CN113582276A - Anti-carbonization agent and preparation method thereof - Google Patents
Anti-carbonization agent and preparation method thereof Download PDFInfo
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- CN113582276A CN113582276A CN202110899250.3A CN202110899250A CN113582276A CN 113582276 A CN113582276 A CN 113582276A CN 202110899250 A CN202110899250 A CN 202110899250A CN 113582276 A CN113582276 A CN 113582276A
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/042—Prevention of deposits
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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
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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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
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/04—Surfactants, used as part of a formulation or alone
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Abstract
The invention belongs to the technical field of wastewater treatment generated in furfural production, and particularly provides an anti-carbonization agent, which comprises the following components in percentage by mass relative to the total mass of the anti-carbonization agent: 10-20% of modified organic silicone oil, 1-15% of organic acid, 1-5% of antioxidant, 1-3% of surfactant and the balance of deionized water; the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, organic acid and antioxidant into a reaction kettle A, stirring and dissolving uniformly, sequentially adding a defoaming agent, a surfactant and prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent; the prepared anti-coking agent can obviously slow down the coking speed of the evaporator, prolongs the cleaning period, is easier to soften and clean the coked substances, and has obvious effect.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment generated in furfural production, and particularly relates to a preparation method of an anti-carbonization agent.
Background
The furfural is used as an important chemical raw material and has wide application. Most of the current furfural production processes are prepared by dehydration after acid-catalyzed hydrolysis of biomass (such as corncobs and bagasse) rich in pentosan under high-temperature steam (160-. And (3) after the generated furfural is discharged from the hydrolysis kettle along with high-temperature water vapor, distilling, concentrating and purifying to obtain a furfural product. The waste water discharged by distillation is heated and pressurized by high-temperature steam (180 ℃) in an evaporation kettle for gasification and then recycled. Because furfural has a certain solubility in water and furfural is easily thermally decomposed and polymerized at high temperature. The waste water contains a small amount of furfural and other organic pasty byproducts generated in the furfural production process, the substances are further polymerized and carbonized in the waste water evaporation process and adsorbed on the wall of a heat exchange pipe in the evaporator, so that the efficiency of the evaporator is gradually reduced, the evaporator needs to be cleaned by carbon deposition after being used for a period of time, and the production progress is influenced by time and labor consumption.
The problem of coking of the furfural wastewater evaporator is an industry common problem, and a scheme which is not solved in the market at present is not provided, so that the research on the problem of coking resistance of furfural wastewater evaporation has important scientific research significance and economic value.
Disclosure of Invention
In order to solve the problems, the invention provides an anti-carbonization agent and a preparation method thereof.
The technical scheme of the invention is as follows:
an anti-caking agent consisting of the following contents in percentage by mass relative to the total mass of the anti-caking agent:
the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, organic acid and antioxidant into a reaction kettle, stirring and dissolving uniformly, sequentially adding the defoaming agent, the surfactant and the prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent.
Further, the molecular structural formula of the modified silicone oil is as follows:
wherein the molar ratio of (x + y)/(m + n) is less than 0.3, preferably less than 0.15.
Further, the modified silicone oil is synthesized by methyl hydrogen-containing silicone oil, a monomer containing unsaturated double bonds and epoxy groups and water-soluble organic amine.
Further, the methyl hydrogen silicone oil has a viscosity in the range of 20 to 100 mPas, preferably 30 to 60 mPas.
Further, the monomer containing unsaturated double bonds and epoxy groups is one or a combination of allyl glycidyl ether, glycidyl methacrylate and glycidyl acrylate.
Preferably, the monomer containing an unsaturated double bond and an epoxy group is allyl glycidyl ether.
Further, the water-soluble organic amine is one or a combination of more of ethanolamine, diethanolamine, isopropanolamine, diisopropanolamine and ethylenediamine.
Preferably, the water-soluble organic amine is one or two of diethanolamine and diisopropanolamine.
Further, the organic acid is one or a combination of more of maleic acid, fumaric acid, itaconic acid, acrylic acid and methacrylic acid.
Preferably, the organic acid is one or more of acrylic acid, methacrylic acid and maleic acid.
Further, the antioxidant is one or more of resorcinol, hydroquinone, tannin, gallic acid, pyrogallic acid, ascorbic acid, and combinations thereof.
Preferably, the antioxidant is one or more of tannin, pyrogallic acid and ascorbic acid.
Further, the surfactant is fatty alcohol-polyoxyethylene ether with HLB value greater than 12, and the defoaming agent is an organic silicon defoaming agent or a polyether defoaming agent.
Further, the preparation process of the modified silicone oil is as follows:
a. weighing a specified amount of monomers of unsaturated double bonds and epoxy groups, adding the monomers into a reaction kettle, adding a platinum catalyst, wherein the effective component of the platinum catalyst is 0.002 percent of the mass of the monomers of the unsaturated double bonds and the epoxy groups, uniformly stirring, adding cyclohexanone with the mass of hydrogen-containing silicone oil and the like, controlling the molar ratio of Si-H bonds of the hydrogen-containing silicone oil to the unsaturated double bonds of the monomers to be 1: 1, stirring, heating to 60-80 ℃, and keeping the temperature for 5 hours.
b. Adding specified amount of organic amine into a reaction kettle, keeping the molar ratio of epoxy group to organic amine molecule at 1: 1.5, keeping the temperature at 80 ℃ for 3h, and then carrying out reduced pressure distillation to remove unreacted organic amine and solvent cyclohexanone, thus obtaining the modified organic silicone oil.
The invention has the beneficial effects that:
according to the anti-carbonization agent provided by the invention, the organic acid and the modified silicone oil are subjected to acid-base reaction to enable the modified silicone oil to have positive charge and water solubility, the organic silicon main chain has good high temperature resistance, and can well disperse tiny particles formed by organic matter polymerization and carbonization in the furfural wastewater evaporation process, and the modified organic silicone oil is compounded with the nonionic surfactant to enable dispersed carbide particles to be more stable, so that the modified silicone oil is not easy to adsorb the tube wall of an evaporator and is discharged along with distillation residual liquid; on the other hand, furfural and other organic impurities can generate oxygen radicals to carry out complex polymerization and decomposition under the high-temperature aerobic environment (160-.
The anti-coking agent can obviously slow down the coking speed of the evaporator, prolong the cleaning period, enable the carbonized substances to be more easily softened and cleaned and have obvious effect.
Drawings
FIG. 1 is a daily evaporation capacity decay curve of furfural wastewater.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Firstly, preparing modified organic silicone oil according to the following steps:
a. weighing a specified amount of allyl glycidyl ether, adding the allyl glycidyl ether into a reaction kettle, adding a platinum catalyst, wherein the effective component of the platinum catalyst is 0.002 percent of the mass of an allyl glycidyl ether monomer, uniformly stirring, adding hydrogen-containing silicone oil with 1.5 percent of hydrogen content and 35mPa & s viscosity and cyclohexanone with equal mass, controlling the molar ratio of Si-H bonds of the hydrogen-containing silicone oil to unsaturated double bonds of the monomer to be 1: 1, stirring, heating to 60 ℃, and keeping the temperature for 5 hours;
b. and adding a specified amount of diethanol amine into the reaction kettle, wherein the molar ratio of the epoxy group to the diethanol amine molecule is 1: 1.5, preserving the temperature at 80 ℃ for 3 hours, and then carrying out reduced pressure distillation to remove unreacted diethanol amine and solvent cyclohexanone, thus obtaining the modified organic silicon oil.
And finally, weighing the following components in percentage by mass relative to the total mass of the anti-coking agent for later use:
the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, acrylic acid and ascorbic acid into a reaction kettle, stirring and dissolving uniformly, sequentially adding the defoaming agent, the surfactant MOA-9 and the prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent.
The anti-carbonization agent of example 1 is added into furfural wastewater, and the daily evaporation capacity decay trends of the evaporator when the addition amount of the anti-carbonization agent is 0.05 percent and 0.1 percent of the amount of the wastewater and a blank wastewater control sample are respectively tested, and the results are shown in the attached figure.
Example 2
Firstly, preparing modified silicone oil according to the following steps:
a. weighing a specified amount of glycidyl acrylate, adding the glycidyl acrylate into a reaction kettle, adding a platinum catalyst, wherein the effective component of the platinum catalyst is 0.002 percent of the mass of a glycidyl acrylate monomer, uniformly stirring, adding hydrogen-containing silicone oil with the hydrogen content of 1.3 percent and the viscosity of 100mPa & s and cyclohexanone with the same mass, controlling the molar ratio of Si-H bonds of the hydrogen-containing silicone oil to unsaturated double bonds of the monomer to be 1: 1, stirring, heating to 60 ℃, and keeping the temperature for 5 hours;
b. and adding a specified amount of diethanol amine into the reaction kettle, wherein the molar ratio of the epoxy group to the diethanol amine molecule is 1: 1.5, preserving the temperature at 80 ℃ for 3 hours, and then carrying out reduced pressure distillation to remove unreacted diethanol amine and solvent cyclohexanone, thus obtaining the modified organic silicon oil.
And finally, weighing the following components in percentage by mass relative to the total mass of the anti-coking agent for later use:
the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, maleic acid and pyrogallic acid into a reaction kettle, stirring and dissolving uniformly, sequentially adding the defoaming agent, the surfactant MOA-15 and the prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent.
Example 3
Firstly, preparing modified organic silicon resin according to the following steps:
a. weighing a specified amount of glycidyl methacrylate, adding the glycidyl methacrylate into a reaction kettle, adding a platinum catalyst, wherein the effective component of the platinum catalyst is 0.002 percent of the mass of a glycidyl methacrylate monomer, uniformly stirring, adding hydrogen-containing silicone oil with the hydrogen content of 1.4 percent and the viscosity of 20mPa & s and cyclohexanone with the same mass, controlling the molar ratio of Si-H bonds of the hydrogen-containing silicone oil to unsaturated double bonds of the monomer to be 1: 1, stirring, heating to 80 ℃, and preserving the heat for 5 hours.
b. Adding a specified amount of diisopropanolamine into the reaction kettle, keeping the molar ratio of epoxy group to diisopropanolamine molecule at 1: 1.5, preserving the temperature at 80 ℃ for 3h, and then carrying out reduced pressure distillation to remove unreacted diisopropanolamine and solvent cyclohexanone, namely modified organic silicon oil.
And finally, weighing the following components in percentage by mass relative to the total mass of the anti-coking agent for later use:
the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, methacrylic acid and tannin into a reaction kettle, stirring and dissolving uniformly, sequentially adding the defoaming agent, the surfactant O-20 and the prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (10)
1. The anti-carbonization agent is characterized by comprising the following components in percentage by mass relative to the total mass of the anti-carbonization agent:
the preparation method of the anti-carbonization agent comprises the steps of adding weighed deionized water, organic acid and antioxidant into a reaction kettle, stirring and dissolving uniformly, sequentially adding the defoaming agent, the surfactant and the prepared modified organic silicone oil, and stirring uniformly to obtain the anti-carbonization agent.
2. The anti-carbonization agent as claimed in claim 1, wherein the modified silicone oil has the following molecular structural formula:
wherein the molar ratio (x + y)/(m + n) is less than 0.3.
3. The anti-carbonization agent according to claim 2, wherein the modified silicone oil is synthesized from methyl hydrogen-containing silicone oil, a monomer containing an unsaturated double bond and an epoxy group, and a water-soluble organic amine.
4. The anti-carbonation agent according to claim 3, wherein said methyl hydrogen silicone oil has a viscosity ranging from 20 to 100 mPa-s.
5. The anti-carbonizing agent according to claim 3, wherein the monomer having an unsaturated double bond and an epoxy group is one or more of allyl glycidyl ether, glycidyl methacrylate, and glycidyl acrylate.
6. The anti-caking agent according to claim 3 wherein the water-soluble organic amine is one or more of ethanolamine, diethanolamine, isopropanolamine, diisopropanolamine, ethylenediamine.
7. The anti-caking agent according to claim 1 wherein the organic acid is one or more of maleic acid, fumaric acid, itaconic acid, acrylic acid, methacrylic acid.
8. The anti-caking agent according to claim 1 wherein the antioxidant is one or more of resorcinol, hydroquinone, tannin, gallic acid, pyrogallol, ascorbic acid.
9. The anti-caking agent according to claim 1 wherein the surfactant is a fatty alcohol polyoxyethylene ether having an HLB value of greater than 12 and the defoaming agent is a silicone defoaming agent or a polyether defoaming agent.
10. The anti-coking agent according to claim 3, characterized in that the modified silicone oil is prepared by the following process:
a. weighing a specified amount of monomers of unsaturated double bonds and epoxy groups, adding the monomers into a reaction kettle, adding a platinum catalyst, wherein the effective component of the platinum catalyst is 0.002 percent of the mass of the monomers of the unsaturated double bonds and the epoxy groups, uniformly stirring, adding hydrogen-containing silicone oil and cyclohexanone with equal mass, controlling the molar ratio of Si-H bonds of the hydrogen-containing silicone oil to the unsaturated double bonds of the monomers to be 1: 1, stirring and heating to 60-80 ℃, and keeping the temperature for 5 hours;
b. adding specified amount of organic amine into a reaction kettle, keeping the molar ratio of epoxy group to organic amine molecule at 1: 1.5, keeping the temperature at 80 ℃ for 3h, and then carrying out reduced pressure distillation to remove unreacted organic amine and cyclohexanone solvent, thus obtaining the modified organic silicone oil.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB740720A (en) * | 1952-06-23 | 1955-11-16 | Du Pont | Chemical products |
| CN102516972A (en) * | 2011-12-07 | 2012-06-27 | 南京美思德新材料有限公司 | Comb-shaped modified polysiloxane anion water-base thick oil viscosity reducer and synthesizing method thereof |
| CN103214679A (en) * | 2013-05-06 | 2013-07-24 | 江南大学 | Preparation method of aminopolyether modified polysiloxane deforming agent |
| CN108949266A (en) * | 2018-07-20 | 2018-12-07 | 北京三聚环保新材料股份有限公司 | A kind of wood tar viscosity reduction polymerization inhibitor and its preparation method and application |
| WO2020261192A1 (en) * | 2019-06-27 | 2020-12-30 | Wacker Metroark Chemicals Pvt. Ltd. | Hydrophillic silicone made of olefinic unsaturated polyoxyalkylene glycidyl ether, its composition and preparation method thereof |
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- 2021-08-05 CN CN202110899250.3A patent/CN113582276B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB740720A (en) * | 1952-06-23 | 1955-11-16 | Du Pont | Chemical products |
| CN102516972A (en) * | 2011-12-07 | 2012-06-27 | 南京美思德新材料有限公司 | Comb-shaped modified polysiloxane anion water-base thick oil viscosity reducer and synthesizing method thereof |
| CN103214679A (en) * | 2013-05-06 | 2013-07-24 | 江南大学 | Preparation method of aminopolyether modified polysiloxane deforming agent |
| CN108949266A (en) * | 2018-07-20 | 2018-12-07 | 北京三聚环保新材料股份有限公司 | A kind of wood tar viscosity reduction polymerization inhibitor and its preparation method and application |
| WO2020261192A1 (en) * | 2019-06-27 | 2020-12-30 | Wacker Metroark Chemicals Pvt. Ltd. | Hydrophillic silicone made of olefinic unsaturated polyoxyalkylene glycidyl ether, its composition and preparation method thereof |
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