CN111729639A - Coating circulating water treatment agent and preparation method thereof - Google Patents
Coating circulating water treatment agent and preparation method thereof Download PDFInfo
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- CN111729639A CN111729639A CN201911025434.6A CN201911025434A CN111729639A CN 111729639 A CN111729639 A CN 111729639A CN 201911025434 A CN201911025434 A CN 201911025434A CN 111729639 A CN111729639 A CN 111729639A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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Abstract
The invention relates to the technical field of water treatment, in particular to a coating circulating water treatment agent and a preparation method thereof. The preparation method of the coating circulating water treatment agent comprises the following steps: dispersing sepiolite powder in an organic solvent, adding a wetting agent to prepare slurry with the solid content of 80%, adding organic acid and methylsilicate into the slurry, heating and stirring to distill and remove volatile components, and grinding to prepare the hydrophobic modified sepiolite powder, wherein the organic solvent comprises a 95% ethanol solution; washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, and drying at 107 deg.C to obtain refined sepiolite powder. The sepiolite is fully wetted with the organic solvent under the action of the wetting agent, and the methyl silicate reacts with the organic acid to form the acid-alkali-resistant methyl silicic acid hydrophobic coating, so that the adsorption of the pore passage to water molecules can be inhibited, a large number of water molecules are prevented from occupying the adsorption pore passage after meeting water, and the adsorption capacity of the sepiolite to organic matters in coating circulating water is greatly improved.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a coating circulating water treatment agent and a preparation method thereof.
Background
Painting is an important step in modern product manufacturing processes. The quality of antirust and anticorrosive coatings is one of the important aspects of the overall quality of products. The appearance quality of the product not only reflects the protection and decoration performance of the product, but also is an important factor forming the value of the product. Along with the wide application of coating, the collection of coating paint mist is more and more emphasized, and the collection of the coating paint mist is basically collected by circulating water at present. The general coating circulating water contains a large amount of toxic and harmful substances such as paint molecules, thinner and the like, and contains a large amount of nonionic wetting dispersant, emulsifier and anionic surfactant. Generally, the coating wastewater is treated by using a sewage treatment agent such as a paint mist coagulant or a flocculating agent, and the treated wastewater can be recycled, so that the enterprise cost is reduced.
In order to purify the coating circulating water, the coating wastewater is usually adsorbed by sepiolite, and the treated circulating water is recycled, so that the enterprise cost is reduced. The particular structure of sepiolite determines its ability to have channels and holes throughout the structure and a large surface area, it has tubular through channels with a cross-sectional area of 0.36nm by 1.06nm and a theoretical surface area of up to 900 square meters per gram. Large amounts of water or polar substances, including low-polarity substances, can be adsorbed in the channels and the holes, so that the sepiolite has strong adsorption capacity. Technical background:
untreated sepiolite absorbs a lot of water when it encounters water and becomes soft and hard once it dries. Although the coating has super large specific surface area and developed adsorption pore channels, a large number of water molecules occupy the adsorption pore channels after meeting water, and the adsorption capacity of the coating on organic matters in coating circulating water is greatly reduced. Therefore, the application of the paint in the field of coating circulating water treatment is restricted.
Disclosure of Invention
In order to solve the above technical problem, the present application provides the following technical solutions.
In a first aspect, the technical scheme of the invention provides a preparation method of a coating circulating water treatment agent, which comprises the following steps:
dispersing sepiolite powder in an organic solvent, adding a wetting agent to prepare slurry with the solid content of 80%, adding organic acid and methylsilicate into the slurry, heating and stirring, raising the temperature to distill and remove volatile components, and grinding to prepare hydrophobic modified sepiolite powder, wherein the organic solvent comprises a 95% ethanol solution;
washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, and drying at 107 deg.C to obtain refined sepiolite powder.
Further, the preparation method of the coating circulating water treatment agent further comprises the following steps: mixing the refined sepiolite powder with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the reacted refined sepiolite powder with deionized water for 3 times, and drying and grinding to obtain the coating circulating water treatment agent.
Further, before dispersing the sepiolite powder in the organic solvent, the method further comprises the following steps: adding organic acid or inorganic acid into sepiolite raw ore powder, stirring, standing, filtering, drying filter cake, grinding into powder, and controlling water content to be 0.1% -4% to obtain sepiolite powder.
Further, the inorganic acid added into the sepiolite raw ore powder is 4-6% of dilute hydrochloric acid, and the solid-liquid ratio of the inorganic acid to the sepiolite raw ore powder is 1: 10.
Further, the organic solvent also comprises 200# solvent oil.
Further, the organic acid added to the slurry includes at least one of oxalic acid, acetic acid, citric acid and tartaric acid.
Further, the methyl silicate is at least one of sodium methyl silicate and potassium methyl silicate.
In a first aspect, the invention provides a coating circulating water treatment agent, which is prepared by the preparation method provided by the application.
Compared with the prior art, the technical scheme adopted by the invention has the following beneficial effects:
the sepiolite is fully wetted with the organic solvent under the action of the wetting agent, the micromolecule methyl silicate can fully enter the sepiolite pore channels along with the solvent, and the methyl silicate reacts with the organic acid to form the acid-base-resistant methyl silicic acid hydrophobic coating, so that the adsorption of the pore channels to water molecules can be inhibited, a large number of water molecules are prevented from occupying the adsorption pore channels after meeting water, and the adsorption capacity of the sepiolite to organic matters in coating circulating water is greatly improved.
Detailed Description
The technical solution of the present invention is described in detail below with reference to examples.
The embodiment of the invention provides a preparation method of a coating circulating water treatment agent, which comprises the following steps:
dispersing sepiolite powder in an organic solvent, adding a wetting agent to prepare slurry with the solid content of 80%, adding organic acid and methylsilicate into the slurry, heating and stirring to distill and remove volatile components, and grinding to prepare the hydrophobic modified sepiolite powder, wherein the organic solvent comprises a 95% ethanol solution; washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, and drying at 107 deg.C to obtain refined sepiolite powder.
The steps finish the hydrophobic modification of the sepiolite pore channels (inhibiting the adsorption of the pore channels to water molecules), wherein 95 percent of ethanol solution contains water, and organic acid can ionize H after meeting water+The methyl silicate is usually selected to be sodium methyl silicate or potassium methyl silicate, and the following chemical reactions can exist in the system:
CH3-SiOOK+H+→CH3-SiOOH+K+or
CH3-SiOONa+H+→CH3-SiOOH+Na+,
The reaction product methylsilicic acid is a hydrophobic substance. The sepiolite powder is fully wetted with the organic solvent under the action of the wetting agent, the micromolecule methyl silicate can fully enter the sepiolite pore passage along with the organic solvent, and after the organic acid is added, the methyl silicate and the H are mixed+Reacting to form an acid-alkali-resistant methyl silicic acid hydrophobic coating which can inhibit the adsorption of the pore channels to water molecules; the alcoholic solution can provide water required by organic acid ionization, and the water required by the reaction is controlled by controlling the addition of the alcoholic solution, so that the modification of the hydrophobicity of the channel is not facilitated by too much water, and the water content is too low to enable the organic acid to be sufficiently ionized to obtain H required by the reaction+In the above process, the reaction can be accelerated by heating and stirring, and in order to further improve the dispersing ability, the reaction can be accelerated by stirringWith 95% ethanol as solvent, other organic solvents, e.g. 200#Solvent oil. The sepiolite powder prepared by the scheme can inhibit the pore channels of the sepiolite powder from adsorbing water molecules, so that a large number of water molecules are prevented from occupying the adsorption pore channels after meeting water, the adsorption capacity of the sepiolite powder on organic matters in coating circulating water is greatly improved, and selective adsorption is realized.
In some examples, the coating cycle water treatment agent is prepared by mixing the refined sepiolite powder prepared in the above examples with an organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the reacted refined sepiolite powder with deionized water for 3 times, and drying and grinding the washed sepiolite powder. After the pore channels of the sepiolite powder are subjected to hydrophobicity modification, in the process of quaternization, the hydrophobic end of the quaternary ammonium salt preferentially enters the pore channels, and a large number of cationic ends are exposed at the port of the pore channels, so that on one hand, a large number of anionic active ingredients can be captured, on the other hand, the pore channels are subjected to hydrophobicity modification, but the sepiolite unit cells still have the function of dispersing in water.
Through the steps, on one hand, a pore channel of the sepiolite powder can adsorb a specific amount of cationic organic matters, so that the channel with a large specific surface area can carry a certain cationic charge, and the high-density cationic charge carried by the channel can adsorb and separate the organic matters with anionic charges in the coating circulating water through electrostatic adsorption, so that the organic matters are inactivated; on the other hand, the pore channels can adsorb a large amount of active ingredients such as nonionic wetting dispersants and emulsifiers in the coating circulating water, so that the coating circulating water resin, the pigment and the filler are separated, and after the active ingredients such as the nonionic wetting dispersants and the emulsifiers are stripped from the surfaces of the resin, the filler and the pigment through the adsorbing materials, the components of the paint are destabilized to form flocculent (emulsion breaking). Finally, paint water separation in the coating circulating water can be thoroughly realized.
In some embodiments, dispersing the sepiolite powder in the organic solvent further comprises: adding organic or inorganic acid into sepiolite raw ore powder, stirring, standing, filtering, drying and grinding a filter cake, and controlling the water content of the filter cake to be 0.1-4% to obtain sepiolite powder. The step can dredge the pore channel of the sepiolite through acidification, and dissolve out acid-soluble ions or organic matters from the pore channel.
Example 1
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: dispersing sepiolite powder in 95% ethanol water solution, adding wetting agent to prepare slurry with solid content of 80%, adding oxalic acid and sodium methylsilicate into the slurry, heating and stirring at 80 ℃ for 4h, then raising the heating temperature to distill and remove volatile oxalic acid, ethanol and the like, and grinding to obtain the hydrophobic modified sepiolite powder with particle size of less than 1250 meshes.
Step 2: and (2) washing the hydrophobic modified sepiolite powder prepared in the step (1) with deionized water for 2-3 times, removing residual organic acid, and drying at the constant temperature of 107 ℃ for 4 hours to obtain the refined sepiolite powder which can be used as a treating agent for purifying coating circulating water.
Example 2
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: dispersing sepiolite powder in 95% ethanol solution, adding wetting agent to prepare slurry with solid content of 80%, adding acetic acid and sodium methylsilicate into the slurry, heating and stirring at 120 ℃ for 2h, then raising the heating temperature to distill and remove volatile acetic acid and ethanol, and grinding to obtain hydrophobic modified sepiolite powder below 1250 meshes;
step 2: washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, removing residual organic acid, and drying at 107 deg.C for 4 hr to obtain refined sepiolite powder.
And step 3: and (3) mixing the refined sepiolite powder prepared in the step (2) with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the refined sepiolite powder after reaction with deionized water for 3 times, washing and removing the redundant organic quaternary ammonium salt, and drying and grinding to obtain the coating circulating water treatment agent.
Example 3
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: adding 4% of dilute hydrochloric acid into raw sepiolite ore powder, wherein the solid-to-liquid ratio of the dilute hydrochloric acid to the raw sepiolite ore powder is 1:10, stirring, standing, performing suction filtration, drying and grinding a filter cake to control the water content of the filter cake to be 0.1% -4%, and thus obtaining the sepiolite powder.
Step 2: dispersing the sepiolite powder prepared in the step 1 in 95% ethanol water, adding a wetting agent to prepare slurry with the solid content of 80%, adding citric acid and sodium methylsilicate into the slurry, heating and stirring at 100 ℃ for 3 hours, then increasing the heating temperature to distill and remove volatile citric acid and ethanol, and grinding to prepare hydrophobic modified sepiolite powder with the particle size of less than 1250 meshes;
and step 3: and (3) washing the hydrophobic modified sepiolite powder prepared in the step (2) with deionized water for 2-3 times, removing residual organic acid, and drying at the constant temperature of 107 ℃ for 4 hours to obtain the refined sepiolite powder.
Example 4
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: adding 6% of dilute hydrochloric acid into raw sepiolite ore powder, wherein the solid-to-liquid ratio of the dilute hydrochloric acid to the raw sepiolite ore powder is 1:10, stirring, standing, performing suction filtration, drying and grinding filter cakes to control the water content of the filter cakes to be 0.1% -4%, and thus obtaining the sepiolite powder.
Step 2: dispersing sepiolite powder in 200#Adding wetting agent into solvent oil and 95% ethanol to prepare slurry with solid content of 80%, adding tartaric acid and methyl potassium silicate into the slurry, heating and stirring at 110 ℃ for 2.5h, raising the heating temperature to distill and remove volatile tartaric acid and ethanol, and grinding to obtain hydrophobic modified sepiolite powder below 1250 meshes;
and step 3: and (3) washing the hydrophobic modified sepiolite powder prepared in the step (2) with deionized water for 2-3 times, removing residual organic acid, and drying at the constant temperature of 107 ℃ for 4 hours to obtain the refined sepiolite powder.
And 4, step 4: mixing the refined sepiolite powder with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the reacted refined sepiolite powder with deionized water for 3 times, and drying and grinding to obtain the coating circulating water treatment agent.
Example 5
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: adding acetic acid and oxalic acid into raw sepiolite ore powder, wherein the solid-to-liquid ratio of the acid to the raw sepiolite ore powder is 1:10, stirring, standing, performing suction filtration, drying and grinding filter cakes to control the water content of the filter cakes to be 0.1-4%, and thus obtaining the sepiolite powder.
Step 2: dispersing sepiolite powder in 200#Adding wetting agent into solvent oil and 95% ethanol water solution to obtain slurry with solid content of 80%, adding oxalic acid and sodium methylsilicate into the slurry, heating and stirring at 120 deg.C for 2 hr, and increasing heating temperature to make the volatile content 200#Distilling to remove solvent oil, ethanol and oxalic acid, and grinding to obtain hydrophobic modified sepiolite powder of 1250 meshes or below;
and step 3: washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, removing residual organic acid, and drying at 107 deg.C for 4 hr to obtain refined sepiolite powder.
And 4, step 4: and (3) mixing the refined sepiolite powder prepared in the step (3) with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the refined sepiolite powder after reaction with deionized water for 3 times, removing the redundant organic quaternary ammonium salt, and drying and grinding to obtain the coating circulation water treatment agent.
Example 6
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: adding citric acid and acetic acid into raw sepiolite ore powder, wherein the solid-to-liquid ratio of the acid to the raw sepiolite ore powder is 1:10, stirring, standing, performing suction filtration, drying and grinding filter cakes to control the water content of the filter cakes to be 0.1-2%, and thus obtaining the sepiolite powder.
Step 2: dispersing sepiolite powder in 95% ethanol water solution, adding wetting agent to prepare slurry with solid content of 80%, adding acetic acid, citric acid and potassium methyl silicate into the slurry, heating and stirring at 100 deg.C for 3 hr, raising heating temperature to distill off volatile acetic acid, ethanol and citric acid, and grinding to obtain hydrophobic modified sepiolite powder of 1250 mesh or less;
and step 3: washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, removing residual organic acid, and drying at 107 deg.C for 4 hr to obtain refined sepiolite powder.
And 4, step 4: and (3) mixing the refined sepiolite powder prepared in the step (3) with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the refined sepiolite powder after reaction with deionized water for 3 times, removing the redundant organic quaternary ammonium salt, and drying and grinding to obtain the coating circulation water treatment agent.
Example 7
A preparation method of a coating circulating water treatment agent comprises the following steps:
step 1: adding acetic acid and 5% diluted hydrochloric acid into raw sepiolite powder with a solid-to-liquid ratio of 1:10, stirring, standing, filtering, drying and grinding filter cake to control water content between 2% -4% to obtain sepiolite powder.
Step 2: dispersing sepiolite powder in 200#Adding wetting agent into solvent oil and 95% ethanol water solution to obtain slurry with solid content of 80%, adding acetic acid and sodium methylsilicate into the slurry, heating and stirring at 110 deg.C for 2 hr, and increasing heating temperature to make the volatile content of 200%#Distilling to remove solvent oil, ethanol and acetic acid, and grinding to obtain hydrophobic modified sepiolite powder of 1250 meshes or below;
and step 3: washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, removing residual organic acid, and drying at 107 deg.C for 4 hr to obtain refined sepiolite powder.
And 4, step 4: and (3) mixing the refined sepiolite powder prepared in the step (3) with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the refined sepiolite powder after reaction with deionized water for 3 times, and drying and grinding to obtain the coating circulating water treatment agent.
Comparative example 1
Raw mineral powder of untreated sepiolite.
Comparative example 2
Example 2 the 95% ethanol solution in step 1 was replaced with pure ethanol and the remaining steps were unchanged.
The coating circulation water treatment agents obtained in examples 1 to 7 and comparative examples 1 to 2 were tested. Adjusting the pH value of paint-containing coating circulating water to 8, adding the coating circulating water treatment agent prepared in the embodiment and the proportion into the coating circulating water treatment agent, wherein the adding amount is 2.5g/1kg of coating circulating water, stirring for 2min after adding, standing, observing the coagulation and floating of paint mist, and fishing paint slag, wherein the percentage content of the paint mist in the adopted coating circulating water is 9.5%. The test indices are listed in table 1. In addition, the water absorption and contact angle of the paint circulation water treatment agent prepared by each group were measured, and the experimental results are shown in table 1.
TABLE 1 results of the experiment
Some embodiments in this specification are described in a parallel or progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A preparation method of a coating circulating water treatment agent is characterized by comprising the following steps:
dispersing sepiolite powder in an organic solvent, adding a wetting agent to prepare slurry with the solid content of 80%, adding organic acid and methylsilicate into the slurry, heating and stirring at the temperature of 80-120 ℃ for 2-4 hours, raising the temperature to distill and remove volatile components, and grinding to prepare hydrophobic modified sepiolite powder, wherein the organic solvent comprises a 95% ethanol solution;
washing hydrophobic modified sepiolite powder with deionized water for 2-3 times, and drying at 107 deg.C to obtain refined sepiolite powder.
2. The method for producing a coating circulation water treatment agent according to claim 1, further comprising: mixing the refined sepiolite powder with organic quaternary ammonium salt, adding a wetting agent, heating and stirring for 2 hours, washing the reacted refined sepiolite powder with deionized water for 3 times, and drying and grinding to obtain the coating circulating water treatment agent.
3. The method for producing a coating circulation water treatment agent according to claim 1, wherein the step of dispersing the sepiolite powder in the organic solvent further comprises: adding organic acid or inorganic acid into sepiolite raw ore powder, stirring, standing, filtering, drying filter cake, grinding into powder, and controlling water content to be 0.1% -4% to obtain sepiolite powder.
4. The preparation method of the coating circulating water treatment agent according to claim 3, wherein the inorganic acid added to the raw sepiolite ore powder is 4% to 6% of dilute hydrochloric acid, and the solid-to-liquid ratio of the inorganic acid to the raw sepiolite ore powder is 1: 10.
5. The method for producing a coating circulation water treatment agent according to claim 1, wherein the organic solvent further comprises 200 parts by weight#Solvent oil.
6. The method for producing a coating circulation water treatment agent according to claim 1, wherein the organic acid added to the slurry includes at least one of oxalic acid, acetic acid, citric acid, and tartaric acid.
7. The method for producing a coating circulating water treatment agent according to claim 1, wherein the methyl silicate is at least one of sodium methyl silicate and potassium methyl silicate.
8. A coating circulation water treatment agent, characterized in that it is produced by the production method according to any one of claims 1 to 7.
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