CN100347197C - Clean preparation process of chitin - Google Patents
Clean preparation process of chitin Download PDFInfo
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- CN100347197C CN100347197C CNB2005100233515A CN200510023351A CN100347197C CN 100347197 C CN100347197 C CN 100347197C CN B2005100233515 A CNB2005100233515 A CN B2005100233515A CN 200510023351 A CN200510023351 A CN 200510023351A CN 100347197 C CN100347197 C CN 100347197C
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Abstract
The present invention provides a clean chitin preparation technology which belongs to the technical field of chemical industry. According to the clean chitin preparation technology, after being processed in advance, the raw material is boiled with alkali, washed with water, soaked with acid and washed with water, and finally, a finished product is obtained. Compared with the existing conventional technology, the clean chitin preparation technology changes the original preparation technology which does not process raw material into the preparation technology processing the raw material in advance, changes the original preparation technology in which raw material is firstly soaked with acid and then boiled with alkali into the preparation technology in which the raw material is firstly boiled with alkali and then soaked with acid, recycles the original acid immersion fluid which is not recovered, and changes the single physicochemical treatment of comprehensive waste water into combined treatment of biochemistry and physicochemistry. Therefore, the discharge quantity of waste can be reduced, resource utilization is carried out on the waste, and the environmental pollution is reduced to the minimum extent.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind of production technique of chitin.
Background technology
Chitin is isolated a kind of natural polymers from shells such as shrimp, crab.Because this biomaterial has nontoxic, good biocompatibility, biodegradable, good film-forming property, thereby obtained using comparatively widely at aspects such as wastewater treatment, foodstuffs industry, weaving, chemical industry, household chemicals, agricultural, biotechnology and medicine.But chitin preparation at present is a raw material with the crustacean waste that produces in the aquatic food processing enterprise course of processing, and in collecting raw material and transportation raw material process, stinking smell assaulting one's nostrils because of the crustacean waste rots to produce, and has a strong impact on environment.Raw material prepares in the point of destination in the chitin production process can produce a kind of high density organic high-salinity wastewater, and its pollutant component is a large amount of CaCl
2, salt such as NaCl, a large amount of animal proteinum (shrimp, crab glutelin) and degraded product thereof, shrimp (crab) shell pigment, grease, raw material itself impurity, a spot of chitin and the chitosan etc. brought into.To produce 1 ton of chitin daily, will discharge 10～150,000 tons of production wastes every year to environment water.Raw water is pitch-black smelly, and eutrophication, aquaculture and water environment environment is brought serious threat, even also can bring out red tide.In the improvement of chitin production waste, take simple end treatment mode at present, disposable having high input, the running expense height, and be difficult to realize up to standard.
If pollutent can be handled in the source, promptly by suitable process for cleanly preparing with the pollutent resource utilization, its pollution load reduction, then its comprehensive discharge waste water can be handled the sewage drainage standard to GB-1996 by the UASB-aerobic process.
There is limited evidence currently of has chitin cleaner production report and treating waste water from production of chitin successful story.Water outlet COD after some manufacturers administer is about 700mg/L (as Zhoushan, Ningbo) generally, can not reach the sewage drainage standard of country.The unfavorable reason of regulation effect is: the existence of chlorion is to the obstruction and itself contribution to the COD measured value of sewage disposal (especially biological treatment).The COD value is 100～150mg/L in the state sewage emission standard, if do not carry out the concentration of chlorion in the recovery of calcium chloride by product in the spent picking solution and the control comprehensive wastewater, water outlet just can not reach national sewage drainage standard.Unless with a large amount of fresh water dilutions (more than 10 times), and the most of producers that produce chitin are all coastal, fresh water is more scarce, moreover does the total release that can not reduce COD like this.So the chitin production waste can not only lean on end treatment.And the end treatment of present most of waste water for producing crust element just becomes waste residue with waste water, and waste residue is stacked landfill, and contaminated soil and underground water form vicious cycle, destroy ecotope.For this reason, some producer has paid very high economic cost, and sewage discharge indexs such as COD are also below standard.
Existing relevant waste water for producing crust element treatment process, mainly containing the Dalian City Environmental Science ﹠ Design Inst adopts biological contact oxidation process to handle waste water for producing crust element (its COD is that 2270mg/l, SS are that 442mg/l and pH are 9.57), treatment scale is 10 cubic metres/hour, the waste water every index of discharge water after treatment reaches " coastland, Liaoning Province sewage directly enters the marine site standard " requirement in (DB21-59-89), and wherein COD, SS and pH are respectively 140mg/l, 62mg/l and 7.27.Jiangsu Province such as target city light industry institute utilize acid-base neutralisation and add the CPF flocculation agent waits until method, reclaims the things such as protein in the waste liquid, does not handle the every index of back discharge water but address in this article.In the period of the 1999-2000, Yuhuan county Huahai chitin refinery, Marine Biological Chemistry Co. Ltd., Yuhuan County, the plump biochemistry corporation,Ltd. in Taizhou, enterprises such as Aoxing Chitin Co., Ltd., Yuhuan County successively entrust the Huzhou City Institute of Environmental Science, Mechano-Electronic Designing research Inst. of Zhejiang Prov environmental protection public works design and research institute, Ecological Envionment Research Centre, Chinese Academy of Sciences, Hangzhou clear water Genie et Environnement, nearly ten units such as Beijing Guohuan Tsinghua Environmental Engineering Design ﹠ Research Institute design 6 waste water for producing crust element processing schemes, wherein successful implementation operates 4 schemes, the waste water treatment engineering of building up adopts materialization to be treated to the master, washing water 80% reuse, fs, discharge water COD was lower than 1000mg/l, SS is 200mg/l, pH6～9, colourity is no more than 80.In addition, some waste water for producing crust element treatment project have also been implemented on ground such as Zhoushan and Qingdao, but treatment effect is not really desirable.
Because waste water for producing crust element is rich in organism and inorganics, constitute complicated, high COD value and high chloride content cause adopting conventional way improvement such as biochemical process, are treated to main end treatment and adopt with materialization, pollutent is all concentrated on afterbody to be handled, quantity is many, and load is big, the resource and the energy can not be maximally utilised, once investment and working cost height can't bear enterprise.Therefore, waste water for producing crust element is treated as a difficult problem of being eager to solve both at home and abroad.
Obviously, fundamentally administer the waste water that is produced in the chitin production process, must reform, adopt process for cleanly preparing production technique.
Summary of the invention
The objective of the invention is at existing the problems referred to above in the existing chitin production process, a kind of clean preparation process of chitin of novelty is provided, pollution source from the chitin production process begins to administer, reduce the waste discharge amount, refuse is carried out recycling, environmental pollution is reduced to minimum degree.
Purpose of the present invention can realize by following technical proposal: this clean preparation process of chitin is finished through the following steps:
1, raw materials pretreatment: animal shell waste raw materials such as the shrimp of collecting, crab shell are placed container, soaked 24～72 hours, squeeze then with sodium hydroxide lye;
2, soda boiling: preparation sodium hydroxide soda boiling liquid, previous step is put into through pretreated raw material, with 120～130 ℃ of steam treatment 0.5～1 hour;
3, washing: shell is put into the pond with the fresh water washing, make the shell drying then;
4, acidleach: it is in 8～9% the hydrochloric acid soln that shell is dropped into concentration, places half an hour approximately, treats to pick up when hydrochloric acid soln no longer produces bubble; Again shell is dropped into concentration and be in 5～6% the hydrochloric acid soln and soaked 3～4 hours.
5, washing: the shell after the acidleach is washed with fresh water, centrifuge dripping then, dry at last or dry finished product.
In above-mentioned clean preparation process of chitin, sodium hydroxide lye is formulated by the waste liquid hydro-oxidation soda of dipping by lye in waste liquid after the soda boiling in the step 2 and the step 1 in the described step 1, and its concentration is 8～15%.Therefore, the alkali soak liquid that leaches through squeezing obtains utilizing.
In above-mentioned clean preparation process of chitin, the concentration of sodium hydroxide soda boiling liquid is 8～15% in the described step 2.
In above-mentioned clean preparation process of chitin, soda boiling liquid can add proper amount of sodium hydroxide and carries out soda boiling next time in the described step 2 after using once.
In above-mentioned clean preparation process of chitin, making shell exsiccant mode in the described step 3 is a kind of in draining, dry, dry or drying.
In step 4, after washing, shell is dried acidleach again, can reduce the water of bringing into by shell and enter pickling liquor.During actually operating, make the pickling liquor original volume as far as possible little; And when acid concentration is little during to decalcification again, add concentrated hydrochloric acid or high density spent acid again, to reduce the energy expenditure of pickling liquor cumulative volume when reducing evaporation.To the certain volume after-filtration, the filtrate crystallisation by cooling plays and reduces calcium chloride content and COD total amount that enters environment and the effect of reclaiming calcium chloride by product and hydrochloric acid waste liquid with evaporator evaporation.The reuse of distillation residual solution is done acidleach with sour, and distillate is washed water as shrimp, crab shell after the acidleach, again with the neutralization of discharging waste lye, but also water saving.
In the acid leaching process of step 4, with the collection and confinement of gases that produces in the reaction, allow it wait by raw material package, moistening lime carbonate pipe (desalination acid mist or hydrogen chloride gas), discolour silica gel (removing water vapour) successively after, be compressed into liquid state, bottle.Reclaim and purifying by product CO
2The solvent of shrimp green grass or young crops (red) plain (ester) is extracted in sale of bottling back or conduct.Simultaneously, make technical grade or food-class CO
2Sell.
In above-mentioned clean preparation process of chitin, water lotion is taken from the waste liquid after the washing in the step 5 in the described step 3.Like this, can reduce the comprehensive wastewater volume, water saving.
Comprehensive wastewater is by the mode of anaerobism or UASB-aerobic treatment (or reflocculation), both can remove organic pollutant, produce biogas, be used for fuel, generating etc., can be converted into available organic fertilizer to nitrogen, phosphorus, the potassium that plant in the waste liquid can not directly utilize again.Enter the pond of exposing to the sun behind the Digestive system separated sludge after the fermentation and carry out aerobic treatment or reflocculation or chemical oxidation, water outlet qualified discharge.Can make the high-quality organic fertilizer after the anaerobic sludge dehydration, the residual active sludge that the aeration tank produces returns anaerobic unit and handles to reduce sludge quantity.
Step 1 is by carrying out pre-treatment to raw material, and environment does not distribute foul smell towards periphery, and most protein are separated with crust, can cut down things such as protein, water significantly and enter post-order process.
In above-mentioned technology, owing to the work in-process with first soda boiling deproteinize, fat and pigment, by the centrifugal waste liquid of sloughing, waste liquid is back to the soda boiling of next batch raw material, except that first, adds the soda boiling water in the whole alkali cooking process as far as possible no longer in addition.Therefore, the cumulative volume and the volume that enters in the subsequent technique of soda boiling waste liquid have been controlled.Simultaneously, the shell after the soda boiling washing also carries out centrifuge dehydration, and with in soda boiling waste liquid and the spent acid that distills out and after reclaiming protein, its clear liquid is incorporated into comprehensive wastewater, or is back to raw materials pretreatment.
In above-mentioned technology, the chitin finished product of biological calcium is sloughed in acidleach, by washing and the centrifugal liquid of sloughing, enter subsequent technique, the cumulative wastewater pickling distills resources such as recyclable residue hydrochloric acid in back and calcium chloride.
At last, the chitin finished product through bleaching is carried out drying and packaging, comprehensive wastewater is flocculated, the supernatant liquor reuse, all the other comprehensive wastewaters carry out anaerobism or acidification hydrolization or UASB and handle the back reuse, have only a small amount of discharging.
Compare with existing conventional technology, the advantage of this clean preparation process of chitin is:
1, this process for cleanly preparing becomes original production process raw material is not treated to pre-treatment.Because raw material has been carried out pre-treatment, do by dipping by lye, squeezing filter fresh feed, not only control the generation of the putrid and deteriorated and foul smell of raw material, and cut down materials such as protein, water significantly and enter this follow-up workshop section of soda boiling, can reduce energy consumption and alkali consumption and soda boiling washes amount in the soda boiling workshop section process.
2, this process for cleanly preparing become after the first acidleach of original production process soda boiling into first soda boiling after acidleach, thereby avoided a large amount of shrimps, crab glutelin and degraded product thereof, astaxanthin, grease etc. to mix with polynary intersection of pickling liquor, for the reuse of pickling liquor and the biochemical treatment of follow-up waste water create conditions, solved original production process because of organism in the pickling liquor and the polynary intersection mixing of inorganics, constitute complexity, high COD value and high chloride content, cause to adopt the 'bottleneck' restrictions of conventional way improvement such as biochemical process.
3, this process for cleanly preparing souring immersion liquid is not recovered as recycling.Behind solid matters such as pickling liquor elimination shrimp shell, be evaporated to certain volume, the filtrate crystallisation by cooling reclaims calcium chloride.The distillation residual solution partly or entirely is back to use the acidleach pond, and with the soda boiling waste liquid, the part distillate of latter stage is used for making flocculation agent FeCl in also can partly or entirely being used for
2(add a small amount of waste iron filing in wherein, behind the reaction certain hour, elimination scum), surplus person as acidleach after first and second time wash water of shrimp shell.
4, the single materialization of this process for cleanly preparing change comprehensive wastewater is treated to the biochemical processing that combines with materialization.Comprehensive wastewater is by natural subsidence, separation, and the reuse of supernatant liquor part is as bath water, after part is handled with anaerobism or UASB, and reflocculation or aerobic again or qualified discharge after the strong oxide treatment of chemistry again.
Description of drawings
Accompanying drawing is the skeleton diagram of this clean preparation process of chitin.
Embodiment
Below in conjunction with accompanying drawing and this clean preparation process of chitin is specified.
It is the animal shell waste that this chitin is produced used raw material, as shrimp shell or crab shell.
Embodiment one
At first animal shell waste raw materials such as the shrimp of collecting, crab shell are placed the large vol plastic tank, add 8% sodium hydroxide lye and soaked 70 hours, squeeze then; With the most liquid reuses that extrude, other liquid and shell are put into the soda boiling pond.
Then, compound concentration was 2.2 tons of 15% sodium hydroxide soda boiling liquid, with 130 ℃ of steam treatment housings 0.5 hour.Boil completely, drained 10 minutes.Carry out for the second time and later soda boiling after adding proper amount of sodium hydroxide in the former soda boiling liquid.Chitin per ton must boil 6～9 ponds.
Then, the shell gradation is put into the pond and wash the shell water rinse after with acidleach.After washing 2～3 batches of housings, wash water drains into the composite wastewater pond.Shell is dried after centrifugal.
During wash water, the weight ratio of shell and water is about 1: 2 when washing for the first time.
It then is acidleach.With 1 ton of the hydrochloric acid soln of last consignment of second acidleach pond spent picking solution preparation 8%, place in the first acidleach pond, drop into an amount of shell, place half an hour approximately, treat to pick up when hydrochloric acid soln no longer produces bubble, and put to the second acidleach pond.Add 6 tons of 5.8% hydrochloric acid in the second acidleach pond, shell is soaked picked up in 3 hours.
After an amount of interpolation technical hydrochloric acid to its concentration is 8% once again in first pond, drop into second batch of shell again, so circulation.
Be washing at last.Shell after the acidleach is washed with water earlier, centrifuge dripping then, dry at last the target product chitin.
Embodiment two
At first animal shell waste raw materials such as the shrimp of collecting, crab shell are placed the large vol plastic tank, add 15% sodium hydroxide lye and soaked 24 hours, squeeze then; With the most liquid reuses that extrude, other liquid and shell are put into the soda boiling pond.
Then, compound concentration was 2.5 tons of 9% sodium hydroxide soda boiling liquid, with 120 ℃ of steam treatment housings 1 hour.Boil completely, drained 10 minutes.Carry out for the second time and later soda boiling after adding proper amount of sodium hydroxide in the former soda boiling liquid.Chitin per ton must boil 6～9 ponds.
Then, the shell gradation is put into pond clear water rinsing.After washing 2～3 batches of housings, wash water drains into the composite wastewater pond.The centrifugal back of shell is dried.
During wash water, the weight ratio of shell and water is about 1: 1.5 when washing for the first time.
It then is acidleach.With 1 ton of the hydrochloric acid soln of last consignment of second acidleach pond spent picking solution preparation 8.9%, place in the first acidleach pond, drop into an amount of shell, place half an hour approximately, treat to pick up when hydrochloric acid soln no longer produces bubble, and put to the second acidleach pond.Add 6 tons of 5% hydrochloric acid in the second acidleach pond, shell is soaked picked up in 4 hours.
After an amount of interpolation technical hydrochloric acid to its concentration is 8.9% once again in first pond, drop into second batch of shell again, so circulation.
Be washing at last.Shell after the acidleach is washed with water earlier, centrifuge dripping then, dry at last the target product chitin.
Through actual tests, adopt this production technique after, can reach following effect:
1, to produce 1 ton of chitin daily, squeezes filtrate in the raw materials pretreatment, 1.5～1.8 tons of the recyclable solid substances that contains high-quality protein 12.93%.In 800 yuan per ton, 1200～1440 yuan of day economic benefits, offset its cost after, also can slightly increase income, have certain economic benefits.
2, the decrement discharge of soda boiling waste water
Recyclable 0.42～0.5 ton of the high-quality protein solid substance such as shrimp red (green grass or young crops) element that is rich in the soda boiling waste liquid, in 2000 yuan per ton, 820～1000 yuan of day economic benefits (need not flocculation agent, only need dry expense).
3, little discharging of spent picking solution
After spent picking solution distilled,, can save 1.9 ton of 30% hydrochloric acid and reclaim 2.5 tons of calcium chloride and all acid diffusion water to produce 1 ton of chitin daily, 1010～1014 yuan of day economic benefits, offset its cost after, also can slightly increase income, have certain economic benefits.
4, can reduce about 0.52 ton of inorganic COD day total release, the discharging of waste liquid total amount be reduced to common process 1/30 (establishing cleaner production equates with spent picking solution cumulative volume in the former technology, waste liquid is after 8 circulations in the cleaner production, the degree of its " dirty " is no more than former technology, and the spent acid amount of little discharging have only its cumulative volume 1/4 or littler, 4 * 8=32 ≈ 30), has significant environmental benefit.
5, adopt the terminal treatment process of comprehensive wastewater, the UASB-aerobic treatment method of the waste water of chitin cleaner production just, CODCr be the waste water of 10000mg/L earlier after anaerobic treatment, water outlet CODCr is reduced to 1400mg/L, average COD Cr clearance reaches more than 75%; After handling with aerobic method, CODCr reaches below the 150mg/L again, and average COD Cr clearance is greater than 86%, and the BOD clearance meets GB-8978-1996II level emission standard greater than 96% simultaneously.
6, the process for cleanly preparing of this chitin reduces 0.5 ton of CODCr day total emission volumn from spent picking solution, and (establish 300 tons of the Sino-Japan waste discharges of old technology, the CODCr discharge value is 300～1000mg/L) to account in the comprehensive wastewater CODCr about 84.7～62.5%; Can save water of productive use every day and be no less than 150 tons; The CODCr value 100～300mg/L of comprehensive washes discharging.
Test-results shows that the process for cleanly preparing of this chitin can satisfy the standard of COD≤150mg/L fully.Simultaneously, because the required equipment investment is less relatively, technology is simpler, and the ton cost of water treatment is less than 3 yuan, and the waste water control expense is relatively low.
Claims (7)
1, a kind of clean preparation process of chitin is characterized in that this technology finishes through the following steps:
(1), raw materials pretreatment: animal shell waste raw materials such as the shrimp of collecting, crab shell are placed container, soaked 24～72 hours, squeeze then with sodium hydroxide lye;
(2), soda boiling: preparation sodium hydroxide soda boiling liquid, previous step is put into through pretreated raw material, with 120～130 ℃ of steam treatment 0.5～1 hour;
(3), washing: shell is put into the pond with the fresh water washing, make the shell drying then;
(4), acidleach: it is in 8～9% the hydrochloric acid soln that shell is dropped into concentration, places half an hour approximately, treats to pick up when hydrochloric acid soln no longer produces bubble; Again shell is dropped into concentration and be in 5～6% the hydrochloric acid soln and soaked 3～4 hours.
(5), washing: the shell after the acidleach is washed with fresh water, centrifuge dripping then, dry at last or dry finished product.
2, clean preparation process of chitin according to claim 1, it is characterized in that, sodium hydroxide lye is formulated by the waste liquid hydro-oxidation soda of dipping by lye in waste liquid after the soda boiling in the step 2 and the step 1 in the described step 1, and its concentration is 8～15%.
3, clean preparation process of chitin according to claim 1 is characterized in that, the concentration of sodium hydroxide soda boiling liquid is 8～15% in the described step 2.
According to claim 1 or 3 described clean preparation process of chitin, it is characterized in that 4, soda boiling liquid can add proper amount of sodium hydroxide and carries out soda boiling next time in the described step 2 after using once.
5, clean preparation process of chitin according to claim 1 is characterized in that, making shell exsiccant mode in the described step 3 is a kind of in draining, dry, dry or drying.
6, clean preparation process of chitin according to claim 1 is characterized in that, the collection and confinement of gases that will produce in will reacting in step 4 allows it successively by behind raw material package, moistening lime carbonate pipe, the discolour silica gel, is compressed into liquid state, bottling.
7, clean preparation process of chitin according to claim 1 is characterized in that, water lotion is taken from the waste liquid after the washing in the step 5 in the described step 3.
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| CN112390448A (en) * | 2020-09-01 | 2021-02-23 | 江西吉润花炮新材料科技有限公司 | Treatment method of nitrified bamboo cellulose alkali cooking wastewater |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW273579B (en) * | 1994-11-30 | 1996-04-01 | China Textile Inst | Method to use chitin as starch agent for warping |
| CN1191863A (en) * | 1997-02-25 | 1998-09-02 | 浙江省商业集团进出口公司 | Chitin preparing process using crust of silkworm chrysalis |
| CN1384121A (en) * | 2001-04-27 | 2002-12-11 | 薛雄生 | Natural chitin extracting technology |
| CN1526739A (en) * | 2003-03-06 | 2004-09-08 | 国家海洋局第二海洋研究所 | Clean chitin producing process |
-
2005
- 2005-01-14 CN CNB2005100233515A patent/CN100347197C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW273579B (en) * | 1994-11-30 | 1996-04-01 | China Textile Inst | Method to use chitin as starch agent for warping |
| CN1191863A (en) * | 1997-02-25 | 1998-09-02 | 浙江省商业集团进出口公司 | Chitin preparing process using crust of silkworm chrysalis |
| CN1384121A (en) * | 2001-04-27 | 2002-12-11 | 薛雄生 | Natural chitin extracting technology |
| CN1526739A (en) * | 2003-03-06 | 2004-09-08 | 国家海洋局第二海洋研究所 | Clean chitin producing process |
Non-Patent Citations (2)
| Title |
|---|
| 甲壳质、壳聚糖的制备及性质 段莉梅，等.哲里木畜牧学院学报，第6卷第2期 1996 * |
| 药用辅料－甲壳素工艺的研究 吴晴斋，等.南京部队医药，第1995年第5期 1995 * |
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Assignee: Jinke Biological-Chemistry Co., Ltd., Zhejiang Assignor: Xu Junyi|Zhou Xiangchi|Lin Rongye Contract fulfillment period: 2007.11.7 to 2023.11.6 contract change Contract record no.: 2008330002548 Denomination of invention: Clean chitin producing process Granted publication date: 20071107 License type: Exclusive license Record date: 20081210 |
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