CN1280104A - Method for preparing flocculent for treatment of chitosan water - Google Patents
Method for preparing flocculent for treatment of chitosan water Download PDFInfo
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- CN1280104A CN1280104A CN 00109435 CN00109435A CN1280104A CN 1280104 A CN1280104 A CN 1280104A CN 00109435 CN00109435 CN 00109435 CN 00109435 A CN00109435 A CN 00109435A CN 1280104 A CN1280104 A CN 1280104A
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Abstract
本发明提出的壳聚糖水处理絮凝剂的制备方法,首先使虾蟹壳脱去无机盐,进行固液分离,烘干得到脱无机盐产物,使虾蟹壳脱去蛋白质,将反应体系进行固液分离,烘干得到甲壳素产物,脱去乙酰基,将反应体系进行固液分离,烘干得到的固体颗粒即为壳聚糖水处理絮凝剂产品。本发明的产品絮体沉淀速度快,脱水效果良好,最终处理处置方便完全,无二次污染。The preparation method of the chitosan water treatment flocculant proposed by the present invention, first removes the inorganic salt from the shrimp and crab shells, performs solid-liquid separation, and dries to obtain the inorganic salt-removed product, removes the protein from the shrimp and crab shells, and solidifies the reaction system. Liquid separation, drying to obtain chitin products, removal of acetyl groups, solid-liquid separation of the reaction system, drying to obtain solid particles that are chitosan water treatment flocculant products. The floc of the product of the present invention has fast sedimentation speed, good dehydration effect, convenient and complete final treatment and disposal, and no secondary pollution.
Description
The present invention relates to a kind of preparation method of chitosan water processing flocculating agent, belong to water treatment flocculation technique field.
The water treatment flocculation technique, be meant in water and waste water and add flocculation agent, colloid in the water body, suspension solid-liquid body and dissolved organic matter are passed through physics chemical action, thereby remove turbidity, COD (chemical oxygen demand (COD)), colourity, suspended solids and other material in water and the waste water, the water quality of water and waste water is purified.The water treatment flocculation technique comprises the content of two aspects, flocculation process and flocculation agent.The medicament that flocculation agent is in the flocculation technique to be added, and flocculation process is meant the dosing method of flocculation agent, reaction times and and the complex method of multiple flocculation agent etc.The employed flocculation agent of water treatment flocculation technique mainly contains inorganic flocculating agent and organic polymer coargulator two big classes at present.Wherein inorganic flocculating agent is divided into ionic and aggretion type, and organic polymer coargulator can be divided three classes, negatively charged ion, positively charged ion and non-ionic type.
Existing water treatment flocculant shortcoming:
It is polymerize aluminum chloride comparatively widely that inorganic water treatment flocculant uses at present, and it is big that shortcoming mainly contains usage quantity, and its consumption is more than ten times of organic water treatment flocculant normally; The flco amount is big, and sedimentation speed is slow, dehydration difficulty, ultimate disposal cost height; The aluminum ion that remains in the water has potential harm to HUMAN HEALTH, and long-term excessive drinking can cause senile dementia; Low to temperature, the water treatment effect that turbidity is low is relatively poor; Removal effect to the organism micropollutant is relatively poor.
Organic water treatment flocculant is many, and to use more at present be polyacrylamide, and it has three kinds of negatively charged ion, positively charged ion and non-ionic types, is to generate with the industrial chemicals acrylamide polymerization, and the main drawback of present homemade polyacrylamide has molecular weight product lower; Remaining a large amount of poisonous acrylamide monomers can not be used for to water treatment; Complex manufacturing; Treatment effect to sanitary sewage and dyeing waste water is not good.
The objective of the invention is to propose a kind of preparation method of chitosan water processing flocculating agent, this flocculation agent is a kind of natural organic high-molecular water treatment flocculant, belongs to the weak cation type, directly preparation from shrimp and crab shells.
The preparation method of the chitosan water processing flocculating agent that the present invention proposes comprises following each step:
1, make shrimp and crab shells slough inorganic salt: add hydrochloric acid in shrimp and crab shells, the concentration of hydrochloric acid is 4～6% (mass ratioes), and the ratio of adding is that 1 gram shrimp and crab shells adds 10～15ml hydrochloric acid, at room temperature, reacts 2.5～15 hours, controls pH less than 4 with hydrochloric acid.
2, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off the inorganic salt product.
3, make the shrimp and crab shells deproteinize: in taking off the inorganic salt product, add sodium hydroxide solution, the concentration of sodium hydroxide solution is 4～10% (mass ratioes), the ratio of adding is that 1 gram takes off inorganic salt product adding 10～15ml sodium hydroxide solution, at 85～95 ℃, reacted 1～4 hour, stirring velocity is 50～90 rev/mins.
4, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains the chitin product.
5, deacetylate: add strong caustic in the chitin product, concentration sodium hydroxide is 45-55% (mass ratio), and the ratio of adding is that 1 gram chitin product adds 5～10ml concentrated sodium hydroxide, is 50～115 ℃ in temperature, reacts 2～16 hours.
6, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, the solid particulate that oven dry obtains is the chitosan water processing flocculating agent product.Product is the translucent solid of sheet, and a small amount of pearliness is arranged.
The chitosan water processing flocculating agent of the present invention's preparation has the following advantages:
The use raw material sources are extensive, and its Prawn shell is the waste of processing of aquatic products industry, and directly discharging pollutes the environment, and hydrochloric acid and sodium hydroxide also are the common chemical product.
Preparation technology is simple, and employed equipment all is conventional chemical industry equipment, and reaction conditions all carries out under normal pressure, and heating condition is realized easily; With short production cycle in addition, simple to operate.
Product is the natural organic high-molecular compound, is provided with toxic side effect, and biological degradation easily is environmentally friendly.
The flco sedimentation speed is fast, and dehydrating effect is good, and final treatment and disposal is fully convenient, non-secondary pollution.
Product has good treatment effect to low turbidity surface water, is that the independent use of low turbid surface water of 13.8NTU can make turbidity removal reach 62.3% to turbidity, can improve greatly with the clearance of the compound use of inorganic flocculating agent to turbidity, reaches 97%.
Product has good treatment effect to high turbidity surface water, uses the yangtze river in nanjing water turbidity clearance to 530NTU to reach 93.8% separately.
Product has good treatment effect and the compound use of inorganic flocculating agent that the clearance of sanitary sewage CODcr is reached 62.6% to sanitary sewage, and turbidity removal rate reaches 79.4%.
Product has good treatment effect to multiple waste water from dyestuff, and product uses separately or with compound use of polymerize aluminum chloride the chroma removal rate of concentration as 500mg/l weak acid red, 42 crowdes of RH, direct light turquoise blue GL, direct green G NB all reached more than 90%.
The used raw material shrimp and crab shells of the present invention is made up of three parts, inorganic salt, protein and chitin, but both content of three parts are different.The inorganic salt content of crab shell about 68%, protein content about 13%, chitin about 19%.The inorganic salt content of shrimp shell about 50%, protein content about 30%, chitin about 20%.By take off inorganic calcium, deproteinization obtains chitin, it is the straight chain shape polysaccharide that a kind of N-ethanoyl-D-Portugal amine sugar connects by β-(1,4) glycosidic link, its molecular formula is as follows:
The ethanoyl of kharophen on the chitin is sloughed, made to have a large amount of amino on the macromolecular chain, thereby make that high molecular solubility property, flocculating property and mating capability are strengthened greatly.This just obtains chitosan water processing flocculating agent, and its molecular formula is as follows:
Introduce embodiments of the invention below.
Embodiment one
1, take by weighing crab shell 10.1 grams, the hydrochloric acid 150ml with 6% at room temperature soaked 12 hours, controlled pH less than 4 with hydrochloric acid.
2, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off inorganic salt product 3.2 grams.
3, restrain the sodium hydroxide solution 32ml that takes off adding 5% in the inorganic salt product 3.2 and reacted 3 hours 80～90 rev/mins of stirring velocitys at 85～90 ℃ down.
4, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains chitin product 2.0 grams.
5, the sodium hydroxide solution 10.0ml of adding 50% in 2.0 gram chitin products reacted 16 hours down at 50～60 ℃.
6, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, the solid particulate that oven dry obtains is chitosan water processing flocculating agent, and weight is 1.8 grams.
Embodiment two
1, take by weighing crab shell 5.5 grams, the hydrochloric acid 82.5ml with 4% at room temperature soaked 15 hours, controlled pH less than 4 with hydrochloric acid.
2, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off inorganic salt product 1.7 grams.
3, restrain the sodium hydroxide solution 25ml that takes off adding 10% in the inorganic salt product 1.7 and reacted 3 hours 50～60 rev/mins of stirring velocitys at 90～95 ℃ down.。
4, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains chitin product 1.1 grams.
5, the sodium hydroxide solution 10.0ml of adding 55% in 1.1 gram chitin products reacted 2 hours down at 105～115 ℃.
6, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, promptly obtain chitosan water processing flocculating agent after the oven dry, weight is 0.95 gram.
Embodiment three
1, take by weighing shrimp shell 5.0 grams, adding concentration is 6% hydrochloric acid 50ml, at room temperature reacts 2.5 hours, controls pH less than 4 with hydrochloric acid.
2, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off inorganic salt product 2.9 grams.
3, take off adding concentration 4% sodium hydroxide 30ml on the inorganic salt product at 2.9 grams, under 85～95 ℃, reacted 70～80 rev/mins of stirring velocitys 1 hour.
4, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains chitin product 0.93 gram.
5, add concentration 45% sodium hydroxide 5ml at 0.93 gram chitin product, under 105～105 ℃, 2 hours reaction times.
6, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, promptly obtain chitosan water processing flocculating agent after the oven dry, weight is 0.82 gram.
Embodiment four
1, take by weighing shrimp shell 5.0 grams, adding concentration is 6% hydrochloric acid 50ml, at room temperature reacts 6 hours, controls pH less than 4 with hydrochloric acid.
2, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off inorganic salt product 2.7 grams.
3, take off adding concentration 4% sodium hydroxide 30ml on the inorganic salt product at 2.7 grams, under 85～95 ℃, reacted 70～80 rev/mins of stirring velocitys 3 hours.
4, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains chitin product 1.0 grams.
5, add concentration 45% sodium hydroxide 5ml at 1.0 gram chitin products, under 105～115 ℃, 2.5 hours reaction times.
6, after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, promptly obtain chitosan water processing flocculating agent after the oven dry, weight is 0.89 gram.
Claims (1)
1, a kind of preparation method of chitosan water processing flocculating agent is characterized in that, this method comprises following each step:
(1) make shrimp and crab shells slough inorganic salt: add hydrochloric acid in shrimp and crab shells, the quality of hydrochloric acid is 4～6% than concentration, and the ratio of adding is that every gram shrimp and crab shells adds 10～15ml hydrochloric acid, at room temperature, reacts 2.5～15 hours, controls pH less than 4 with hydrochloric acid;
(2) after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains taking off the inorganic salt product;
(3) make the shrimp and crab shells deproteinize: in taking off the inorganic salt product, add sodium hydroxide solution, the quality of sodium hydroxide solution is 4～10% than concentration, the ratio of adding is that every gram takes off inorganic salt product adding 10～15ml sodium hydroxide solution, at 85～95 ℃, reacted 1～4 hour, stirring velocity is 50～90 rev/mins;
(4) after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, oven dry obtains the chitin product;
(5) deacetylate: add strong caustic in the chitin product, the quality of sodium hydroxide is 45-55% than concentration, and the ratio of adding is that every gram chitin product adds 5～10ml concentrated sodium hydroxide, is 50～115 ℃ in temperature, reacts 2～16 hours;
(6) after reaction finishes, reaction system is carried out solid-liquid separation, the solid phase after separating is flushed to neutrality, the solid particulate that oven dry obtains is chitosan water processing flocculating agent product of the present invention.
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| CN 00109435 CN1119294C (en) | 2000-06-23 | 2000-06-23 | Method for preparing flocculent for treatment of chitosan water |
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| CN 00109435 CN1119294C (en) | 2000-06-23 | 2000-06-23 | Method for preparing flocculent for treatment of chitosan water |
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| CN1280104A true CN1280104A (en) | 2001-01-17 |
| CN1119294C CN1119294C (en) | 2003-08-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390076C (en) * | 2006-08-02 | 2008-05-28 | 袁毅桦 | Preparation method of chitin-alginic acid copolymer flocculant |
| CN101284693B (en) * | 2008-05-26 | 2010-06-02 | 董超平 | Natural organic polymer composite flocculant, method for preparing the same and applications |
| CN101200505B (en) * | 2007-11-29 | 2011-01-19 | 湖北东方天琪生物工程股份有限公司 | Method for preparing high deacetylate degree and high viscosity chitosan by using shrimp shell |
| CN102108101A (en) * | 2010-11-24 | 2011-06-29 | 重庆工商大学 | Preparation method for natural polymer flocculant used for oil liquid purification |
| CN106006890A (en) * | 2016-06-24 | 2016-10-12 | 佛山科学技术学院 | Preparation method of chitosan coagulant |
| CN106467424A (en) * | 2015-08-19 | 2017-03-01 | 武汉禾之壮农业科技有限公司 | A kind of chitosan and its preparation technology of organic water-soluble fertilizer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343180C (en) * | 2004-12-31 | 2007-10-17 | 西北大学 | Chitin/chitosan water processing flocculating agent and its preparing method |
-
2000
- 2000-06-23 CN CN 00109435 patent/CN1119294C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390076C (en) * | 2006-08-02 | 2008-05-28 | 袁毅桦 | Preparation method of chitin-alginic acid copolymer flocculant |
| CN101200505B (en) * | 2007-11-29 | 2011-01-19 | 湖北东方天琪生物工程股份有限公司 | Method for preparing high deacetylate degree and high viscosity chitosan by using shrimp shell |
| CN101284693B (en) * | 2008-05-26 | 2010-06-02 | 董超平 | Natural organic polymer composite flocculant, method for preparing the same and applications |
| CN102108101A (en) * | 2010-11-24 | 2011-06-29 | 重庆工商大学 | Preparation method for natural polymer flocculant used for oil liquid purification |
| CN102108101B (en) * | 2010-11-24 | 2013-02-20 | 重庆工商大学 | Preparation method for natural polymer flocculant used for oil liquid purification |
| CN106467424A (en) * | 2015-08-19 | 2017-03-01 | 武汉禾之壮农业科技有限公司 | A kind of chitosan and its preparation technology of organic water-soluble fertilizer |
| CN106467424B (en) * | 2015-08-19 | 2019-07-23 | 武汉禾之壮农业科技有限公司 | A kind of preparation process of chitosan and its organic water-soluble fertilizer |
| CN106006890A (en) * | 2016-06-24 | 2016-10-12 | 佛山科学技术学院 | Preparation method of chitosan coagulant |
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