CN108675365A - A kind of preparation method of water purification agent - Google Patents
A kind of preparation method of water purification agent Download PDFInfo
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- CN108675365A CN108675365A CN201810538709.5A CN201810538709A CN108675365A CN 108675365 A CN108675365 A CN 108675365A CN 201810538709 A CN201810538709 A CN 201810538709A CN 108675365 A CN108675365 A CN 108675365A
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- water purification
- purification agent
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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
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention discloses a kind of preparation methods of water purification agent, using shellfish shell as raw material, it is handled through soda acid and chitin is made in potassium permanganate decoloration, then chitosan is prepared, prepared chitosan and Herba Andrographitis extracting solution are re-dubbed water purification agent, water purification agent prepared by the method have no toxic side effect when drinking water disinfection, without peculiar smell, does not generate secondary pollution.
Description
Technical field
The present invention relates to technical field of water purification, more particularly to a kind of preparation method of water purification agent.
Background technology
As Chinese society, rapid economic development and population constantly increase, shortage of water resources and water environment pollution day are increasingly
Play seriously constrains China's sustainable economic development, influences health, to meet industrial and agricultural production and people's living needs,
Using water wisely, water pollution processing and reuse are particularly important.Physico-chemical process, biochemical process, membrane separation technique, the analysis of electric osmose system etc.
Reason method is successively applied to industrial wastewater and sanitary sewage disposal.
Wastewater treatment in China industry development progress is later, before arriving reform and opening-up since the establishment of the nation, the demand of wastewater treatment in China
Mainly based on industry and the use of national defence tip.After reform and opening-up, the fast development of national economy, living standards of the people are shown
It writes and improves, pulled the demand of sewage disposal.Into after nineteen nineties, wastewater treatment in China industry entry is quickly sent out
The speedup in the duration of an exhibition, sewage disposal demand is horizontal far above the whole world.
The depuration quality of drinking water has been increasingly subject to the attention of people with the improvement of people's health awareness, however, now
Commonly used water purification agent is formulated with the broken and bentonite etc. with the capture huge sum of money function of dominant of adsorbent activity mostly, is had
Purifying water effect it is bad, some produces pure water with filter membrane, but it is excessive often to there is dechlorination, and water is made to be not easy to deposit long, and except
Also the shortcomings that making iron, zinc, calcium needed by human body element largely lose while heavy metal relation by marriage, lead.The present invention in view of the foregoing,
And provide a kind of preparation method for the water purification agent being re-dubbed the chitosan for extracting and preparing from shrimp shell, crab shell to people.
Invention content
The purpose of the present invention is to provide a kind of to the mankind and Environmental security, and raw material sources are abundant, are readily biodegradable, valence
The preparation method of the low water purification agent of lattice.
In order to achieve the goal above, the technical solution adopted in the present invention is：Commercially available chitosan is immersed in containing peroxidating
Hydrogen, water-soluble humic acid solution in, after being soaked for a period of time, filtering obtains filter residue, and gained filter residue is carried out at freezing three times
Reason thaws, the chitosan after defrosting is dried in the shade, fine powder is ground into, gained fine powder is carried out to radiation treatment at normal temperatures and pressures and is obtained
Low-molecular weight chitoglycan is obtained, the low-molecular weight chitoglycan is scattered in Herba Andrographitis extracting solution, multiple pin phenol sodium is added, is made compound
Body, in complex plus water purification agent is just made in artificial bentonite, and the low-molecular weight chitoglycan is relative molecular weight 105Below
Chitosan.
The specific preparation method of the low-molecular weight chitoglycan is as follows：
1) it is 5~12% hydrogenperoxide steam generator to take mass concentration, and water-soluble humic acid, the matter of water-soluble humic acid is added
Amount is the 0.2~0.6% of above-mentioned hydrogenperoxide steam generator, stirs evenly, obtains mixed liquor；
2) chitosan is immersed in mixed liquor obtained by step S1, the mass concentration of chitosan is 25~35%, impregnates 30
~50min, filtering, obtains filter residue；
3) filter residue obtained by step S2 is subjected to freezing processing three times, first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2~4h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1~3h, and third time cryogenic temperature is -19 DEG C,
Third time cooling time is 40~60min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40~60 mesh sieve, obtains
Fine powder；
4) fine powder obtained by step S3 being subjected to radiation treatment at normal temperatures and pressures, irradiation dose is 20~30kGy, dry,
To obtain the final product.
Through obtained low-molecular weight chitoglycan of degrading, especially relative molecular mass is 105Chitosan oligomer below, no
It is only soluble in water, also there is unique physiological activity and physico-chemical property, thus application range is widened significantly.As chitosan oligomer has
Promote spleen antibody tormation, inhibits the physiological function of tumour growth；The cholesterol in liver and serum can effectively be reduced；It can strengthen
Liver function prevents gout and gastric ulcer.In addition, it can be additionally used in food additives, the purification of immobilized enzyme, protein, papermaking
Industry and water treatment industry etc..Low-molecular weight chitoglycan preparation method has acid-hydrolysis method, oxidation degradation method, enzymatic isolation method and spoke
According to method etc..Enzyme edman degradation Edman is to carry out biodegradable method to chitosan with specificity or non-specific enzyme, using this method energy
Access the lower oligosaccharide of average relative molecular mass and monosaccharide.It is added without other reaction reagents in entire degradation process, without it
Its side reaction occurs, and degradation condition is mild, and degradation process and molecular weight of product distribution are relatively easy to control.The disadvantage is that used enzyme compared with
To be special, the vigor of enzyme is limited, while of high cost, and the production cycle is long, is difficult to industrialized production.Physical degradation methods are mainly
Using physics modes such as microwave, ultrasonic wave and gamma-rays come chitosan of degrading, the most commonly used is sonications.Ultrasonic degradation
Method is easy to operate, but 95% ultrasonic energy is acted on for system heat effect rather than product degradation, therefore degradation efficiency is relatively low,
Have that molecular weight of product is distributed more widely simultaneously, the higher problem of molecular weight.
The Herba Andrographitis extracting solution is extracted by following method：
1) dry Herba Andrographitis be crushed into 90 mesh sieve, the Extraction solvent of 10~20 times of quality is then added, is in rotating speed
It is stirred evenly under conditions of 800 revs/min；Then in the case where output power is the microwave condition of 1200W, 20~40 points of Microwave Extraction
Clock, filtering repeat extraction 2~3 times, merge extracting solution；
2) it is that 7~11kPa is concentrated into original volume under the conditions of temperature is 50~60 DEG C in vacuum degree by gained extracting solution
1/3~1/2, obtain Herba Andrographitis extracting solution.
The Extraction solvent be tap water, the ethanol solution of 30~70 weight %, a concentration of 1.0mol/L sodium chloride,
One or more of the hydrochloric acid of the acetic acid of a concentration of 0.1mol/L, a concentration of 0.01mol/L.
Due to the application of the above technical scheme, make compared with the prior art, the present invention has the following advantages：
The method have the characteristics that preparation method is simple, material source is extensive, at low cost, the water purification prepared in this way
Agent purifying water effect is good, has the function of sterilization, desinsection, especially more notable to the performance of heavy metal in trapping water, water purification amount
Greatly, and to needed by human body elements such as iron, zinc, calcium in water it is not filtered out, not only there is good catharsis to drinking water, it is right
Industry, sanitary sewage also share good catharsis and reach environmental requirement.
Specific implementation mode
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.
【Embodiment 1】
A) the preparation of low-molecular weight chitoglycan：
1) it is 5% hydrogenperoxide steam generator to take mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
2) 500g chitosans are immersed in mixed liquor obtained by step 1), the mass concentration of chitosan is 25%, is impregnated
30min, filtering, obtains filter residue；
3) filter residue obtained by step 2) is subjected to freezing processing three times, first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40 mesh sieve, obtains fine powder；
4) fine powder obtained by step 3) is subjected to radiation treatment at normal temperatures and pressures, irradiation dose 20kGy, it is dry to get.
B) the preparation of Herba Andrographitis extracting solution
1) the 500g Herba Andrographitis dried be crushed into 90 mesh sieve, 10Kg water is then added, be 800 revs/min in rotating speed
Under the conditions of stir evenly；Then in the case where output power is the microwave condition of 1200W, Microwave Extraction 40 minutes, filtering repeats to extract
3 times, merge extracting solution；
2) it is that 11kPa is concentrated into the 1/2 of original volume, obtains under the conditions of temperature is 60 DEG C in vacuum degree by gained extracting solution
Herba Andrographitis extracting solution.
C water purification agent) is prepared
10g chitosans are scattered in 50mL Herba Andrographitis extracting solutions, 10g is added to sell phenol sodium again, complex are made, in complex
In plus the artificial bentonites of 20g just be made water purification agent.
【Embodiment 2】
A) the preparation of low-molecular weight chitoglycan：
1) it is 5% hydrogenperoxide steam generator to take mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
2) 10kg chitosans are immersed in mixed liquor obtained by step 1), the mass concentration of chitosan is 25%, is impregnated
30min, filtering, obtains filter residue；
3) filter residue obtained by step 2) is subjected to freezing processing three times, first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40 mesh sieve, obtains fine powder；
4) fine powder obtained by step 3) is subjected to radiation treatment at normal temperatures and pressures, irradiation dose 20kGy, it is dry to get.
B) the preparation of Herba Andrographitis extracting solution
1) the 5kg Herba Andrographitis dried be crushed into 90 mesh sieve, 50Kg water is then added, the item for being 800 revs/min in rotating speed
It is stirred evenly under part；Then in the case where output power is the microwave condition of 1200W, Microwave Extraction 40 minutes, filtering repeats extraction 2
It is secondary, merge extracting solution；
2) it is that 11kPa is concentrated into the 1/2 of original volume, obtains under the conditions of temperature is 60 DEG C in vacuum degree by gained extracting solution
Herba Andrographitis extracting solution.
C water purification agent) is prepared
1Kg chitosans are scattered in 2L Herba Andrographitis extracting solutions, 500g is added to sell phenol sodium again, complex are made, in complex
In plus the artificial bentonites of 300g just be made water purification agent.
【Embodiment 3】
A) the preparation of low-molecular weight chitoglycan：
1) it is 5% hydrogenperoxide steam generator to take mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
2) 1 ton of chitosan is immersed in mixed liquor obtained by step 1), the mass concentration of chitosan is 25%, is impregnated
30min, filtering, obtains filter residue；
3) filter residue obtained by step 2) is subjected to freezing processing three times, first time cryogenic temperature is -4 DEG C, when freezing for the first time
Between be 2h, second cryogenic temperature is -10 DEG C, and second of cooling time is 1h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40 mesh sieve, obtains fine powder；
4) fine powder obtained by step 3) is subjected to radiation treatment at normal temperatures and pressures, irradiation dose 20kGy, it is dry to get.
B) the preparation of Herba Andrographitis extracting solution
1) the 600kg Herba Andrographitis dried be crushed into 90 mesh sieve, 6 tons of water is then added, be 800 revs/min in rotating speed
Under the conditions of stir evenly；Then in the case where output power is the microwave condition of 1200W, Microwave Extraction 40 minutes, filtering repeats to extract
2 times, merge extracting solution；
2) it is that 11kPa is concentrated into the 1/3 of original volume, obtains under the conditions of temperature is 60 DEG C in vacuum degree by gained extracting solution
Herba Andrographitis extracting solution.
C water purification agent) is prepared
50Kg chitosans are scattered in 300L Herba Andrographitis extracting solutions, 20Kg is added to sell phenol sodium again, complex are made, compound
In body plus water purification agent is just made in the artificial bentonites of 100Kg.
Above description has fully disclosed the specific implementation mode of the present invention.It should be pointed out that being familiar with the field
Technical staff is to any change for being done of specific implementation mode of the present invention all without departing from the range of claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (8)
1. a kind of preparation method of water purification agent, it is characterised in that：
By commercially available chitosan be immersed in containing hydrogen peroxide, water-soluble humic acid solution in, after being soaked for a period of time, filtering obtains
Gained filter residue is carried out freezing processing three times, thaws, the chitosan after defrosting is dried in the shade, fine powder is ground by filter residue, and gained is thin
Powder carries out radiation treatment and obtains low-molecular weight chitoglycan at normal temperatures and pressures, and the low-molecular weight chitoglycan is scattered in Herba Andrographitis
In extracting solution, add multiple pin phenol sodium, complex is made, in complex plus water purification agent, the low molecule is just made in artificial bentonite
Amount chitosan is relative molecular weight 105Chitosan below.
2. the preparation method of water purification agent according to claim 1, which is characterized in that the low-molecular weight chitoglycan it is specific
Preparation method is as follows：
1) it is 5~12% hydrogenperoxide steam generator to take mass concentration, and water-soluble humic acid is added, and the quality of water-soluble humic acid is
The 0.2~0.6% of above-mentioned hydrogenperoxide steam generator, stirs evenly, and obtains mixed liquor；
2) chitosan being immersed in mixed liquor obtained by step 1), the mass concentration of chitosan is 25~35%, immersion 30~
50min, filtering, obtains filter residue；
3) filter residue obtained by step 2) is subjected to freezing processing three times, first time cryogenic temperature is -4 DEG C, and first time cooling time is 2
~4h, second of cryogenic temperature are -10 DEG C, and second of cooling time is 1~3h, and third time cryogenic temperature is -19 DEG C, third time
Cooling time is 40~60min, thaws, the filter residue after defrosting is dried in the shade, and is ground into fine powder, crosses 40~60 mesh sieve, obtains fine powder；
4) fine powder obtained by step S3 is subjected to radiation treatment at normal temperatures and pressures, irradiation dose is 20~30kGy, it is dry to get.
3. the preparation method of water purification agent according to claim 2, it is characterised in that：The mass concentration of chitosan in step 2)
It is 30%.
4. the preparation method of water purification agent according to claim 2, it is characterised in that：40min is impregnated in step 2).
5. the preparation method of water purification agent according to claim 2, it is characterised in that：First time, cooling time was in step 3)
3h, second of cooling time are 2h, and third time cooling time is 50min.
6. the preparation method of water purification agent according to claim 2, it is characterised in that：Radiation treatment when institute is carried out in step 4)
It is 60Co- gamma-rays with radiation source.
7. the preparation method of water purification agent according to claim 1, it is characterised in that：The Herba Andrographitis extracting solution is by following
Method is extracted：
1) dry Herba Andrographitis be crushed into 90 mesh sieve, the Extraction solvent of 10~20 times of quality is then added, be 800 in rotating speed
It is stirred evenly under conditions of rev/min；Then in the case where output power is the microwave condition of 1200W, Microwave Extraction 20~40 minutes,
Filtering repeats extraction 2~3 times, merges extracting solution；
2) it is that 7~11kPa is concentrated into the 1/3 of original volume under the conditions of temperature is 50~60 DEG C in vacuum degree by gained extracting solution
~1/2, obtain Herba Andrographitis extracting solution.
8. the preparation method of water purification agent according to claim 7, it is characterised in that：The Extraction solvent be tap water,
The sodium chloride of a concentration of 1.0mol/L, the acetic acid of a concentration of 0.1mol/L, a concentration of 0.01mol/L hydrochloric acid in one kind or several
Kind.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5269939A (en) * | 1992-07-13 | 1993-12-14 | Laurent Edward L | Method of solids recovery for use in animal feed or as a fuel utilizing natural flocculents |
| CN102259965A (en) * | 2011-05-19 | 2011-11-30 | 中国林业科学研究院资源昆虫研究所 | Moringa oleifera water purifying agent |
| CN105271452A (en) * | 2014-07-18 | 2016-01-27 | 重庆市昂多环境治理有限责任公司 | Water purifying agent production method |
| CN107652373A (en) * | 2017-09-26 | 2018-02-02 | 广州华大生物科技有限公司 | A kind of preparation method of low-molecular weight chitoglycan |
| CN107935136A (en) * | 2017-12-08 | 2018-04-20 | 方政 | A kind of special degerming water purification agent of aquaculture and its preparation process |
-
2018
- 2018-05-30 CN CN201810538709.5A patent/CN108675365A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5269939A (en) * | 1992-07-13 | 1993-12-14 | Laurent Edward L | Method of solids recovery for use in animal feed or as a fuel utilizing natural flocculents |
| CN102259965A (en) * | 2011-05-19 | 2011-11-30 | 中国林业科学研究院资源昆虫研究所 | Moringa oleifera water purifying agent |
| CN105271452A (en) * | 2014-07-18 | 2016-01-27 | 重庆市昂多环境治理有限责任公司 | Water purifying agent production method |
| CN107652373A (en) * | 2017-09-26 | 2018-02-02 | 广州华大生物科技有限公司 | A kind of preparation method of low-molecular weight chitoglycan |
| CN107935136A (en) * | 2017-12-08 | 2018-04-20 | 方政 | A kind of special degerming water purification agent of aquaculture and its preparation process |
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Effective date of registration: 20191025 Address after: Room 934, floor 9, building 9, yard 16, Junying street, Shunyi District, Beijing Applicant after: Beijing Xiangyun Zhihui Technology Co., Ltd. Address before: 528000 104 6 of South Jing Wan garden, 103 South Avenue, Leping Town, Sanshui District, Foshan, Guangdong (residence declaration) Applicant before: Foshan hang Xiang Qian an Technology Co., Ltd. |
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