CN101215053B - Circulation utilization method for waste water in seaweed chemical industry production - Google Patents
Circulation utilization method for waste water in seaweed chemical industry production Download PDFInfo
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- CN101215053B CN101215053B CN2007101163044A CN200710116304A CN101215053B CN 101215053 B CN101215053 B CN 101215053B CN 2007101163044 A CN2007101163044 A CN 2007101163044A CN 200710116304 A CN200710116304 A CN 200710116304A CN 101215053 B CN101215053 B CN 101215053B
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Abstract
The invention discloses a method of sewage water recycling in seaweed chemical industry production, the steps of which include that pre-treating sodium alginate crude liquid gum, checking the capacity of alginic acid in the pre-treated liquid gum and adding corresponding weight of calcium chloride according to the capacity of alginic acid to precipitate out calcium alginate sufficiently, collecting the separated supernatant fluid and the sewage water formed in the process of generation, checking the capacity of calcium chloride and adding corresponding weight of water treatment agent which can deposit all calcium ions, displaying still for one night and separating out the supernatant fluid, which replaces tap water to be directly used for the dilution of next sodium alginate crude liquid gum; the separated supernatant fluid can be reciprocally used according to the method of the invention. The manufacturing technique of the invention can reduce the discharging capacity of the seaweed chemical industry sewage water at 80% or more, further, the invention not only doesn't influence the volume of production and the quality of the chemical product, but also creates remarkable economic benefit, still achieves distinct social benefit and ecological benefit.
Description
Technical field
The present invention relates to a kind of method of cycling utilization of wastewater, relate in particular to the cycling utilization of wastewater method in a kind of seaweed chemical production.Belong to cycling utilization of wastewater technical field in " energy-saving and emission-reduction ".
Background technology
Marine alga is important marine chemical industry raw material.The marine alga of present industrial development and use mainly is a brown alga, comprises that sea-tangle, bulk kelp, laver, sargassun, black wrack, bladder wrack, the gloomy algae of love, thick leaf separate that graceful algae, sea accumulate, wakame, Sargassum fusiforme etc.The marine alga industry of American States is many to be raw material with the bulk kelp, and Japan is raw material many accumulateing with sea-tangle and sea.The advantage brown alga resource of China is a sea-tangle, and annual production accounts for more than 70% of world wide production, and therefore, the marine alga industry of China all is raw material basically with the sea-tangle.
The sodium alginate of producing with brown alga (also being called algin), iodine, N.F,USP MANNITOL, fucoidin etc. are the important source material of industries such as medicine, food, weaving.Wherein sodium alginate is the product of output maximum, and its production technique has had the history in more than 30 year.Sodium alginate along with the development in market, has been widely used in aspects such as seal spins, food, chemical industry, medicine, agricultural since finding, its demand is increasing.
The seaweed chemical manufacturing enterprise of China all is that the old technology of employing is the production that raw material carries out sodium alginate with the sea-tangle now, 1000 tons of the about water consumptions of one ton of sodium alginate of every production, these water have discharged after all being taken as waste water process simple process at present, not only waste precious water resource in a large number, and power consumption is high, also causes heavy environmental pressure.Along with strengthening day by day and national strictness restriction in proposition aspect the energy-saving and emission-reduction of people's environmental consciousness, existing sodium alginate production technique has been difficult to satisfy the demand of each side, is badly in need of setting up the sodium alginate new process of production that meets " energy-saving and emission-reduction " requirement.
The technology that with the sea-tangle is the raw material production sodium alginate is: with dried sea-tangle with a large amount of water logging bubbles more than 10 hours, extract iodine and N.F,USP MANNITOL composition, be cut into fragment about 10 centimetres with machine then, use the clear water repetitive scrubbing, clean bur attached to the sea-tangle surface; Use the Na of 1-3% then
2CO
3Make digestive pharmaceutical, the Lalgine in the sea-tangle is changed into the sodium alginate of solubility; Become the thick glue of mud shape thickness sodium alginate after the sea-tangle digestion, wherein contain a large amount of fiber-like and do not allow residue and impurity, because sodium alginate viscosity is very big, could remove tiny dregs and impurity makes sodium alginate dilution glue cleaning by operations such as floating, filtrations after needing to add a large amount of water and diluting; The sodium alginate dilution glue that to handle after filtration again adds an amount of calcium chloride, makes water soluble algae acid sodium change water-insoluble alginate calcium into and separates out; Alginate calcium is transformed into Lalgine through the dilute hydrochloric acid decalcification; Obtain sodium alginate after Lalgine after the decalcification handled with sodium carbonate solution or solid sodium carbonate.
In this technological process, produce a large amount of waste water, wherein contain impurity such as large amount of organic and inorganic salt.Especially dilute the wastewater flow rate maximum that the thick glue of the postdigestive thickness sodium alginate of sea-tangle alkaline hydrolysis produces.Handling these waste water had both needed complex apparatus, also consumed lot of energy, human and material resources and financial resources, not only increased production cost, and the serious waste water resources, and serious environment pollution has caused huge pressure for local ecotope.This is main and one of difficult problem key that present seaweed chemical industry faces.
Summary of the invention
Big at water consumption in the seaweed chemical technology, produce the big difficult problem of wastewater flow rate, the problem that the present invention requires to solve provides the cycling utilization of wastewater method of a kind of seaweed chemical in producing.
The inventor has studied successfully seaweed chemical cycling utilization of wastewater technology through repetition test and improvement, makes the water consumption of whole seaweed chemical technological process save more than 80%, has not only reduced production cost, and has saved water resources, has reduced environmental pollution.
Cycling utilization of wastewater method during seaweed chemical of the present invention is produced, step comprises:
(1) the thick glue of sposh shape thickness sodium alginate that marine alga alkaline hydrolysis digestion back is formed, tap water dilution with 6-10 times of volume, sodium alginate glue after the dilution is removed still indigested marine alga root, piece through conventional coarse filtration earlier, centrifugal with the rotating speed more than the 3000rpm then, separate the suspended substance of removing in marine alga slag and the sodium alginate dilution glue, obtain clarifying sodium alginate dilution glue;
(2) the pH value of usual manner regulating step (1) sodium alginate dilution glue is to neutral, detect sodium alginate and dilute the Lalgine content in the glue and comply with the calcium chloride that its amount adds corresponding amount, stirring makes water soluble algae acid sodium change water-insoluble alginate calcium into and fully separates out;
(3) calcium alginate gel is leached or carry out liquid-solid separation through the draining device, it is standby to collect separated liquid supernatant; Isolated alginate calcium is with the dilute hydrochloric acid solution decalcification of 1-3 times of volume, the Lalgine after the decalcification in a usual manner again with yellow soda ash prepared in reaction sodium alginate, the waste water that forms in its process is same collect standby;
(4) calcium chloride content in detection step (3) supernatant liquor, that complies with its amount adding corresponding amount can make the abundant sedimentary water conditioner of calcium ion, standing over night is isolated supernatant liquor, and the described tap water of supernatant liquor alternative steps (1) directly applies to the dilution of the thick glue of next batch sodium alginate; Separated liquid supernatant is with the use that moves in circles of step (1) to (4) method;
Perhaps, supernatant liquor and waste water that combining step (3) is collected, with calcium chloride is index, detect the calcium chloride content that merges in the solution of back, that complies with its amount adding corresponding amount can make the abundant sedimentary water conditioner of calcium ion, standing over night is isolated supernatant liquor, and the described tap water of supernatant liquor alternative steps (1) directly applies to the dilution of the thick glue of next batch sodium alginate; Separated liquid supernatant is with the use that moves in circles of step (1) to (4) method.
In the cycling utilization of wastewater method during above-mentioned seaweed chemical is produced: described water conditioner is to form the harmless chemical reagent that the insoluble solid precipitation is removed at the calcium ion impurities that can making of the development of the impurity in the seaweed chemical waste water is unfavorable for the waste water recycled and influences quality product.The moiety of described water conditioner mainly is aluminum oxide flocculation agent and inorganic salt, and its mixed weight ratio is 1: 2～4, preferred 1: 3.The preferred commercially available water conditioner of described water conditioner is as the aluminum oxide flocculation agent that Yellow River in Henan jewel Industry investment limited-liability company sells, the yellow soda ash that grouping of the world economy factory in mountain sells in the Nanjing.
In the cycling utilization of wastewater method during above-mentioned seaweed chemical is produced: described marine alga is that sea-tangle, bulk kelp, sea accumulate, in the wakame one or more.
The waste water generation is greatly one of crucial difficult problem of facing of seaweed chemical industry, for example produces the sea-tangle chemical industry factory of 25 tons of sodium alginates daily, will produce more than 25000 ton of waste water in process of production every day.If these a large amount of waste water are handled the back qualified discharge according to relevant emission standard, need to drop into a large amount of funds and set up special-purpose water processing establishment, not only consume big energy, fund and manpower, take very large space, and cause the waste of great lot of water resources.If administer boundary's discharging without strictness, then both waste water resources causes serious environmental to pollute again.The present invention has realized the recycle of seaweed chemical 80% above waste water by to produce the chemical treatment and the recycled of the formed waste water of sodium alginate with marine alga, has saved water resources, has reduced the discharging of seaweed chemical waste water, has reduced production cost.Experiment confirm: can carry out recycled more than 15 times with the method for step of the present invention, and not influence the quality of sodium alginate, have economic benefit, social benefit and the ecological benefits of highly significant.
Embodiment
Embodiment 1:
Get dried sea-tangle 150kg, add 1500L water logging bubble 2h, filter, add 500L water logging bubble 2h again, filter, add 500L water logging bubble 2h again, filter, filtrate being used to extracted iodine and N.F,USP MANNITOL, the sea-tangle of soaking is cut into fragment about 10cm with machine, soaks 4h with 1% formaldehyde again, carry out chromopexy, water rinses out formaldehyde then.The sea-tangle of rinsing well is with 1% Na
2CO
3Solution, under 60 ℃ of temperature condition, digestion 4h obtains the molten product of heavy-gravity mud shape sea-tangle alkali, approximately 3000L.
These thickness glues are divided into 15 parts, every part of about 200L, number 1.-
(1) get and number 1. glue, add the 1200L fresh water towards rare, the glue after rare is removed still indigested Radix Laminariae, piece through coarse filtration earlier, goes out suspended substance in kelp residue and the glue by centrifugation then, obtains clarifying glue.Reconcile about pH value to 7, the Lalgine content in the check and analysis glue calculates the amount that calcium chloride need add.In glue, add 10% calcium chloride 60L according to calculation result, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 1. supernatant liquor reclaims standby immediately with calcium alginate gel.Dilute hydrochloric acid decalcification with 3% washes with water one time at last, drains away the water; With 2M soaking in sodium carbonate solution Lalgine, make pH about 8, and keep stable, add dehydrated alcohol precipitation sodium alginate.The gained sodium alginate is carried out centrifugal, remove supernatant liquor, obtain sodium alginate.
(2) detect the calcium chloride content of supernatant liquor in 1., calculating need all to precipitate impurity such as calcium ion the amount of the water conditioner that adds, adding water conditioner 25g all precipitates impurity such as calcium ion, and standing over night, supernatant liquor is used to number the 2. dilution of glue, glue after rare is removed still indigested Radix Laminariae, piece through coarse filtration earlier, goes out suspended substance in kelp residue and the glue by centrifugation then, obtains clarifying glue.Regulate about pH value to 7, the Lalgine content in the check and analysis glue calculates the amount that calcium chloride need add.In glue, add an amount of 10% calcium chloride 62L according to calculation result, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 2. supernatant liquor reclaims standby immediately with calcium alginate gel.Dilute hydrochloric acid decalcification with 3% washes with water one time, drains away the water, and pulverize, press 1: 1 mixed with 90% ethanol, add 40% sodium hydroxide solution then, pH is maintained about 8, and keep stable, the gained sodium alginate is carried out centrifugal, remove supernatant liquor, and dewater to water content to 65%, pulverize, add the anhydrous Na of alginic acid weight 8%
2CO
3Powder, through thorough mixing, neutralization is complete, and making its apparent pH is 7, is dried to water content 15% then once, pulverizes the sodium alginate that gets product.
By that analogy, recycle, up to using supernatant liquor
After treatment, be used for numbering
The flushing of glue, and the above-mentioned identical row operation of process obtains numbering
Sodium alginate.
Merge 1.-
The finished product sodium alginate, amount to 27kg, towards rare water consumption 1200L, save towards rare water about 93%.
Embodiment 2
Get dried sea-tangle 300kg, add 3000L water logging bubble 2h, filter, add 1000L water logging bubble 2h again, filter, add 1000L water logging bubble 1h again, filter, filtrate being used to extracted iodine and N.F,USP MANNITOL, the sea-tangle of soaking is cut into stick about 10cm with machine, soaks 4h with 1% formaldehyde again, carry out chromopexy, water rinses out formaldehyde then.The sea-tangle of rinsing well is with 1.2% Na
2CO
3Solution, under 60 ℃ of temperature condition, digestion 4h obtains heavy-gravity alginic acid mud shape thing, approximately 6000L.
These thickness glues are divided into 15 parts, every part of about 400L, number 1.-
(1) get and number 1. glue, add the 2400L fresh water towards rare, the glue after rare is removed still indigested Radix Laminariae, piece through coarse filtration earlier, goes out suspended substance in kelp residue and the glue by centrifugation then, obtains clarifying glue.Reconcile about pH value to 7, the Lalgine content in the check and analysis glue calculates the amount that calcium chloride need add.In glue, add 10% calcium chloride 120L according to calculation result, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 1. supernatant liquor reclaims standby immediately with calcium alginate gel.Decalcification washes with water one time at last with 3% dilute hydrochloric acid, drains away the water, and pulverize, press 1: 1 mixed with 90% ethanol, add 40% sodium hydroxide solution then, pH is maintained about 8, and keep stable, the gained sodium alginate is carried out centrifugal, remove supernatant liquor, and dewater to water content to 65%, pulverize, add the anhydrous Na of alginic acid weight 8%
2CO
3Powder, through thorough mixing, neutralization is complete, and making its apparent pH is 7, is dried to water content 15% then once, pulverizes the sodium alginate that gets product.
(2) detect the calcium chloride content of supernatant liquor in 1., calculating makes the amount that impurity such as calcium ion all precipitates needs to add water conditioner, adding water conditioner 50g all precipitates impurity such as calcium ion, and standing over night, it is rare that supernatant liquor is used to number dashing of 2. glue, glue after rare is removed still indigested Radix Laminariae, piece through coarse filtration earlier, goes out suspended substance in kelp residue and the glue by centrifugation then, obtains clarifying glue.Reconcile about pH value to 7, the Lalgine content in the check and analysis glue calculates the amount that calcium chloride need add.In glue, add 10% calcium chloride 123L according to calculation result, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 2. supernatant liquor reclaims standby immediately with calcium alginate gel.Decalcification washes with water one time at last with 3% dilute hydrochloric acid, drains away the water, and pulverize, press 1: 1 mixed with 90% ethanol, add 40% sodium hydroxide solution then, pH is maintained about 8, and keep stable, the gained sodium alginate is carried out centrifugal, remove supernatant liquor, and dewater to water content to 65%, pulverize, add the anhydrous Na of alginic acid weight 8%
2CO
3Powder, through thorough mixing, neutralization is complete, and making its apparent pH is 7, is dried to water content 15% then once, pulverizes the sodium alginate that gets product.
By that analogy, recycle, up to using supernatant liquor
After treatment, be used for numbering
The flushing of glue, and the above-mentioned identical row operation of process obtains numbering
Sodium alginate.
Merge 1.-
The finished product sodium alginate, amount to 55kg, towards rare water consumption 2400L, save towards rare water about 92%.
Embodiment 3
Get dried bulk kelp 100kg, add 1000L water logging bubble 2h, filter, add 350L water logging bubble 2h again, filter, add 350L water logging bubble 2h again, filter, filtrate being used to extracted iodine and N.F,USP MANNITOL, the bulk kelp of soaking is cut into stick about 5cm with machine, soaks 4h with 1% formaldehyde again, carry out chromopexy, water rinses out formaldehyde then.The bulk kelp of rinsing well is with 1% Na
2CO
3Solution, under 60 ℃ of temperature condition, digestion 4h obtains heavy-gravity alginic acid mud shape thing, approximately 2000L.
These thickness glues are divided into 15 parts, every part of about 135L, number 1.-
(1) get and number 1. glue, add the 810L fresh water towards rare, the glue after rare is removed still impurity such as indigested bulk kelp earlier through coarse filtration, goes out suspended substance in bulk kelp slag and the glue by centrifugation then, obtains clarifying glue.Reconcile about pH value to 7, the Lalgine content in the check and analysis glue calculates the amount that calcium chloride need add.In glue, add calcium chloride solution 41L according to calculation result, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 1. supernatant liquor reclaims standby immediately with calcium alginate gel.Dilute hydrochloric acid decalcification with 3% washes with water one time, drains away the water.With 2M soaking in sodium carbonate solution Lalgine, make pH about 8, and keep stable, add dehydrated alcohol precipitation sodium alginate.The gained sodium alginate is carried out centrifugal, remove supernatant liquor, obtain sodium alginate.
(2) detect the calcium chloride content of supernatant liquor in 1., calculating makes the amount that impurity such as calcium ion all precipitates needs to add water conditioner, add water conditioner 17g, impurity such as calcium ion are all precipitated, and standing over night, it is rare that supernatant liquor is used to number dashing of 2. glue, and the glue after rare is removed still indigested bulk kelp root, piece through coarse filtration earlier, go out suspended substance in bulk kelp slag and the glue by centrifugation then, obtain clarifying glue.Reconcile about pH value to 7, the Lalgine content in the check and analysis glue calculates and makes the excessive slightly volume that needs 10% calcium chloride of adding of calcium chloride.In glue, add 10% calcium chloride 42L according to the volume that calculates, obtain calcium alginate gel.Through draining device draining, with the decalcification of dilute hydrochloric acid solution wash-out, 2. supernatant liquor reclaims standby immediately with calcium alginate gel.Decalcification washes with water one time at last with 3% dilute hydrochloric acid, drains away the water, and pulverize, press 1: 1 mixed with 90% ethanol, add 40% sodium hydroxide solution then, pH is maintained about 8, and keep stable, the gained sodium alginate is carried out centrifugal, remove supernatant liquor, and dewater to water content to 65%, pulverize, add the anhydrous Na of alginic acid weight 8%
2CO
3Powder, through thorough mixing, neutralization is complete, and making its apparent pH is 7, is dried to water content 15% then once, pulverizes the sodium alginate that gets product.
By that analogy, recycle, up to using supernatant liquor
After treatment, be used for numbering
The flushing of glue, and the above-mentioned identical row operation of process obtains numbering
Sodium alginate.
Merge 1.-
The finished product sodium alginate, amount to 20kg, towards rare water consumption 810L, save towards rare water about 90%.
The moiety of the described water conditioner of the embodiment of the invention mainly is aluminum oxide flocculation agent and inorganic salt (yellow soda ash), and its mixed weight ratio is 1: 3.Wherein, the aluminum oxide flocculation agent is available from Yellow River in Henan jewel Industry investment limited-liability company, and yellow soda ash is available from grouping of the world economy factory in mountain in the Nanjing.
Claims (6)
1. the cycling utilization of wastewater method during a seaweed chemical is produced, step comprises:
(1) the thick glue of sposh shape thickness sodium alginate that marine alga alkaline hydrolysis digestion back is formed, tap water dilution with 6-10 times of volume, sodium alginate glue after the dilution is removed still indigested marine alga root, piece through conventional coarse filtration earlier, centrifugal with the rotating speed more than the 3000rpm then, separate the suspended substance of removing in marine alga slag and the sodium alginate dilution glue, obtain clarifying sodium alginate dilution glue;
(2) the pH value of usual manner regulating step (1) sodium alginate dilution glue is to neutral, detect sodium alginate and dilute the Lalgine content in the glue and comply with the calcium chloride that its amount adds corresponding amount, stirring makes water soluble algae acid sodium change water-insoluble alginate calcium into and fully separates out;
(3) calcium alginate gel is leached or carry out liquid-solid separation through the draining device, it is standby to collect separated liquid supernatant;
Isolated alginate calcium is with the dilute hydrochloric acid solution decalcification of 1-3 times of volume, the Lalgine after the decalcification in a usual manner again with yellow soda ash prepared in reaction sodium alginate, the waste water that forms in its process is same collect standby;
(4) calcium chloride content in detection step (3) supernatant liquor, that complies with its amount adding corresponding amount can make the abundant sedimentary water conditioner of calcium ion, standing over night is isolated supernatant liquor, and the described tap water of supernatant liquor alternative steps (1) directly applies to the dilution of the thick glue of next batch sodium alginate; Separated liquid supernatant is with the use that moves in circles of step (1) to (4) method;
Perhaps, supernatant liquor and waste water that combining step (3) is collected, with calcium chloride is index, detect the calcium chloride content that merges in the solution of back, that complies with its amount adding corresponding amount can make the abundant sedimentary water conditioner of calcium ion, standing over night is isolated supernatant liquor, and the described tap water of supernatant liquor alternative steps (1) directly applies to the dilution of the thick glue of next batch sodium alginate; Separated liquid supernatant is with the use that moves in circles of step (1) to (4) method;
Wherein: above-mentioned water conditioner is meant that the calcium ion impurities that is unfavorable for the waste water recycled and influences quality product at can making of the development of the impurity in the seaweed chemical waste water forms the harmless chemical reagent that the insoluble solid precipitation is removed.
2. the cycling utilization of wastewater method during seaweed chemical is produced according to claim 1 is characterized in that: described marine alga is that sea-tangle, bulk kelp, sea accumulate, in the wakame one or more.
3. the cycling utilization of wastewater method during seaweed chemical is produced according to claim 1, it is characterized in that: described water conditioner is commercially available water conditioner.
4. the cycling utilization of wastewater method in producing as seaweed chemical as described in the claim 3, it is characterized in that: the moiety of described water conditioner is flocculation agent and inorganic salt.
5. the cycling utilization of wastewater method in producing as seaweed chemical as described in the claim 4, it is characterized in that: the moiety of described water conditioner is aluminum oxide flocculation agent and yellow soda ash, its mixed weight ratio is 1: 2～4.
6. the cycling utilization of wastewater method in producing as seaweed chemical as described in the claim 5, it is characterized in that: the moiety of described water conditioner is aluminum oxide flocculation agent and yellow soda ash, its mixed weight ratio is 1: 3.
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| CN101870528B (en) * | 2010-05-27 | 2011-11-02 | 中国水产科学研究院黄海水产研究所 | Dibasic precipitation method for treating calcium-containing wastewater in phaeophyceae industry |
| CN102701513B (en) * | 2011-11-29 | 2014-10-01 | 青岛聚大洋藻业集团有限公司 | New process for wastewater recycling comprehensive treatment in alga processing |
| CN102745841B (en) * | 2012-05-25 | 2013-10-09 | 中国水产科学研究院黄海水产研究所 | Novel brown algae chemical waste calcium water recycling process |
| CN103360511B (en) * | 2013-07-31 | 2016-01-20 | 青岛海之林生物科技开发有限公司 | A kind of production technique of self-solidifying type sodium alginate |
| CN103665184B (en) * | 2013-12-23 | 2015-08-19 | 山东洁晶集团股份有限公司 | A kind of method reducing hydrochloric acid calcium chloride consumption in sodium alginate production |
| CN104292361A (en) * | 2014-09-27 | 2015-01-21 | 山东黄河三角洲纺织科技研究院有限公司 | Method for recycling sodium alginate from reactive dye printing wastewater by virtue of calcium coagulation-chelating agent process |
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