CN107381841B - Preparation method and application of green scale inhibiting material with cellulose as raw material - Google Patents
Preparation method and application of green scale inhibiting material with cellulose as raw material Download PDFInfo
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- CN107381841B CN107381841B CN201710806055.5A CN201710806055A CN107381841B CN 107381841 B CN107381841 B CN 107381841B CN 201710806055 A CN201710806055 A CN 201710806055A CN 107381841 B CN107381841 B CN 107381841B
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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
Abstract
The application discloses a preparation method of a green scale inhibition material taking cellulose as a raw material, which comprises the following steps: (1) extracting cellulose; (2) cellulose oxidation; (3) the oxidized cellulose is carboxylated. The green scale inhibiting material prepared by the method has the carboxyl content of 25-30% by mass and the pH of 6.8-7.2. In addition, the application also relates to application of the green scale inhibition material. The preparation method comprises the steps of oxidizing cellulose and then carboxylating to obtain a green scale inhibiting material (ST3), which is an environment-friendly novel scale inhibitor and has the properties of naturalness, no toxicity and easy biodegradation; can resist high salt, high temperature, strong acid and strong alkali environment, and has wide application range.
Description
Technical Field
The application relates to the technical field of water treatment, in particular to a preparation method and application of a green scale inhibition material taking cellulose as a raw material.
Background
Industrial circulating water precipitates a large amount of dissolved salts to adhere to the inner walls of equipment and pipelines during operation, and the precipitates are called scale, wherein calcium carbonate is the main component. Circulating water can also directly or indirectly corrode metal equipment within the circulating water system.
Cellulose is a natural compound rich in hydroxyl, and oxidation and carboxylation are carried out, so that the scale inhibition performance is greatly improved, the characteristics of stable property and high temperature and high salt resistance are realized, and the cellulose can be widely applied to industrial circulating water, for example, CN106277375A discloses an environment-friendly scale and corrosion inhibitor and a preparation method and application thereof, wherein the scale and corrosion inhibitor is composed of the following raw materials in parts by weight: 7-15 parts of microcrystalline cellulose, 5-12 parts of acrylic emulsion, 23-31 parts of halloysite, 15-23 parts of polyethylene glycol and 3-8 parts of acetyl tributyl citrate, and has the advantages of good corrosion inhibition performance, high scale inhibition efficiency and the like. CN102627359A introduces a phosphorus-free composite corrosion and scale inhibitor containing natural biodegradable substances, which is prepared by mixing the following raw materials: the corrosion inhibitor can avoid the deposition of calcium carbonate, calcium sulfate and calcium phosphate by adopting the corrosion inhibitor in the circulating cooling water treatment, and has obvious scale inhibition effect and excellent corrosion inhibition performance.
However, although the existing scale inhibitors contain cellulose components, the overall composition is complex and the preparation steps are complicated.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method and application of a green scale inhibiting material taking cellulose as a raw material.
In order to achieve the above purpose, the invention provides a preparation method and application of a green scale inhibition material using cellulose as a raw material, which adopts the following technical scheme:
a method for preparing a green scale inhibition material by taking cellulose as a raw material comprises the following steps:
(1) extracting cellulose: boiling plant in 5% NaOH solution for 100min, cooling to 70 deg.C, adding 10% hydrogen peroxide (H)2O2) Continuously heating for 1h, keeping the temperature at 70 ℃, then filtering, fully washing filter residue to be neutral by using distilled water, and drying to obtain cellulose for later use;
(2) cellulose oxidation: preparing a cellulose solution with the mass concentration of 30% from the cellulose obtained in the step (1) by using pure water as a solvent, adding the cellulose solution into a reaction tank, adjusting the pH to 7.5, maintaining the temperature at 50 ℃, adding hydrogen peroxide with the mass of 2% of the dry basis mass of the cellulose, reacting for 4 hours, washing and drying;
(3) carboxylation of oxidized cellulose: and (3) adding pure water and HClO with the mass fraction of 1% into the oxidized cellulose obtained in the step (2), refluxing and heating, cooling and drying to obtain the scale inhibition material.
The carboxyl content of the prepared green scale inhibiting material can reach 25-30% by mass fraction.
The pH value of the prepared green scale inhibition material is 6.8-7.2.
Preferably, Na is used in the step (2)2CO3The pH was adjusted.
Preferably, the mass of the pure water added in the step (3) is 2 times that of the oxidized cellulose, and the mass of the 1% HClO added is 5% of that of the oxidized cellulose.
Preferably, the reflux heating time in the step (3) is 10 h.
The green scale inhibition material prepared by the method is applied to water treatment.
The green scale inhibiting material prepared by the method can be applied to household domestic water treatment, including the pretreatment of water for electric water heaters and solar water heaters, and also can be applied to prefilters, faucet filters and water purifiers.
Compared with the prior art, the scale inhibition material prepared by the preparation method has the following beneficial effects:
(1) the preparation method comprises the steps of oxidizing cellulose and then carboxylating to obtain the green scale inhibiting material (ST3), which is an environment-friendly novel scale inhibitor and has the properties of naturalness, no toxicity and easy biodegradation.
(2) The obtained green scale inhibiting material (ST3) has an obvious scale inhibiting effect, and the scale inhibiting efficiency can reach more than 95% by 5-10 ppm; the green scale inhibition material has stable property and low solubility, can be used for a long time, and cannot be quickly dissolved to lose the long-term scale inhibition effect; the pH value of the green scale inhibition material tends to be neutral, is 6.8-7.2, is beneficial to processing equipment and environment, and does not change the acid-base environment; the ST3 material can resist high salt, high temperature, strong acid and strong alkali environment, and has wide application range.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
A method for preparing a green scale inhibition material by taking cellulose as a raw material comprises the following steps:
(1) extracting cellulose: boiling plant in 5% NaOH solution for 100min, cooling to 70 deg.C, adding 10% hydrogen peroxide (H)2O2) Continuously heating for 1h, keeping the temperature at 70 ℃, then filtering, fully washing filter residue to be neutral by using distilled water, and drying to obtain cellulose for later use;
(2) cellulose oxidation: the cellulose obtained in the step (1) is treatedPreparing a cellulose solution with the mass concentration of 30% by adopting pure water as a solvent, adding the cellulose solution into a reaction tank, and adding Na2CO3Adjusting the pH value to 7.5, maintaining the temperature at 50 ℃, adding hydrogen peroxide with the dry basis weight of the cellulose obtained in the step (1) being 2%, reacting for 4h, washing and drying;
(3) carboxylation of oxidized cellulose: and (3) adding 2 times of the mass of pure water and 1% of HClO into the oxidized cellulose obtained in the step (2), wherein the mass of the added pure water is 2 times of that of the oxidized cellulose added in the step, the mass of the added 1% of HClO is 5% of that of the oxidized cellulose added in the step, refluxing and heating for 10h, and cooling and drying to obtain the scale inhibition material.
The carboxyl content of the prepared green scale inhibiting material is 25-30% by mass fraction.
The pH value of the prepared green scale inhibition material is 6.8-7.2.
Hard water preparation: 2.740g of calcium carbonate and 0.276g of magnesium oxide were weighed out, dissolved with a small amount of 2mol/L hydrochloric acid and evaporated to dryness on a water bath to remove excess hydrochloric acid. The residue was then transferred completely to a 100mL volumetric flask with water and diluted to the mark with distilled water, and 10mL of this solution was taken out in a 1000mL volumetric flask and diluted to the mark with distilled water.
The green scale inhibition material prepared in the embodiment is used in the prepared water for scale inhibition rate test:
the scale inhibition rate calculation formula is as follows:
in the formula, V is the volume of EDTA consumed by the unheated blank water sample, and the unit is mL; VC is the volume of EDTA (ethylene diamine tetraacetic acid) consumed by a water sample added with the scale inhibitor after heating, and the unit is mL; v0 is the volume of EDTA (ethylene diamine tetraacetic acid) consumed by a water sample without the scale inhibitor after heating, and the unit is mL; k is concentration multiple.
In the titration process, when the color is changed from wine red to blue, the titration reaches the end point, and after the test is finished, the scale inhibition rate is 96 percent.
Example 2
A method for preparing a green scale inhibition material by taking cellulose as a raw material comprises the following steps:
(1) extracting cellulose: boiling plant in 5% NaOH solution for 100min, cooling to 70 deg.C, adding 10% hydrogen peroxide (H)2O2) Continuously heating for 1h, keeping the temperature at 70 ℃, then filtering, fully washing filter residue to be neutral by using distilled water, and drying to obtain cellulose for later use;
(2) cellulose oxidation: preparing the cellulose obtained in the step (1) into a cellulose solution with the mass concentration of 30%, adding the cellulose solution into a reaction tank, and adding Na2CO3Adjusting the pH value to 7.5, maintaining the temperature at 50 ℃, adding hydrogen peroxide with the cellulose dry basis amount of 2%, reacting for 4h, washing and drying;
(3) carboxylation of oxidized cellulose: and (3) adding 2 times of the mass of pure water and 1% of HClO into the oxidized cellulose obtained in the step (2), wherein the mass of the added pure water is 2 times of that of the oxidized cellulose added in the step, the mass of the added 1% of HClO is 5% of that of the oxidized cellulose added in the step, refluxing and heating for 10h, and cooling and drying to obtain the scale inhibition material.
The carboxyl content of the prepared green scale inhibiting material is 25-30% by mass fraction.
The pH value of the prepared green scale inhibition material is 6.8-7.2.
Hard water preparation: 2.740g of calcium carbonate and 0.276g of magnesium oxide were weighed out, dissolved with a small amount of 2mol/L hydrochloric acid and evaporated to dryness on a water bath to remove excess hydrochloric acid. The residue was then transferred completely to a 100mL volumetric flask with water and diluted to the mark with distilled water, and 10mL of this solution was taken out in a 1000mL volumetric flask and diluted to the mark with distilled water.
The green scale inhibition material prepared in the embodiment is used in prepared water for scale inhibition rate test, and the scale inhibition rate test standard and method are as follows:
the scale inhibition rate calculation formula is as follows:
in the formula, V is the volume of EDTA consumed by the unheated blank water sample, and the unit is mL; VC is the volume of EDTA (ethylene diamine tetraacetic acid) consumed by a water sample added with the scale inhibitor after heating, and the unit is mL; v0 is the volume of EDTA (ethylene diamine tetraacetic acid) consumed by a water sample without the scale inhibitor after heating, and the unit is mL; k is concentration multiple.
In the titration process, when the color is changed from wine red to blue, the titration reaches the end point, and after the test is finished, the scale inhibition rate is measured to be 95.8%.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (5)
1. A method for preparing a green scale inhibition material by taking cellulose as a raw material is characterized by comprising the following steps: (1) extracting cellulose: boiling plants in NaOH with the mass concentration of 5% for 100min, adding hydrogen peroxide with the mass concentration of 10% when the temperature of the solution is reduced to 70 ℃, continuously heating for 1h, keeping the temperature at 70 ℃, filtering, fully washing filter residues with distilled water to be neutral, and drying to obtain cellulose for later use;
(2) cellulose oxidation: preparing a cellulose solution with the mass concentration of 30% from the cellulose obtained in the step (1) by using pure water as a solvent, adding the cellulose solution into a reaction tank, adjusting the pH to 7.5, maintaining the temperature at 50 ℃, adding hydrogen peroxide with the mass of 2% of the dry basis mass of the cellulose, reacting for 4 hours, washing and drying;
(3) carboxylation of oxidized cellulose: adding pure water and HClO with the mass fraction of 1% into the oxidized cellulose obtained in the step (2), refluxing and heating, cooling and drying to obtain a scale inhibition material; the carboxyl content of the prepared green scale inhibiting material reaches 25-30% by mass;
the mass of the pure water added in the step (3) is 2 times that of the oxidized cellulose, and the mass of the added 1% HClO is 5% of that of the oxidized cellulose; the time for reflux heating in the step (3) is 10 hours.
2. The method for preparing the green scale inhibition material by taking cellulose as the raw material according to claim 1, wherein the pH value of the prepared green scale inhibition material is 6.8-7.2.
3. The method for preparing the green scale inhibiting material taking cellulose as the raw material according to claim 1, wherein Na is adopted in the step (2)2CO3The pH was adjusted.
4. The green scale inhibition material prepared by the method according to any one of claims 1 to 3 and taking cellulose as a raw material is applied to water treatment.
5. The green scale inhibition material prepared by the method according to any one of claims 1 to 3 and taking cellulose as a raw material is applied to household water treatment.
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| CN110342654B (en) * | 2019-05-30 | 2021-12-21 | 智淳新材料科技(广州)有限公司 | Phosphorus-free corrosion and scale inhibitor and preparation method thereof |
| CN110330122B (en) * | 2019-05-30 | 2021-12-21 | 智淳新材料科技(广州)有限公司 | Multifunctional environment-friendly water treatment agent and preparation method thereof |
| CN114456277B (en) * | 2022-02-22 | 2023-03-21 | 华电电力科学研究院有限公司 | Preparation method of ternary scale and corrosion inhibitor |
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| CN103790056A (en) * | 2012-10-31 | 2014-05-14 | 中国科学院青岛生物能源与过程研究所 | Method for pretreating cellulosic biomass |
| CN104017090A (en) * | 2014-05-05 | 2014-09-03 | 华南理工大学 | Method for preparing carboxycellulose by using hydrogen peroxide |
| CN105131131A (en) * | 2015-09-24 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Synthesis method of high-carboxylation-degree oxidized cellulose |
| CN105143547A (en) * | 2013-03-15 | 2015-12-09 | Gp纤维素股份有限公司 | Low viscosity kraft fiber having enhanced carboxyl content and methods of making and using the same |
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| US6524348B1 (en) * | 1999-03-19 | 2003-02-25 | Weyerhaeuser Company | Method of making carboxylated cellulose fibers and products of the method |
| JP2003073402A (en) * | 2001-06-06 | 2003-03-12 | Weyerhaeuser Co | Method for producing stabilized carboxylated cellulose |
| CN103790056A (en) * | 2012-10-31 | 2014-05-14 | 中国科学院青岛生物能源与过程研究所 | Method for pretreating cellulosic biomass |
| CN105143547A (en) * | 2013-03-15 | 2015-12-09 | Gp纤维素股份有限公司 | Low viscosity kraft fiber having enhanced carboxyl content and methods of making and using the same |
| CN104017090A (en) * | 2014-05-05 | 2014-09-03 | 华南理工大学 | Method for preparing carboxycellulose by using hydrogen peroxide |
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