CN107381841A - A kind of preparation method and application using cellulose as the green scale material of raw material - Google Patents
A kind of preparation method and application using cellulose as the green scale material of raw material Download PDFInfo
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- CN107381841A CN107381841A CN201710806055.5A CN201710806055A CN107381841A CN 107381841 A CN107381841 A CN 107381841A CN 201710806055 A CN201710806055 A CN 201710806055A CN 107381841 A CN107381841 A CN 107381841A
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- cellulose
- green scale
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- raw material
- scale material
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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
This application discloses a kind of preparation method using cellulose as the green scale material of raw material, comprise the following steps：(1) cellulose extracts；(2) cellulose oxidation；(3) oxycellulose carboxylated.The carboxyl-content for the green scale material being prepared according to this method reaches 25%~30%, pH for 6.8~7.2 in terms of mass fraction.Other the application further relates to the application of green scale material.The application preparation method is natural by first by cellulose oxidation, then the green scale material (ST3) that carboxylated obtains is a kind of Novel scale inhibitor of environment-friendly type, having, nontoxic, the performance being readily biodegradable；Can high salt tolerance, high temperature, strong acid and strong base environment is applied widely.
Description
Technical field
The application is related to water-treatment technology field, and specifically, the application is related to a kind of green using cellulose as raw material
The preparation method and application of scale inhibition material.
Background technology
Industrial circulating water can separate out substantial amounts of dissolved salts and be attached on the inwall of equipment and pipeline in operation, this
Precipitating thing is referred to as incrustation scale, wherein based on calcium carbonate.Recirculated water can also be directly or indirectly to hardware in circulation
Corroded.
Cellulose is a kind of native compound rich in hydroxyl, through peroxidating and carboxylated, increases its scale inhibition performance significantly
Can, its character is stable, the characteristic of high-temperature-resistant high-salt, it is can be widely applied in industrial cycle water, for example,
CN106277375A discloses a kind of environment-friendly type anti-incrustation corrosion inhibitor and its preparation method and application, and the anti-incrustation corrosion inhibitor by pressing below
Formed according to the raw material of parts by weight：Microcrystalline cellulose 7-15 parts, acrylic emulsion 5-12 parts, red halloysite 23-31 parts, polyethylene glycol
15-23 parts, tributyl 2-acetylcitrate 3-8 parts, have the advantages that corrosion inhibition is good, scale inhibition efficiency high.CN102627359A is situated between
Continued a kind of without phosphorus composite slow-corrosion scale resistor containing natural biodegradable thing, is mixed by following raw materials：Zinc sulfate or nitre
Sour zinc, APG, poly-aspartate, carboxymethyl cellulose, poly-epoxy succinic acid, polymeric amino acid, sodium gluconate, methyl
Benzotriazole or benzotriazole, water or deionized water, calcium carbonate, calcium sulfate, phosphorus can be avoided using this agent in circulating water cooling treatment
The deposition of sour calcium, scale inhibition effect is obvious, and corrosion inhibition is excellent.
But although the component containing cellulose in existing numerous antisludging agents, overall composition complexity, preparation process are numerous
It is trivial.
The content of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of using cellulose as raw material
The preparation method and application of green scale material.
To realize object above, a kind of preparation side using cellulose as the green scale material of raw material provided by the invention
Method and application, are adopted the following technical scheme that：
A kind of preparation method using cellulose as the green scale material of raw material, comprise the following steps：
(1) cellulose extracts：By plant after mass concentration is to boil 100min in 5% NaOH, treat that solution temperature drops
During to 70 DEG C, the hydrogen peroxide (H that mass concentration is 10% is added2O2), continue to heat 1h, maintain the temperature at 70 DEG C, filter afterwards,
Filter residue is fully washed with distilled water to neutrality, cellulose is obtained after drying, it is stand-by；
(2) cellulose oxidation：The cellulose that step (1) is obtained, use pure water as solvent be configured to mass concentration for
30% cellulose solution is added in retort, is adjusted to pH=7.5, is maintained temperature 50 C, and add cellulose butt matter
The hydrogen peroxide of amount 2%, 4h is reacted, washed, dried；
(3) oxycellulose carboxylated：The cellulose for the oxidation that step (2) is obtained, add pure water and mass fraction 1%
HClO, be heated at reflux, cool drying, obtain scale inhibition material.
The carboxyl-content of the green scale material being prepared can reach 25%~30% in terms of mass fraction.
The pH of the green scale material being prepared is 6.8~7.2.
Preferably, Na is used in the step (2)2CO3Adjust PH.
Preferably, the quality of the pure water added in the step (3) is 2 times of the cellulose of oxidation, the 1% of addition
HClO quality is the 5% of the cellulose of oxidation.
Preferably, the time being heated at reflux in the step (3) is 10h.
The green scale materials application being prepared according to the above method is in water process.
The green scale material being prepared according to the above method, it can apply to household water processing, including electricity
Water heater, the pretreatment with water of solar water heater, also including fore filter, in faucet water purifier and water purifier should
With.
Compared with prior art, the scale inhibition material that the application preparation method is prepared, has the advantages that：
(1) the application preparation method by being first by cellulose oxidation, then the green scale material (ST3) that carboxylated obtains
A kind of Novel scale inhibitor of environment-friendly type, there is natural, nontoxic, the performance being readily biodegradable.
(2) green scale material (ST3) scale inhibition effect obtained by the application is obvious, and 5~10ppm can effectively reach 95%
Scale inhibition efficiency above；Green scale material character itself is stable, and solubility is low, can be long-term use of, will not quickly dissolve and
Lose the effect of long-term scale inhibition；Green scale material pH value tends to be neutral, between being 6.8~7.2, to the equipment and environment of processing
Favorably, its acid or alkali environment will not be changed；ST3 materials can high salt tolerance, high temperature, strong acid and strong base environment is applied widely.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
A kind of preparation method using cellulose as the green scale material of raw material, comprise the following steps：
(1) cellulose extracts：By plant after mass concentration is to boil 100min in 5% NaOH, treat that solution temperature drops
During to 70 DEG C, the hydrogen peroxide (H that mass concentration is 10% is added2O2), continue to heat 1h, maintain the temperature at 70 DEG C, filter afterwards,
Filter residue is fully washed with distilled water to neutrality, cellulose is obtained after drying, it is stand-by；
(2) cellulose oxidation：The cellulose that step (1) is obtained, use pure water as solvent be configured to mass concentration for
30% cellulose solution is added in retort, uses Na2CO3Regulation maintains temperature 50 C, and add step to pH=7.5
(1) hydrogen peroxide of the cellulose butt amount 2% obtained, 4h is reacted, washed, dried；
(3) oxycellulose carboxylated：The cellulose for the oxidation that step (2) is obtained, add the pure water and matter of 2 times of quality
Measure the HClO of fraction 1%, the quality of the pure water of addition is 2 times of the cellulose of the oxidation added in this step, the 1% of addition
HClO quality is the 5% of the cellulose of the oxidation added in this step, is heated at reflux 10h, cool drying, obtains scale inhibition material
Material.
The carboxyl-content of the green scale material being prepared reaches 25%~30% in terms of mass fraction.
The pH of the green scale material being prepared is 6.8~7.2.
The configuration of hard water：2.740g calcium carbonate and 0.276g magnesia are weighed, with a small amount of 2mol/L dissolving with hydrochloric acid, in water-bath
On be evaporated to dryness to remove unnecessary hydrochloric acid.Then residue is transferred in 100mL volumetric flasks completely with swallow distilled water, and with steam
Distilled water is diluted to scale, the 10mL solution is further taken out in 1000mL volumetric flask, with distilled water diluting to scale.
The Ying Shuizhong that the green scale material prepared in the present embodiment is used to configure, carry out scale inhibition performance test：
Scale inhibition performance calculation formula is:
In formula, EDTA volumes that V is consumed for non-heated blank water sample, unit mL；VC is the water sample added with antisludging agent
The EDTA volumes consumed after heating, unit mL；V0 is the EDTA volumes not consumed plus after the water sample heating of antisludging agent, singly
Position is mL；K is cycles of concentration.
In titration process, when color is by wine red change blueness, titration reaches terminal, and after off-test, the scale inhibition performance measured is
96%.
Embodiment 2
A kind of preparation method using cellulose as the green scale material of raw material, comprise the following steps：
(1) cellulose extracts：By plant after mass concentration is to boil 100min in 5% NaOH, treat that solution temperature drops
During to 70 DEG C, the hydrogen peroxide (H that concentration is 10% is added2O2), continue to heat 1h, maintain the temperature at 70 DEG C, filter afterwards, with steaming
Distilled water fully washs filter residue to neutrality, and cellulose is obtained after drying, stand-by；
(2) cellulose oxidation：The cellulose that step (1) is obtained, it is configured to the cellulose solution that mass concentration is 30%
It is added in retort, uses Na2CO3Regulation maintains temperature 50 C, and add the dioxygen of cellulose butt amount 2% to pH=7.5
Water, 4h is reacted, washed, dried；
(3) oxycellulose carboxylated：The cellulose for the oxidation that step (2) is obtained, add the pure water and matter of 2 times of quality
Measure the HClO of fraction 1%, the quality of the pure water of addition is 2 times of the cellulose of the oxidation added in this step, the 1% of addition
HClO quality is the 5% of the cellulose of the oxidation added in this step, is heated at reflux 10h, cool drying, obtains scale inhibition material
Material.
The carboxyl-content of the green scale material being prepared reaches 25%~30% in terms of mass fraction.
The pH of the green scale material being prepared is 6.8~7.2.
The configuration of hard water：2.740g calcium carbonate and 0.276g magnesia are weighed, with a small amount of 2mol/L dissolving with hydrochloric acid, in water-bath
On be evaporated to dryness to remove unnecessary hydrochloric acid.Then residue is transferred in 100mL volumetric flasks completely with swallow distilled water, and with steam
Distilled water is diluted to scale, the 10mL solution is further taken out in 1000mL volumetric flask, with distilled water diluting to scale.
The Ying Shuizhong that the green scale material prepared in the present embodiment is used to configure, carry out scale inhibition performance test, scale inhibition performance
Testing standard and method：
Scale inhibition performance calculation formula is:
In formula, EDTA volumes that V is consumed for non-heated blank water sample, unit mL；VC is the water sample added with antisludging agent
The EDTA volumes consumed after heating, unit mL；V0 is the EDTA volumes not consumed plus after the water sample heating of antisludging agent, singly
Position is mL；K is cycles of concentration.
In titration process, when color is by wine red change blueness, titration reaches terminal, and after off-test, the scale inhibition performance measured is
95.8%.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of preparation method using cellulose as the green scale material of raw material, it is characterised in that comprise the following steps：
(1) cellulose extracts：By plant after mass concentration is to boil 100min in 5% NaOH, treat that solution temperature is down to 70
DEG C when, add mass concentration be 10% hydrogen peroxide, continue heat 1h, maintain the temperature at 70 DEG C, filter afterwards, filled with distilled water
Point washing filter residue obtains cellulose to neutrality after drying, stand-by；
(2) cellulose oxidation：The cellulose that step (1) is obtained, uses pure water to be configured to mass concentration as solvent as 30%
Cellulose solution be added in retort, adjust to pH=7.5, maintain temperature 50 C, and add cellulose butt quality 2%
Hydrogen peroxide, react 4h, wash, dry；
(3) oxycellulose carboxylated：The cellulose for the oxidation that step (2) is obtained, addition pure water and mass fraction 1%
HClO, after being heated at reflux, cooling, dry, obtain scale inhibition material.
2. the preparation method according to claim 1 using cellulose as the green scale material of raw material, it is characterised in that
The carboxyl-content for the green scale material being prepared reaches 25%~30% in terms of mass fraction.
3. the preparation method according to claim 1 using cellulose as the green scale material of raw material, it is characterised in that
The pH for the green scale material being prepared is 6.8~7.2.
4. the preparation method according to claim 1 using cellulose as the green scale material of raw material, it is characterised in that
Na is used in the step (2)2CO3Adjust PH.
5. the preparation method according to claim 1 using cellulose as the green scale material of raw material, it is characterised in that
The quality of the pure water added in the step (3) is 2 times of the cellulose of oxidation, and 1% HClO of addition quality is oxidation
Cellulose 5%.
6. the preparation method according to claim 1 using cellulose as the green scale material of raw material, it is characterised in that
The time being heated at reflux in the step (3) is 10h.
7. the green scale material using cellulose as raw material being prepared according to any one of claim 1~6 methods described
Applied to water process.
8. the green scale material using cellulose as raw material being prepared according to any one of claim 1~6 methods described
Applied to household water processing.
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| CN201710806055.5A CN107381841B (en) | 2017-09-08 | 2017-09-08 | Preparation method and application of green scale inhibiting material with cellulose as raw material |
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| CN110330122A (en) * | 2019-05-30 | 2019-10-15 | 广东智淳环境科技有限公司 | A kind of multi-functional environment-protection water treatment agent and preparation method thereof |
| CN110342654A (en) * | 2019-05-30 | 2019-10-18 | 广东智淳环境科技有限公司 | A kind of novel non-phosphate corrosion inhibiting and descaling agent and preparation method thereof |
| CN114456277A (en) * | 2022-02-22 | 2022-05-10 | 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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| CN114456277A (en) * | 2022-02-22 | 2022-05-10 | 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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