CN114177565A - Wet oxidation treatment method for low-content organic waste salt - Google Patents
Wet oxidation treatment method for low-content organic waste salt Download PDFInfo
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Abstract
The invention relates to the field of waste treatment, and discloses a wet oxidation treatment method for low-content organic waste salt. The removal rate of organic matters in the low-content organic waste salt is high; the catalyst has the advantages of good stability, long service life, simple preparation process, low cost, easy large-scale industrial production and capability of efficiently catalyzing and degrading organic matters, and batch treatment can be recycled after the ultraviolet fixed bed oxidizer is simply washed. The invention also has the advantages that the reaction catalysis reaction is easy to realize; simple process, reliable technology, no increase of three-waste discharge and high economic benefit.
Description
Technical Field
The invention relates to the field of waste treatment, in particular to a wet oxidation treatment method for low-content organic waste salt.
Background
Among solid wastes generated from industrial activities, wastes having one or more hazardous characteristics such as corrosiveness, toxicity, flammability, reactivity, and infectivity or having a possibility of having a harmful effect on the environment and human health are called hazardous wastes. According to the types of raw materials and the use characteristics of additives in the production process of industrial (especially organic chemical industry) products, the saline solid waste can be generally classified as dangerous waste, and if the saline solid waste is not properly disposed, the saline solid waste can cause harm to the surrounding environment and personnel. The salt-containing solid waste not only contains alkali metal salt, but also remains part of toxic and harmful organic compounds, and the complex components increase the difficulty of disposing the salt-containing solid waste.
CN112978766A relates to an industrial waste salt advanced treatment method, which comprises the following steps: step one, pyrolysis impurity removal: the TOC content and TN content in the treated waste salt are 100-300 mg/kg and 30-75 mg/kg respectively; step two, physicochemical impurity removal: firstly, carrying out liquid phase dissolution on the waste salt subjected to pyrolysis impurity removal to obtain brine, wherein the concentration of the brine is 300-310 g/L, the temperature of the brine is 40-60 ℃, then carrying out chemical agent impurity removal on the brine, and then carrying out solid-liquid separation on the brine and removing most insoluble substances; step three, deep oxidation: firstly, sequentially carrying out electrochemical oxidation, air stripping and ultrasonic oxidation on the brine after physicochemical impurity removal, and then removing residual medicament from the brine, wherein the TOC concentration of the treated brine is less than 10ppm, and the TN concentration is less than 3 ppm; step four, adsorption and nanofiltration: firstly, carrying out activated carbon adsorption on the deeply oxidized brine, diluting the adsorbed brine to 100-200 g/L, and then carrying out nanofiltration on the diluted brine to remove impurities; step five, evaporating to prepare salt: and evaporating and crystallizing the salt water subjected to adsorption and nanofiltration to obtain a salt product.
CN112645462A discloses an industrial wastewater desalination system, which comprises a salt-containing detection instrument, a valve control unit, a desalination pool, a biological membrane salt filtering system and an intelligent control system; the salt-containing detection instrument is used for detecting the salt-containing concentration in the sewage, and the valve control unit is used for controlling a water inlet valve arranged at a water inlet of the desalting tank; the biological membrane salt filtering system is arranged along the direction vertical to the water flow in the desalting tank and is used for removing salt substances in sewage; the industrial wastewater desalting system provided by the invention adopts a biomembrane salt filtering system to remove salt substances in sewage, the biomembrane salt filtering system is arranged along the direction vertical to the water flow in the desalting tank, the desalting tank is divided into a plurality of sewage channels along the sewage flow direction, and each sewage channel is provided with a reverse osmosis membrane filter plate; the grid bars that the interval set up in the middle part of the reverse osmosis membrane filter, set up reverse osmosis membrane on the blank between the grid bars, utilize reverse osmosis membrane's characteristic to detach the aquatic through the unnecessary salt class material that neutralization reaction and biochemical reaction produced.
CN110216125B discloses a method for treating industrial waste salt, which comprises the following steps: crushing and homogenizing waste salt, and then sending the waste salt into a dryer; introducing air into a heat exchanger by using a fan for heating, filtering the heated air, and then feeding the filtered air into the dryer from the bottom of the dryer so as to float waste salt at the bottom of the dryer, wherein the air forms an air-lift circulating flow in the dryer; spraying a vaporous wall material into the dryer to coat the waste salt to form microcapsule particles; collecting the microcapsule particles. The invention realizes the non-selective harmless treatment of the industrial waste salt by adopting a mode that the wall material wraps the industrial waste salt to form the microcapsule.
At present, the industrial waste salt is mainly treated by a high-temperature incineration mode, but the waste salt with low content of organic matters has low heat value, is easy to form molten salt under the high-temperature condition, and is very easy to cause equipment corrosion and bed material slagging to stop the furnace.
Disclosure of Invention
In order to solve the problems, the invention provides a wet oxidation treatment method of low-content organic waste salt.
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
according to the mass parts, 100-180 parts of low-content organic waste salt is put into a grinder to be ground into 20-80 meshes of powder, then the powder is added into 140-200 parts of water to be uniformly stirred and mixed to prepare slurry, and then the pH value of the slurry is adjusted to 3-5 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30-60 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 40-60 ℃, the slurry is continuously reacted for 20-30min after being added, the reaction is completed, the discharging is completed, the temperature is reduced to 20-30 ℃, insoluble salt is filtered out, the filtrate is evaporated and crystallized to obtain recycled salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 10-15 parts by mass of glass fiber into short fiber with the length of 3-6cm, soaking the short glass fiber into 100-130 parts by mass of nitric acid with the mass percentage concentration of 5-15%, heating to 60-80 ℃, treating for 30-60min, washing and drying for later use;
b) adding 1.2-1.8 parts by mass of zirconium isooctanoate, 0.2-0.8 part by mass of sodium vanadate, 1.6-2.4 parts by mass of glacial acetic acid, 20-35 parts by mass of ethanol and 8-14 parts by mass of pure water into a reaction kettle, uniformly stirring and mixing, and adding 24-40 parts by mass of an ethanol solution of tetrabutyl titanate with the mass percentage concentration of 2.5% -5.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 30-120min, drying at 40-60 ℃, calcining at 400-480 ℃, and cooling to room temperature;
d) and soaking 20-40 parts of calcined glass fiber in 100-200 parts of soaking solution, stirring at 60-75 ℃ for 2-4 hours, filtering, and drying to obtain the glass fiber loaded ultraviolet catalyst, wherein the filtrate is recycled.
The composition of the steeping liquor in the step d is as follows;
parts by weight (based on solids)
Mercaptosiloxanes 10-18
Vinylpyridine 4-12
Methacrylic acid cerium 1-5
Microcrystalline paraffin 0.06-0.2
Triethylamine 2-5
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 20 to 30 wt.% solids.
Further, the oxidant is ozone or hydrogen peroxide gas or oxygen.
Furthermore, the aeration rate of the oxidant is 10-18 g/h.L.
Further, the wavelength of the ultraviolet light is 200-300 nm.
Further, the pH value regulator is sodium hydroxide or sulfuric acid solution with the mass percentage concentration of 10% -20%.
Further, the mercaptosiloxane is selected from 2-mercapto-1-ethyltriethoxysilane, 1-mercapto-1-ethyltriethoxysilane, 3-mercapto-1-propylmethyldiethoxysilane, 3-mercapto-1-propyltrimethoxysilane, 2-mercapto-1-ethyltrimethoxysilane and mercaptomethyltrimethoxysilane;
the reaction mechanism is as follows:
the invention makes the low-content organic waste salt into slurry in a fluid state, and finishes the oxidation reaction of the organic matters in the oxidation reactor. The oxidation reactor is provided with an ultraviolet fixed bed oxidizer, and materials are catalytically oxidized in a fluid state in the reactor to achieve the purpose of degrading organic matters; the glass fiber loaded ultraviolet catalyst prepared by the invention adopts a gel sol process, titanium oxide, zirconium oxide and vanadium oxide are loaded on the surface of glass fiber through the gel process to form a nano-scale catalytic active layer, and then a small amount of cerium is loaded on the surface of the catalytic active layer through a dipping method and a sulfydryl-alkene addition reaction to form a high-activity catalyst layer; the catalyst has good stability and long service life, and the catalytic performance is still unchanged after the catalyst is circulated for many times.
The technical effects are as follows:
the wet oxidation treatment method of the low-content organic waste salt, disclosed by the invention, uses ozone or oxygen and hydrogen peroxide as oxidants, and has the advantages of small environmental pollution and simple process. The removal rate of organic matters in the low-content organic waste salt is high; the catalyst has the advantages of good stability, long service life, simple preparation process, low cost, easy large-scale industrial production and capability of efficiently catalyzing and degrading organic matters, and batch treatment can be recycled after the ultraviolet fixed bed oxidizer is simply washed. The invention also has the advantages that the reaction catalysis reaction is easy to realize; simple process, reliable technology, no increase of three-waste discharge and high economic benefit.
Drawings
FIG. 1 is a scanning electron microscope image of SU8010 cold field emission with low content of organic waste salts used in example 1.
FIG. 2 is a scanning electron microscope image of SU8010 cold field emission with low content of organic waste salts used in example 2.
Detailed Description
The method for detecting the organic matter residue in the recovered salt, which is finally prepared, comprises the following steps: the recovered salt which is dried and homogenized by taking l0g is leached for 1 hour at a liquid-solid ratio of 10:1, and then the COD value is determined. The organic residue in the slurry after oxidation treatment and the recovered salt was measured according to the method for measuring chemical oxygen demand of national standard GB 11914-89.
The invention is further illustrated by the following specific examples:
the cerium methacrylate is prepared by self-made method according to the research on the performance of the cerium methacrylate and the reinforced natural rubber thereof.
Example 1
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 100kg of low-content organic waste salt into a grinder, grinding into powder of 20 meshes, adding into 140kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 3 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 40 ℃, the slurry is continuously reacted for 20min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 20 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 10kg of glass fiber into short fibers with the length of 3cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 5%, heating to 60 ℃, treating for 30min, washing and drying for later use;
b) adding 1.2kg of zirconium isooctanoate, 0.2kg of sodium vanadate, 1.6kg of glacial acetic acid, 20kg of ethanol and 8kg of pure water into a reaction kettle, stirring and mixing uniformly, and then adding 24kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 2.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 30min, drying at 40 ℃, calcining at 400 ℃, and cooling to room temperature;
d) and soaking 20 parts of calcined glass fiber in 100 parts of soaking solution, stirring for 2 hours at 60 ℃, filtering and drying to obtain the glass fiber loaded ultraviolet catalyst, wherein the filtrate is recycled.
The composition of the steeping liquor in the step d is as follows;
kg
mercaptosiloxane 10
Vinylpyridine 4
Methacrylic acid cerium 1
Microcrystalline paraffin 0.06
Triethylamine 2
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 20 wt.% solids.
The oxidant is ozone.
The aeration rate of the oxidant is 10 g/h.L.
The wavelength of the ultraviolet light is 200 nm.
The pH value regulator is a sodium hydroxide solution with the mass percentage concentration of 10%.
The mercaptosiloxane is selected from 2-mercapto-1-ethyltriethoxysilane.
Example 2
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 140kg of low-content organic waste salt into a grinder, grinding into powder of 50 meshes, adding into 160kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 4 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 40 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 50 ℃, the slurry is continuously reacted for 25min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 25 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 13kg of glass fiber into short fibers with the length of 5cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 10%, heating to 70 ℃, treating for 40min, washing and drying for later use;
b) adding 1.5kg of zirconium isooctanoate, 0.5kg of sodium vanadate, 1.8kg of glacial acetic acid, 28kg of ethanol and 12kg of pure water into a reaction kettle, stirring and mixing uniformly, and then adding 32kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 3.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 60min, drying at 50 ℃, calcining at 450 ℃, and cooling to room temperature;
d) and soaking 25 parts of calcined glass fiber in 150 parts of soaking solution, stirring for 2.5 hours at 65 ℃, filtering and drying to obtain the glass fiber supported ultraviolet catalyst, and recycling the filtrate.
The composition of the steeping liquor in the step d is as follows;
kg
mercaptosiloxane 15
Vinylpyridine 6
Methacrylic acid cerium 2
Microcrystalline paraffin 0.1
Triethylamine 3
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 23 wt.% solids.
The oxidant is hydrogen peroxide gas.
The aeration rate of the oxidant is 15 g/h.L.
The wavelength of the ultraviolet light is 256 nm.
The pH value regulator is sodium hydroxide solution with the mass percentage concentration of 15%.
The mercaptosiloxane is selected from 1-mercapto-1-ethyltriethoxysilane.
Example 3
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 180kg of low-content organic waste salt into a grinder, grinding into powder of 80 meshes, adding into 200kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 5 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 60 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 60 ℃, the slurry is continuously reacted for 30min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 30 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 15kg of glass fiber into short fibers with the length of 6cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 15%, heating to 80 ℃, treating for 60min, washing and drying for later use;
b) adding 1.8kg of zirconium isooctanoate, 0.8kg of sodium vanadate, 2.4kg of glacial acetic acid, 35kg of ethanol and 14kg of pure water into a reaction kettle, stirring and mixing uniformly, and adding 40kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 5.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 120min, drying at 60 ℃, calcining at 480 ℃, and cooling to room temperature;
d) and soaking 20-40 parts of calcined glass fiber in 100-200 parts of soaking solution, stirring at 60-75 ℃ for 2-4 hours, filtering, and drying to obtain the glass fiber loaded ultraviolet catalyst, wherein the filtrate is recycled.
The composition of the steeping liquor in the step d is as follows;
kg
mercaptosiloxanes 18
Vinylpyridine 12
Methacrylic acid cerium 5
Microcrystalline paraffin 0.2
Triethylamine 5
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 30% by weight solids.
Further, the oxidant is oxygen.
Further, the aeration rate of the oxidizing agent is 18 g/h.L.
Further, the wavelength of the ultraviolet light is 300 nm.
Further, the pH value regulator is sodium hydroxide with the mass percentage concentration of 20%.
Further, the mercaptosiloxane is selected from mercaptomethyltrimethoxysilane.
Comparative example 1
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 100kg of low-content organic waste salt into a grinder, grinding into powder of 20 meshes, adding into 140kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 3 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 40 ℃, the slurry is continuously reacted for 20min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 20 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 10kg of glass fiber into short fibers with the length of 3cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 5%, heating to 60 ℃, treating for 30min, washing and drying for later use;
b) adding 1.2kg of zirconium isooctanoate, 1.6kg of glacial acetic acid, 20kg of ethanol and 8kg of pure water into a reaction kettle, stirring and mixing uniformly, and then adding 24kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 2.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 30min, drying at 40 ℃, calcining at 400 ℃, and cooling to room temperature;
d) and soaking the calcined glass fiber in 0.1 mass percent mercaptosiloxane solution, drying at 40 ℃, calcining at 430 ℃, and cooling to room temperature to obtain the glass fiber loaded ultraviolet catalyst.
Further, the oxidant is ozone.
Further, the aeration amount of the oxidizing agent is 10 g/h.L.
Further, the wavelength of the ultraviolet light is 200 nm.
Further, the pH value regulator is a sodium hydroxide solution with the mass percentage concentration of 10%.
Comparative example 2
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 100kg of low-content organic waste salt into a grinder, grinding into powder of 20 meshes, adding into 140kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 3 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 40 ℃, the slurry is continuously reacted for 20min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 20 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 10kg of glass fiber into short fibers with the length of 3cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 5%, heating to 60 ℃, treating for 30min, washing and drying for later use;
b) adding 1.2kg of zirconium isooctanoate, 0.2kg of sodium vanadate, 1.6kg of glacial acetic acid, 20kg of ethanol and 8kg of pure water into a reaction kettle, stirring and mixing uniformly, and then adding 24kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 2.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 30min, drying at 40 ℃, calcining at 400 ℃, and cooling to room temperature to obtain the glass fiber loaded ultraviolet catalyst.
Further, the oxidant is ozone.
Further, the aeration amount of the oxidizing agent is 10 g/h.L.
Further, the wavelength of the ultraviolet light is 200 nm.
Further, the pH value regulator is a sodium hydroxide solution with the mass percentage concentration of 10%.
Comparative example 3
A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
putting 100kg of low-content organic waste salt into a grinder, grinding into powder of 20 meshes, adding into 140kg of water, stirring and mixing uniformly to prepare slurry, and then adjusting the pH value of the slurry to 3 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30 min; an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; the temperature in the oxidation reactor is 40 ℃, the slurry is continuously reacted for 20min after being added, the reaction is completed, the discharging is completed, the insoluble salt is filtered after the temperature is reduced to 20 ℃, the filtrate is evaporated and crystallized to obtain the recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed; the method is characterized in that the ultraviolet light oxidation catalyst is a glass fiber loaded ultraviolet light catalyst and is prepared according to the following method:
a) cutting 10kg of glass fiber into short fibers with the length of 3cm, soaking the short glass fibers into nitric acid with the mass percentage concentration of 5%, heating to 60 ℃, treating for 30min, washing and drying for later use;
b) adding 0.2kg of sodium vanadate, 1.6kg of glacial acetic acid, 20kg of ethanol and 8kg of pure water into a reaction kettle, stirring and mixing uniformly, and then adding 24kg of ethanol solution of tetrabutyl titanate with the mass percentage concentration of 2.5% into the reaction kettle to obtain a catalyst precursor;
c) adding the treated glass fiber into a catalyst precursor, soaking for 30min, drying at 40 ℃, calcining at 400 ℃, and cooling to room temperature;
d) and soaking 20 parts of calcined glass fiber in 100 parts of soaking solution, stirring for 2 hours at 60 ℃, filtering and drying to obtain the glass fiber loaded ultraviolet catalyst, wherein the filtrate is recycled.
The composition of the steeping liquor in the step d is as follows;
kg
mercaptosiloxane 15
Vinylpyridine 6
Microcrystalline paraffin 0.1
Triethylamine 3
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 23 wt.% solids.
Further, the oxidant is ozone.
Further, the aeration amount of the oxidizing agent is 10 g/h.L.
Further, the wavelength of the ultraviolet light is 200 nm.
Further, the pH value regulator is a sodium hydroxide solution with the mass percentage concentration of 10%.
The mercaptosiloxane is selected from 2-mercapto-1-ethyltriethoxysilane.
The results of the tests of examples 1 to 3 and comparative examples 1 to 3 are shown in tables 1 and 2.
Table 1:
table 2:
| COD value (mg/L) of oxidized slurry | COD value of recovered salt (mg/kg) | |
| Example 1 | 12.3 | 5.8 |
| Example 2 | 8.6 | 4.3 |
| Example 3 | 6.8 | 3.8 |
| Comparative example 1 | 26.1 | 18.9 |
| Comparative example 2 | 36.8 | 32.7 |
| Comparative example 3 | 16.1 | 8.6 |
The inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained desirable results.
Claims (7)
1. A wet oxidation treatment method of low-content organic waste salt comprises the following steps:
according to the mass parts, 100-180 parts of low-content organic waste salt is put into a grinder to be ground into 20-80 meshes of powder, then the powder is added into 140-200 parts of water to be uniformly stirred and mixed to prepare slurry, and then the pH value of the slurry is adjusted to 3-5 by using a pH value regulator; slowly adding the prepared slurry into an oxidation reactor, and introducing an oxidant, wherein the slurry adding time is 30-60 min; the method is characterized in that an ultraviolet light oxidation catalyst is added into the oxidation reactor in advance, and the ultraviolet light oxidation catalyst is fixed on an ultraviolet light fixed bed oxidizer; and the temperature in the oxidation reactor is 40-60 ℃, the slurry is continuously reacted for 20-30min after being added, the reaction is completed, the discharging is completed, the temperature is reduced to 20-30 ℃, insoluble salt is filtered out, the filtrate is evaporated and crystallized to obtain recovered salt, and the wet oxidation treatment of the low-content organic waste salt can be completed.
2. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that: the ultraviolet oxidation catalyst is a glass fiber loaded ultraviolet catalyst and is prepared by the following method:
a. cutting 10-15 parts of glass fiber into short fibers with the length of 3-6cm according to the parts by mass, soaking the short fibers in nitric acid with the mass percentage concentration of 5% -15%, heating to 60-80 ℃, treating for 30-60min, washing and drying for later use;
b. adding 1.2-1.8 parts by mass of zirconium iso-octoate, 0.2-0.8 part by mass of sodium vanadate, 1.6-2.4 parts by mass of glacial acetic acid, 20-35 parts by mass of ethanol and 8-14 parts by mass of pure water into a reaction kettle, stirring and mixing uniformly, and adding 24-40 parts by mass of tetrabutyl titanate ethanol solution with the mass percentage concentration of 2.5% -5.5% into the reaction kettle to obtain a catalyst precursor;
c. adding the treated glass fiber into a catalyst precursor, soaking for 30-120min, drying at 40-60 ℃, calcining at 400-480 ℃, and cooling to room temperature;
d. and (2) soaking 20-40 parts of calcined glass fiber in 100-200 parts of soaking solution, stirring for 2-4 hours at 60-75 ℃, filtering, and drying to obtain the glass fiber loaded ultraviolet catalyst.
3. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that:
the composition of the steeping liquor in the step d is as follows;
parts by weight (based on solids)
Mercaptosiloxanes 10-18
Vinylpyridine 4-12
Methacrylic acid cerium 1-5
Microcrystalline paraffin 0.06-0.2
Triethylamine 2-5
Ethanol comprises the balance of the composition and is present in an amount sufficient to adjust the solids content of the composition to 20 to 30 wt.% solids.
4. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that: further, the oxidant is ozone or hydrogen peroxide gas or oxygen.
5. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that: furthermore, the aeration rate of the oxidant is 10-18 g/h.L.
6. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that: further, the wavelength of the ultraviolet light is 200-300 nm.
7. The wet oxidation treatment method of low content organic waste salt according to claim 1, characterized in that: further, the pH value regulator is sodium hydroxide or sulfuric acid solution with the mass percentage concentration of 10% -20%.
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