CN115260385B - Preparation method of gold tailing powder modifier, obtained product and application - Google Patents
Preparation method of gold tailing powder modifier, obtained product and application Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
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- C08F2/06—Organic solvent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/405—Compounds of aluminium containing combined silica, e.g. mica
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a preparation method of a gold tailing powder modifier, an obtained product and application thereof. The modifier is simple to prepare and low in cost, can realize a good modification effect by simply reacting with the gold tailing powder, enables the surface of the gold tailing powder to be provided with polar groups such as carboxyl, amino, hydroxyl and epoxy groups, greatly improves the compatibility of the gold tailing powder with high polymer organic materials, overcomes the defect of application of the gold tailing powder in the field of building materials, and has a relatively wide application prospect in the aspect of modifying inorganic powder.
Description
Technical Field
The invention relates to a preparation method of a gold tailing powder modifier, an obtained product and application thereof, and belongs to the technical field of processing aids.
Background
Gold tailings are solid waste discharged after gold or other useful components are recovered through a gold extraction process. In general, gold tailings are alkaline and have a pH > 10. Gold tailings contain relatively high levels of silica and alumina, along with amounts of iron oxide, calcium oxide, magnesium oxide, small amounts of precious metals (e.g., gold, silver), heavy metals (e.g., copper, lead, zinc), and residual cyanide and flotation agents. With continuous gold exploitation, the accumulation amount of gold tailings is increased year by year, so that a large amount of land is wasted, the surrounding environment is damaged, and the human health is endangered. The comprehensive utilization of gold tailings has important significance for the healthy development and natural resource protection of the gold industry.
The gold tailings are mainly characterized by containing more than 60% of inorganic minerals such as silicon aluminum oxide and the like, and the components of the gold tailings are close to the raw material components of a plurality of building material products, so the gold tailings are widely used in the field of building materials. The building material is mixed with high molecular material and small amount of other auxiliary additives, and the mixture is treated with certain technology to obtain ideal building material. But the gold tailing powder has poor compatibility with commonly used high polymer materials, can influence the mechanical properties of building materials, has higher hardness, and is easy to damage a die in the preparation process, thereby limiting the application of the gold tailing powder in the field of building materials.
Disclosure of Invention
Aiming at the application status of gold tailing powder, the invention provides a preparation method of a gold tailing powder modifier and an obtained product, wherein raw materials containing polar groups such as carboxyl, amino, hydroxyl, epoxy groups and the like are selected in the method, and react according to the method, and the obtained modifier contains a large number of polar groups such as carboxyl, amino, hydroxyl, epoxy groups and the like, and the polar groups can not only react with inorganic component surface groups in the gold tailing powder, but also generate interactions such as hydrogen bond, complexation, static electricity and the like, so that the gold tailing powder surface is provided with the polar groups such as carboxyl, amino, hydroxyl, epoxy groups and the like, the compatibility of the gold tailing powder and a high polymer organic material is greatly improved, and the defect of the application of the gold tailing powder in the field of building materials is overcome.
The specific technical scheme of the invention is as follows:
the preparation method of the gold tailing powder modifier comprises the following steps:
(1) Stirring butyl methacrylate and a solvent uniformly, and then adding an initiator to react;
(2) Adding glycidyl methacrylate, acrylamide, hydroxyethyl methacrylate, vinyl pyrrolidone and oleic acid into the mixture in the step (1) to continue the reaction;
(3) And adding an organic solvent into the reacted mixture to precipitate, and drying the obtained precipitate to obtain the gold tailing powder modifier.
The invention takes butyl methacrylate, oleic acid, hydroxyethyl methacrylate, glycidyl methacrylate, acrylamide and vinyl pyrrolidone as raw materials, and the multicomponent copolymer gold tailing powder modifier is obtained through polymerization reaction. Wherein the mass ratio of the butyl methacrylate to the glycidyl methacrylate to the acrylamide to the hydroxyethyl methacrylate to the vinylpyrrolidone to the oleic acid is 1:0.05-0.2:0.01-0.05:0.05-0.1:0.01-0.05:0.05-0.1. Under the relation of the dosage, the obtained modifier has better modifying effect on the gold tailings, the modified gold tailings have better compatibility with the high polymer organic material, and the mechanical property of the building material prepared from the gold tailings and the high polymer organic material can be improved.
Further, in the step (1), the solvent is a mixture of absolute ethyl alcohol and ethyl acetate. Preferably, the volume ratio of absolute ethanol to ethyl acetate is from 1:0.5 to 10, for example from 1:0.5, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, more preferably from 1:0.5 to 3. Within the preferred range, the method has the advantages of good reaction effect, easy purification of the product, high product yield and the like.
Further, in the step (1), the initiator is dibenzoyl peroxide or azobisisobutyronitrile. The initiator is generally used in an amount of 0.1% to 1.5% by mass, preferably 1% to 1.5% by mass, based on the mass of butyl methacrylate.
Further, in the step (1), the reaction temperature is 55℃to 75℃and preferably 60℃to 70 ℃. The reaction time is 30-60min.
Further, in step (1), the concentration of butyl methacrylate in the solvent is 1 to 8wt%, for example 1wt%, 4wt%, 8wt%.
Further, in the step (2), after glycidyl methacrylate, acrylamide, hydroxyethyl methacrylate, vinyl pyrrolidone and oleic acid are added, the reaction is continued for 4 to 9 hours at 55 to 75 ℃.
Further, in both steps (1) and (2), the reaction is carried out under a gas atmosphere, and the shielding gas may be nitrogen or an inert gas such as argon.
Further, in the step (3), the organic solvent is n-hexane. And adding n-hexane into the mixture after the reaction to precipitate, and drying after the precipitation, so as to obtain a white amorphous product, namely the gold tailing powder modifier. Wherein the drying temperature is generally 60-70 ℃.
Furthermore, the gold tailing powder modifier prepared by the method contains a large number of polar groups such as carboxyl, amino, hydroxyl, epoxy and the like, and the structural formula of the gold tailing powder modifier is as follows:
wherein m, n, o, p, q, r is the degree of polymerization of each repeating unit.
Further, the invention also provides a modification method of the gold tailing powder, which comprises the following steps: mixing the gold tailing powder with the prepared gold tailing powder modifier, and stirring and reacting for 15-30min at 110-130 ℃ to obtain modified gold tailing powder.
Further, the gold tailing powder and the gold tailing powder modifier are mixed in a high-speed mixer, the mixing and stirring speed is 40-60r/min, the modifier is uniformly coated on the surface of the gold tailing powder in the high-speed mixer through stirring, and the polar groups of the modifier can interact with the surface groups of inorganic components in the gold tailing powder under the heating condition.
Furthermore, in order to better disperse and mix the gold tailing powder and the gold tailing powder modifier, a low-boiling-point organic solvent can be added in the mixing process, and the low-boiling-point organic solvent aims to improve the dispersibility of the raw materials, so long as the organic solvent with better solubility to the modifier and a boiling point lower than the reaction temperature is adopted, for example, the organic solvent can be tetrahydrofuran, cyclohexane, ethyl acetate, acetone and the like. The amount of the organic solvent may be selected as desired, as long as the modifier is sufficiently dissolved.
The invention synthesizes a multi-component copolymer gold tailing powder modifier under the action of a solvent environment and an initiator by taking butyl methacrylate, oleic acid, hydroxyethyl methacrylate, glycidyl methacrylate, acrylamide and vinyl pyrrolidone as raw materials. Compared with the prior art, the invention has the following beneficial effects:
1. the raw materials selected by the invention are environment-friendly, and contain a large number of polar groups such as carboxyl, amino, hydroxyl, epoxy and the like, the polar groups can not only react with the surface groups of inorganic components in the gold tailing powder body, but also generate interactions such as hydrogen bonds, complexation, static electricity and the like, in addition, the modifier also contains longer alkyl chains, and the long alkyl chains can interact with high polymer organic materials (such as matrix resin) so that the modification effect is better.
2. The method has the advantages of simple operation, single step, low cost and wide application prospect in the aspect of modifying inorganic powder.
3. The gold tailing powder modifier can be modified by mixing with the gold tailing powder under heating, is simple to operate, greatly improves the compatibility of the modified gold tailing powder with high-molecular organic materials, and has better application prospect in the field of building materials.
Drawings
FIG. 1 is a graph showing the dispersion of the modified gold tailing powder of example 1 in different solvents, wherein (a) is unmodified gold tailing powder and (b) is modified gold tailing powder.
Fig. 2 is a graph of the internal mixing time torque for different samples.
Detailed Description
The present invention will be described in further detail with reference to specific examples. In the following examples, materials such as ethyl acetate, absolute ethyl alcohol, butyl methacrylate, oleic acid, hydroxyethyl methacrylate, glycidyl methacrylate, acrylamide and vinylpyrrolidine were commercially available.
Example 1
(1) 50g of ethyl acetate, 4g of butyl methacrylate (volume ratio 1:1.2) and azodiisobutyronitrile as an initiator with the weight percent of 1 percent of butyl methacrylate are added into a reactor provided with a stirring device, a condensation return pipe and nitrogen. The reactor was placed in a 70 ℃ water bath to control the polymerization system temperature.
(2) After reacting for 1h, 0.4g glycidyl methacrylate, 0.1g acrylamide, 0.2g hydroxyethyl methacrylate, 0.1g vinyl pyrrolidone and 0.2g oleic acid are added, and the mixture is subjected to heat preservation and polymerization for 6h, and then is cooled and discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Example 2
A gold tailings powder modifier was prepared as in example 1, except that: in the step (1), the amount of butyl methacrylate was 8g, in the step (2), the amount of glycidyl methacrylate added was 1.6g, the amount of acrylamide added was 0.08g, the amount of hydroxyethyl methacrylate added was 0.8g, the amount of vinylpyrrolidone added was 0.08g, and the amount of oleic acid added was 0.8g.
Example 3
A gold tailings powder modifier was prepared as in example 1, except that: in the step (2), the added amount of glycidyl methacrylate was 0.2g, the added amount of acrylamide was 0.2g, the added amount of hydroxyethyl methacrylate was 0.2g, the added amount of vinylpyrrolidone was 0.2g, and the added amount of oleic acid was 0.2g.
Example 4
(1) 50g of ethyl acetate, 4g of butyl methacrylate (volume ratio 1:3) and azodiisobutyronitrile as an initiator with the weight percent of 1 percent of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen gas. The reactor was placed in a 60 ℃ water bath to control the polymerization system temperature.
(2) After 1h of reaction, 0.4g of glycidyl methacrylate, 0.1g of acrylamide, 0.2g of hydroxyethyl methacrylate, 0.1g of vinyl pyrrolidone and 0.2g of oleic acid are added, and after 8h of polymerization, the mixture is cooled and discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Example 5
(1) 100g of ethyl acetate, absolute ethyl alcohol (volume ratio 1:10) and 4g of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen gas, stirred and mixed uniformly, and then 1.5wt% of butyl methacrylate initiator azodiisobutyronitrile is added. The reactor was placed in a 55℃water bath to control the polymerization system temperature.
(2) After 1h of reaction, 0.4g of glycidyl methacrylate, 0.1g of acrylamide, 0.2g of hydroxyethyl methacrylate, 0.1g of vinyl pyrrolidone and 0.2g of oleic acid are added, and after 9h of polymerization, the mixture is cooled and discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 1
A gold tailings powder modifier was prepared as in example 1, except that: in step (1), 50g of a mixture of ethyl acetate and absolute ethanol was replaced with 50g of tetrahydrofuran.
Comparative example 2
(1) 50g of ethyl acetate and absolute ethyl alcohol (volume ratio 1:1.2), 4g of butyl methacrylate, 0.4g of glycidyl methacrylate, 0.1g of acrylamide, 0.2g of hydroxyethyl methacrylate, 0.1g of vinylpyrrolidone and 0.2g of oleic acid are added into a reactor equipped with a stirring device, a condensation return pipe and nitrogen gas inlet, stirred and mixed uniformly, and then 1wt% of butyl methacrylate initiator azodiisobutyronitrile is added. The reactor was placed in a 70 ℃ water bath to control the polymerization system temperature.
(2) And (5) after polymerization for 6 hours, cooling and discharging.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 3
(1) 50g of ethyl acetate, absolute ethyl alcohol (1:1.2) and 4g of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen gas, stirred and mixed uniformly, and then 1wt% of butyl methacrylate initiator azodiisobutyronitrile is added. The reactor was placed in a 70 ℃ water bath to control the polymerization system temperature.
(2) After 1h, 0.5g of glycidyl methacrylate, 0.3g of oleic acid and 0.2g of vinylpyrrolidone are added, and after 6h of polymerization, the mixture is discharged after cooling.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 4
(1) 50g of ethyl acetate, absolute ethyl alcohol (1:1.2) and 4g of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen gas, stirred and mixed uniformly, and then 1wt% of butyl methacrylate initiator azodiisobutyronitrile is added. The reactor was placed in a 70 ℃ water bath to control the polymerization system temperature.
(2) After 1h, 0.5g of acrylamide and 0.5g of glycidyl methacrylate are added, and after polymerization for 6h, the temperature is reduced and the material is discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 5
(1) 50g of ethyl acetate, absolute ethyl alcohol (1:1.2) and 4g of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen, stirred and mixed uniformly, then 1wt% of butyl methacrylate initiator azodiisobutyronitrile is added, and the reactor is placed in a water bath at 70 ℃ to control the temperature of a polymerization system.
(2) After 1h, 0.5g of vinylpyrrolidone and 0.5g of hydroxyethyl methacrylate are added, and after polymerization for 6h, the mixture is cooled and discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 6
(1) 50g of ethyl acetate, absolute ethyl alcohol (1:1.2) and 4g of butyl methacrylate are added into a reactor provided with a stirring device, a condensing reflux pipe and nitrogen gas, stirred and mixed uniformly, and then 1wt% of butyl methacrylate initiator azodiisobutyronitrile is added. The reactor was placed in a 70 ℃ water bath to control the polymerization system temperature.
(2) After 1h, 0.5g of vinylpyrrolidone and 0.5g of hydroxyethyl methacrylate are added, and after polymerization for 6h, the mixture is cooled and discharged.
(3) Taking out the product, precipitating with n-hexane, and drying at 65 ℃ to obtain a white amorphous product, namely the gold tailing powder modifier.
Comparative example 7
A gold tailings powder modifier was prepared as in example 1, except that: in step (1), 50g of a mixture of ethyl acetate and absolute ethanol was replaced with 50g of absolute ethanol.
Comparative example 8
A gold tailings powder modifier was prepared as in example 1, except that: in step (1), 50g of a mixture of ethyl acetate and absolute ethanol was replaced with 50g of ethyl acetate.
Experiment verification
And (3) dissolving the modifiers prepared in the examples and the comparative examples in cyclohexane to obtain a mixed solution, placing the mixed solution and gold tailing powder in a high-speed mixer, and blending for 15min at the temperature of 120 ℃ and the rotating speed of 45 r/min, wherein if the solvent cyclohexane is not volatilized completely, the time can be prolonged properly, and the modified gold tailing powder is obtained.
1g of the gold tailing powder modified by the modifier in the embodiment 1 is respectively poured into a test tube containing 10g of water, 10g of paraffin and 10g of mixed solution of water and paraffin (volume ratio is 1:1), shaken for 3min, then kept stand for 25min, and finally the suspension (or sedimentation) height of the mineral powder is recorded by a ruler. And meanwhile, unmodified gold tailing powder is used as a control. The results are shown in FIG. 1 and Table 1.
As can be seen from Table 1 and FIG. 1, the dispersibility of the gold tailing powder modified by the modifier in different solvents is greatly improved compared with that of the gold tailing powder modified by the modifier, and the modification is successful.
The modified gold tailing powder can be used as a filler of building boards, such as hard PVC boards. The filler is an important component of the hard PVC plate, the oil absorption value of the filler can influence the addition amount of various auxiliary agents in a formula system, and the larger the oil absorption value of the filler is, the more the liquid auxiliary agent is absorbed, and the addition amount of the liquid auxiliary agent is correspondingly increased, so that the raw material cost is increased intangibly. In addition, the greater the sedimentation volume of the filler, the better the dispersibility of the filler in the PVC resin. The modified gold tailings powder of each of the examples and comparative examples was tested for oil absorption and sedimentation volume according to standard GB/T19281-2014, while the unmodified gold tailings powder was used as a control, and the results are shown in Table 2 below.
As can be seen from Table 2, compared with the unmodified gold tailing powder, the modified gold tailing powder has significantly reduced oil absorption value and significantly increased sedimentation volume, wherein the modification effect of the modifier prepared in example 1 is best.
In order to further verify the modification effect of the modified gold tailing powder, the raw materials in parts by weight are accurately weighed according to the following formula: 100 parts of PVC, 50 parts of gold tailing powder after modification of comparative example or example, 3.2 parts of stabilizer, 0.6 part of paraffin, 0.5 part of stearic acid and 9 parts of CPE. Meanwhile, unmodified gold tailing powder is used as a control.
The raw materials in the formula are uniformly mixed, and then banburying is carried out in an internal mixer at the temperature of 170 ℃ and the banburying speed of 30 r/min, and the banburying result is shown in figure 2. As can be seen from fig. 2, the torque of the mixture of the modified gold tailing powder by the modifier of example 1 is smaller than that of the mixture of the unmodified gold tailing powder, which indicates that the rough surface of the modified gold tailing powder particles is coated with a layer of polymer film, so that the molecular winding force among the mineral powder particles can be reduced, the agglomeration effect among the mineral powder particles can be reduced, the dispersion effect of the mineral powder in the PVC resin can be improved, and the mineral powder and the PVC particles can be mutually and continuously embedded, thereby improving the melt flow property and reducing the torque of the PVC dry mixture. The mixture of the modified gold tailing powder by the modifier of comparative examples 2 and 3 has larger torque than the mixture of the modified gold tailing powder by the modifier of example 1, which indicates that the dispersibility of the gold tailing powder modified by the modifier is poor, and good compatibility of the gold tailing powder and PVC resin particles cannot be well realized, so that the influence of the types of raw materials and the addition sequence of the raw materials on the performance of the modifier is larger.
In combination, the gold tailing powder modified by the modifier has excellent physical and chemical properties, can be used as a material filler and raw materials of a plurality of nonmetallic materials, and can obtain an ideal building material through a certain technical treatment.
Claims (10)
1. The preparation method of the gold tailing powder modifier is characterized by comprising the following steps of:
(1) Stirring butyl methacrylate and a solvent uniformly, and then adding an initiator to react;
(2) Adding glycidyl methacrylate, acrylamide, hydroxyethyl methacrylate, vinyl pyrrolidone and oleic acid into the mixture in the step (1) to continue the reaction;
(3) Adding an organic solvent into the reacted mixture for precipitation, and drying the obtained precipitation to obtain a gold tailing powder modifier;
the mass ratio of the butyl methacrylate to the glycidyl methacrylate to the acrylamide to the hydroxyethyl methacrylate to the vinyl pyrrolidone to the oleic acid is 1:0.05-0.2:0.01-0.05:0.05-0.1:0.01-0.05:0.05-0.1;
in the step (1), the solvent is a mixture of absolute ethyl alcohol and ethyl acetate.
2. The preparation method according to claim 1, characterized in that: in the step (1), the volume ratio of the absolute ethyl alcohol to the ethyl acetate is 1.2:1, 3:1 or 10:1.
3. The preparation method according to claim 1, characterized in that: in the step (1), the initiator is dibenzoyl peroxide or azobisisobutyronitrile.
4. A method of manufacture according to claim 3, characterized in that: in the step (1), the amount of the initiator is 0.1-1.5% of the mass of the butyl methacrylate.
5. The preparation method according to claim 1, characterized in that: in the step (1), the reaction temperature is 55-75 ℃ and the reaction time is 30-60min.
6. The preparation method according to claim 1, characterized in that: in step (1), the concentration of butyl methacrylate in the solvent is 1 to 8wt%.
7. The preparation method according to claim 1, characterized in that: in the step (2), after glycidyl methacrylate, acrylamide, hydroxyethyl methacrylate, vinyl pyrrolidone and oleic acid are added, the reaction is continued for 4 to 9 hours at the temperature of 55 to 75 ℃.
8. The preparation method according to claim 1, characterized in that: in the step (3), the organic solvent is n-hexane.
9. A gold tailings powder modifier prepared in accordance with the method of any one of claims 1 to 8.
10. A modification method of gold tailing powder is characterized by comprising the following steps: uniformly mixing the gold tailing powder and the gold tailing powder modifier of claim 9, and stirring and reacting for 15-30min at 110-130 ℃ to obtain modified gold tailing powder.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1328136A (en) * | 1969-08-15 | 1973-08-30 | Commw Scient Ind Res Org | Polymeric dispersants for minerals |
| CN101321817A (en) * | 2005-09-27 | 2008-12-10 | 聚合物Crc有限公司 | Dispersing agents in composites |
| CN113493326A (en) * | 2020-03-18 | 2021-10-12 | 中国科学院过程工程研究所 | Flame-retardant foamed heat-insulation board made of gold tailings and preparation method of flame-retardant foamed heat-insulation board |
| CN114349911A (en) * | 2021-12-17 | 2022-04-15 | 武汉科技大学 | Silicon micropowder dispersing agent based on carboxylic acid monomer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7288585B2 (en) * | 2003-06-24 | 2007-10-30 | Ciba Specialty Chemicals Corp. | Acrylic dispersing agents in nanocomposites |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1328136A (en) * | 1969-08-15 | 1973-08-30 | Commw Scient Ind Res Org | Polymeric dispersants for minerals |
| CN101321817A (en) * | 2005-09-27 | 2008-12-10 | 聚合物Crc有限公司 | Dispersing agents in composites |
| CN113493326A (en) * | 2020-03-18 | 2021-10-12 | 中国科学院过程工程研究所 | Flame-retardant foamed heat-insulation board made of gold tailings and preparation method of flame-retardant foamed heat-insulation board |
| CN114349911A (en) * | 2021-12-17 | 2022-04-15 | 武汉科技大学 | Silicon micropowder dispersing agent based on carboxylic acid monomer |
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