, the drying treatment is to dry the modified slurry by microwave equipment and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
In this comparative example, the artificial granite waste residue comprises the following components: 88 parts by mass of calcium carbonate and 7 parts by mass of a thermosetting unsaturated resin.
In this comparative example, the composite modifier components were: 1.5 parts of water-soluble titanate coupling agent, 0.6 part of silane coupling agent, 1.2 parts of aqueous titanate chelate, 0.15 part of fatty alcohol-polyoxyethylene ether, 2.1 parts of stearic acid and 1.4 parts of polyethylene wax.
The modified artificial granite waste residue powders prepared in the above example 3 and comparative example 3 were subjected to oil absorption value measurement.
The reagent for measuring the oil absorption value is dioctyl phthalate DOP.
Weighing about 5g of powder sample, accurately measuring to 0.01g, placing on a glass plate or a glazed porcelain plate, and dripping DOP into a dropping bottle which is wiped by a known substance and contains DOP. During the dropping, the sample is continuously stirred and ground by using the adjustable knife, the sample is dispersed at first, and then the sample is gradually agglomerated until the sample is completely wetted by DOP, and the end point is formed.
The oil absorption value is expressed as the mass (g) of DOP absorbed per 100g of calcium carbonate
| Waste residue of granite (Dry) | Common wet modification | Microwave-assisted wet modification | |
| Oil absorption number | 37.28g | 26.34g | 22.82g |
After modification treatment, the oil absorption value of the granite waste residue is obviously reduced, and under the same formula condition, the oil absorption value of the modified powder body by microwave assistance is superior to that of the common wet modification.
Testing HDPE standard sample strip prepared by filling 30 parts of powder, and comparing tensile strength
The method has the advantages that the direct filling of plastic by untreated granite waste residues can affect the tensile property, the granite waste residues cannot be directly used, the granite waste residues can be used as a filler to be applied to plastic products only by modification treatment, and the microwave auxiliary effect is better after the granite waste residues are treated by the modifier with the same formula.
Although the invention has been described in detail above with reference to specific embodiments, it will be apparent to one skilled in the art that modifications or improvements may be made based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (4)
1. A recycling process method for modifying artificial granite waste residue by a microwave wet method is characterized by comprising the following steps: the method comprises the following steps:
step 1, preparing raw materials, wherein the raw materials comprise: 100 parts of artificial granite waste residue; 1-12 parts by mass of a composite modifier; the composite modifier comprises a water-soluble titanate coupling agent and a water-soluble titanate chelate;
step 2, adding water into the artificial granite waste residue, grinding the mixture by using a colloid mill to form slurry with the solid content of 45-55%, and adding a composite modifier to fully grind for 10-15 min; carrying out auxiliary modification on the slurry for 15-30 min by microwaves with the frequency of 915MHZ and the power of 0.5-1 kw to obtain modified slurry; and drying the modified slurry and then crushing to obtain modified artificial granite waste residue powder.
2. The process method for recycling artificial granite waste residue through microwave wet modification according to claim 1, characterized in that: and the drying treatment is to dry the modified slurry by microwaves with the frequency of 915MHZ and the power of 1.5-1.8 kw and then crush the dried modified slurry to obtain modified artificial granite waste residue powder.
3. The process method for recycling artificial granite waste residue through microwave wet modification according to claim 1, characterized in that: the artificial granite waste residue comprises the following components: 88-93 parts by mass of calcium carbonate and 7-12 parts by mass of thermosetting unsaturated resin.
4. The process method for recycling artificial granite waste residue through microwave wet modification according to claim 1, characterized in that: the composite modifier comprises the following components: 0.5-2 parts of water-soluble titanate coupling agent, 0.05-1 part of silane coupling agent, 0.5-1.5 parts of water-based titanate chelate, 0.05-0.3 part of fatty alcohol-polyoxyethylene ether, 0.75-3 parts of stearic acid and 0.5-2 parts of polyethylene wax.
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| CN114276727A (en) * | 2021-11-20 | 2022-04-05 | 广西科学院 | Waterproof and anti-fouling water-based paint based on waste artificial granite powder and preparation method thereof |
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