CN1393410A - Organic-inorganic composite flocculant and its preparing process - Google Patents
Organic-inorganic composite flocculant and its preparing process Download PDFInfo
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- CN1393410A CN1393410A CN 01108579 CN01108579A CN1393410A CN 1393410 A CN1393410 A CN 1393410A CN 01108579 CN01108579 CN 01108579 CN 01108579 A CN01108579 A CN 01108579A CN 1393410 A CN1393410 A CN 1393410A
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Abstract
A composite organic-inorganic flocculant with the merits of organic and inorganic flocculants especially suitable for treating the high-basicity and high-chromaticity sewage is prepared from the polymer of dicyanobiamine with formaldehyde, aluminium chloride polysulfide and/or aluminium calcium chloride polysulfide through hydrolysis reaction, polymerizing and polycondensation. Its advantages are simple process and no waste discharge.
Description
The invention belongs to the flocculation agent field, particularly a kind of flocculation agent of use in waste water treatment and production method thereof.
Flocculation agent is widely used in wastewater treatment, with regard to existing flocculation agent, can be divided into inorganic flocculating agent and organic floculant two big classes by Chemical Composition.In inorganic flocculating agent, take the status as the leading factor with inorganic polymer flocculant, as molysite class and aluminium saline flocculating agents such as polymerized ferric-aluminum chloride, polymeric aluminum sulfate silicate and poly-phosphorus Tai-Ace S 150 such as poly-sulphur iron(ic) chloride, poly-phosphorus iron(ic) chloride, polymeric silicicacid iron, polymer phosphate iron.Though sterilization, the sterilization effectively of this type of flocculation agent, purify liquid waste, have that consumption is big, efficient is low, produce shortcomings such as scum silica frost is many.The principal item of organic polymer coargulator has polyacrylamide (PAM), polymethacrylate-acrylonitrile copolymer, polyester polyamines, polyvinyl phenmethyl quaternary ammonium salt etc., they are compared with inorganic polymer flocculant has advantages such as consumption is little, flocculation ability is strong, efficient is high, the generation scum silica frost is few, but weak point is a waste residue water ratio height, and the soiling solution volume that is produced is bigger.
The objective of the invention is to overcome the deficiencies in the prior art, a kind of organic-inorganic composite flocculant and production method thereof are provided, this kind flocculation agent has the advantage of existing inorganic flocculating agent and organic floculant concurrently, be specially adapted to the processing of high basicity, high-colour intensity wastewater, its production method technology is simple, use conventional equipment, no waste gas, waste water, waste residue are discharged.
Organic-inorganic composite flocculant provided by the present invention comprises the polymkeric substance of Dicyanodiamide and formaldehyde, poly-sulphur aluminum chloride and/or poly-sulphur aluminum calcium chloride, is transparent thick, and the chemical general formula of the polymkeric substance of Dicyanodiamide and formaldehyde is [C
3H
6N
4O]
n, 5≤n≤10 and be integer.
The production method of above-mentioned composite flocculation agent is that to adopt " one bathes synthesis method " to carry out organic floculant and inorganic flocculating agent composite, and concrete technology has two kinds.
One, first kind of technology
1. raw material and prescription thereof (massfraction)
Aluminium salt 5～15%
Calcium salt 10～20%
Dicyanodiamide 2～8%
Formaldehyde 2～9%
Water surplus
2. processing step and processing parameter
Comprise following processing step successively, each processing step all carries out under normal pressure.
(1) hydrolysis reaction
Aluminium salt is put into 50 ℃～65 ℃ water, hydrolysis under agitation, after the dissolving of aluminium salt, with the pH value of acid or alkali accent solution, PH is controlled at 1.0～3.0.
(2) polyreaction
The hydrolyzed solution that under agitation calcium salt is added aluminium salt is warming up to 90 ℃～100 ℃, adds polymerization promotor then, and the reaction times is 1～3 hour.
(3) polycondensation
Under agitation will fuse agent and Dicyanodiamide and add in the above-mentioned solution, and wait to dissolve the back and add formaldehyde, promptly get product in 5～8 hours 90 ℃～100 ℃ reactions.
In this technology, aluminium salt is Tai-Ace S 150 or aluminum chloride; Calcium salt is calcium chloride or nitrocalcite; It is organic acid or mineral acid that the used acid of solution pH value is separated in water transfer, organic acid can be formic acid or acetate or oxalic acid or tartrate or citric acid etc., mineral acid can be sulfuric acid or hydrochloric acid or phosphoric acid etc., alkali is generally selected sodium hydroxide for use, polymerization promotor is water glass or rare earths salt, the add-on of water glass is 1～2% (massfraction), and rare earths salt can be light rare earths salt such as cerium salt, and its add-on is 0.1～0.2% (massfraction); Fused agent is an inorganic ammonium salt, can select ammonium sulfate or ammonium chloride or monoammonium sulfate or primary ammonium phosphate etc. for use, and its add-on is 1～2% (massfraction).
Two, second kind of technology
1. raw material and prescription thereof (massfraction)
Aluminium salt 10～30%
Dicyanodiamide 6～15%
Formaldehyde 8～16%
Water surplus
2. processing step and processing parameter
Processing step comprises hydrolysis reaction, polyreaction and polycondensation, above-mentioned processing step has two kinds of order, a kind of order is polycondensation → hydrolysis and polyreaction, and another kind of order is hydrolysis reaction → polycondensation and polyreaction, and each processing step all carries out under normal pressure.
(1) polycondensation → hydrolysis and polyreaction
A, polycondensation
At first heat water to 90 ℃～100 ℃ and adding acid accent pH value, PH is controlled at 1.0～2.0, under agitation adds Dicyanodiamide then, adds formaldehyde after waiting to dissolve and be incubated 4～5 hours at 90 ℃～100 ℃ promptly to finish polycondensation.
B, hydrolysis and polyreaction
Under agitation aluminium salt is added in the solution that polycondensation obtained, then the temperature of solution is reduced to 80 ℃～90 ℃ insulation reaction and promptly got product in 2～3 hours.
(2) hydrolysis reaction → polycondensation and polyreaction
A, hydrolysis reaction
At first heat water to 90 ℃～100 ℃ and adding acid accent pH value, PH is controlled at 0.5～1.0, under agitation adds aluminium salt then, promptly gets hydrating solution after the dissolving of aluminium salt.
B, polycondensation and polyreaction
Under agitation Dicyanodiamide is added said hydrolyzed solution, solubilizing reaction added formaldehyde in 0.5～1 hour, promptly got product in 5～7 hours 90 ℃～100 ℃ insulation reaction.
In this technology, aluminium salt is Tai-Ace S 150 or aluminum chloride; The used acid of the pH value of water transfer is organic acid or mineral acid, and organic acid can be formic acid or acetate or oxalic acid or tartrate or citric acid etc., and mineral acid can be sulfuric acid or hydrochloric acid or phosphoric acid etc.
The present invention has the following advantages and positively effect:
1. amount of consumption of drugs is low during wastewater treatment, and the add-on of composite flocculation agent only is 10～800mg/L.
2. water treatment effect ideal, every index of waste water after treatment are that SS reduces by 96%～100%; COD
CrReduce by 76%～88%; BOD reduces by 70%～82%; Colourity reduces by 96%～100%.Especially to the waste water of high basicity, high chroma, the reuse again of the water after the processing.
3. compare with organic polymer coargulator, the water ratio of waste residue can reduce by 40%～60%, and the volume of mud can reduce 50%～60%.
4. to the waste water of high basicity, high chroma, the waste residue after the processing can be used as the raw material of products such as synthol, super strength water absorbent, paint filler, turns waste into wealth.
5. product stability is good, and nontoxic and fragrance slightly uses and is not subjected to season, region limits, is convenient to deposit and transport.
6. production technique is simple, and raw materials for production are easy to get, and is with short production cycle, reaction temperature and, required equipment is a conventional equipment, is convenient to existing chemical plant and practices midwifery.
7. whole process flow does not have waste gas, waste water, waste sludge discharge, is a kind of free of contamination Production Flow Chart that cleans.
Fig. 1 is a kind of process flow sheet according to the production method of organic-inorganic composite flocculant proposed by the invention;
Fig. 2 is second kind of process flow sheet according to the production method of organic-inorganic composite flocculant proposed by the invention;
Fig. 3 is the third process flow sheet according to the production method of organic-inorganic composite flocculant proposed by the invention.
Further specify the present invention with embodiment below.
Embodiment 1:
The raw material of present embodiment and prescription thereof (massfraction):
Tai-Ace S 150 10%
Calcium chloride 15%
Dicyanodiamide 5%
Formaldehyde 5%
Water surplus
The processing step of present embodiment and processing parameter:
The processing step of present embodiment and order as shown in Figure 1, each processing step all carries out under normal pressure.
(1) hydrolysis reaction
Add required water in reactor, water temperature is controlled at 60 ℃, under agitation adds Tai-Ace S 150 then, and after the Tai-Ace S 150 dissolving, the pH value of test soln is transferred pH value to 2.5 with hydrochloric acid or sodium hydroxide.
(2) polyreaction
Calcium chloride is under agitation added in the said hydrolyzed liquid, be warming up to 95 ℃ and to add massfraction be that 1.0% water glass promotes polymerization then, the reaction times is 2 hours.
(3) polycondensation
With massfraction is that fused agent of 1.2% ammonium sulfate and Dicyanodiamide under agitation add in the solution after polyreaction is finished, adds formaldehyde again after waiting to dissolve, and promptly gets the composite flocculant product in 6 hours 95 ℃ of insulation reaction.
Embodiment 2:
The raw material of present embodiment and prescription thereof (massfraction):
Aluminum chloride 20%
Dicyanodiamide 10%
Formaldehyde 10%
Water surplus
The processing step of present embodiment and processing parameter:
The processing step of present embodiment and order as shown in Figure 2, each processing step all carries out under normal pressure.
(1) polycondensation
Add required water in reactor, water temperature is controlled at 100 ℃, and adding formic acid transfers to 1.5 with the pH value of water, under agitation adds Dicyanodiamide then, waits to dissolve the back and adds formaldehyde and promptly finished polycondensation in 4 hours 100 ℃ of insulations.
(2) hydrolysis and polyreaction
Under agitation aluminum chloride is added in the solution that polycondensation obtains, then the temperature of solution is reduced to 80 ℃ of insulation reaction and promptly got the composite flocculation agent product in 3 hours.
Embodiment 3:
The raw material of present embodiment and prescription thereof (massfraction):
Aluminum chloride 15%
Dicyanodiamide 8%
Formaldehyde 10%
Water surplus
The processing step of present embodiment and processing parameter:
The processing step of present embodiment and order as shown in Figure 3, each processing step all carries out under normal pressure.
(1) hydrolysis reaction
Add required water in the reactor, water temperature is controlled at 90 ℃, adds the industrial vitriol oil pH value of water is transferred to 1.0, under agitation adds aluminum chloride then, promptly gets hydrating solution after the aluminum chloride dissolving.
(2) polycondensation and polyreaction
Under agitation Dicyanodiamide is added said hydrolyzed solution, solubilizing reaction added formaldehyde in 1 hour, promptly got the composite flocculation agent product in 7 hours 90 ℃ of insulation reaction.
Claims (10)
1. an organic-inorganic composite flocculant is characterized in that comprising the polymkeric substance of Dicyanodiamide and formaldehyde, poly-sulphur aluminum chloride and/or poly-sulphur aluminum calcium chloride, is transparent thick, and the chemical general formula of the polymkeric substance of Dicyanodiamide and formaldehyde is [C
3H
6N
4O]
n, 5≤n≤10 and be integer.
2. the production method of the described organic-inorganic composite flocculant of claim 1 is characterized in that:
(1) raw material and prescription thereof (massfraction)
Aluminium salt 5～15%
Calcium salt 10～20%
Dicyanodiamide 2～8%
Formaldehyde 2～9%
Water surplus
(2) processing step and processing parameter
Comprise following processing step successively, each processing step all carries out under normal pressure,
A, hydrolysis reaction
Aluminium salt is put into 50～65 ℃ water, hydrolysis under agitation, after the dissolving of aluminium salt, with the pH value of acid or alkali accent solution, PH is controlled at 1.0～3.0,
B, polyreaction
The hydrolyzed solution that under agitation calcium salt is added aluminium salt is warming up to 90 ℃～100 ℃, adds polymerization promotor then, and the reaction times is 1～3 hour,
C, polycondensation
Under agitation will fuse agent and Dicyanodiamide and add in the above-mentioned solution, and wait to dissolve the back and add formaldehyde, promptly get product in 5～8 hours 90 ℃～100 ℃ reactions.
3. the production method of the described organic-inorganic composite flocculant of claim 1 is characterized in that:
(1) raw material and prescription thereof (massfraction)
Aluminium salt 10～30%
Dicyanodiamide 6～15%
Formaldehyde 8～16%
Water surplus
(2) processing step and processing parameter
Processing step comprises hydrolysis reaction, polyreaction and polycondensation, above-mentioned processing step has two kinds of order, and a kind of order is polycondensation → hydrolysis and polyreaction, and another kind of order is hydrolysis reaction → polycondensation and polyreaction, each processing step all carries out under normal pressure
A, polycondensation → hydrolysis and polyreaction
A. polycondensation
At first heat water to 90 ℃～100 ℃ and also add acid accent pH value, PH is controlled at 1.0～2.0, under agitation adds Dicyanodiamide then, and wait to dissolve back adding formaldehyde and promptly finished polycondensation in 4～5 hours 90 ℃～100 ℃ insulations,
B. hydrolysis and polyreaction
Under agitation aluminium salt is added in the solution that polycondensation obtained, then the temperature of solution is reduced to 80 ℃～90 ℃ insulation reaction and promptly got product in 2～3 hours,
B, hydrolysis reaction → polycondensation and polyreaction
A. hydrolysis reaction
At first heat water to 90 ℃～100 ℃ and adding acid accent pH value, PH is controlled at 0.5～1.0, under agitation adds aluminium salt then, promptly gets hydrating solution after the dissolving of aluminium salt,
B. polycondensation and polyreaction
Under agitation Dicyanodiamide is added said hydrolyzed solution, solubilizing reaction added formaldehyde in 0.5～1 hour, promptly got product in 5～7 hours 90 ℃～100 ℃ insulation reaction.
4. the production method of organic-inorganic composite flocculant according to claim 2 is characterized in that polymerization promotor is water glass or rare earths salt, and the add-on of water glass is 1～2%, and the add-on of rare earths salt is 0.1～0.2%.
5. according to the production method of claim 2 or 4 described organic-inorganic composite flocculants, it is characterized in that fused agent is an inorganic ammonium salt, add-on is 1～2%.
6. according to the production method of claim 2 or 4 described organic-inorganic composite flocculants, it is characterized in that calcium salt is calcium chloride or nitrocalcite.
7. the production method of organic-inorganic composite flocculant according to claim 5 is characterized in that calcium salt is calcium chloride or nitrocalcite.
8. according to the production method of claim 2 or 3 described organic-inorganic composite flocculants, it is characterized in that aluminium salt is Tai-Ace S 150 or aluminum chloride.
9. according to the production method of claim 2 or 3 described organic-inorganic composite flocculants, it is characterized in that transferring the used acid of pH value is organic acid or mineral acid.
10. the production method of organic-inorganic composite flocculant according to claim 8, it is characterized in that transferring the used acid of pH value is organic acid or mineral acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011085797A CN1192979C (en) | 2001-06-26 | 2001-06-26 | Organic-inorganic composite flocculant and its preparing process |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB011085797A CN1192979C (en) | 2001-06-26 | 2001-06-26 | Organic-inorganic composite flocculant and its preparing process |
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| CN1393410A true CN1393410A (en) | 2003-01-29 |
| CN1192979C CN1192979C (en) | 2005-03-16 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241818A (en) * | 2013-05-29 | 2013-08-14 | 滁州友林科技发展有限公司 | Organic/inorganic compound type flocculant |
| CN103253752A (en) * | 2013-05-29 | 2013-08-21 | 滁州友林科技发展有限公司 | High-efficiency flocculant |
| CN108046466A (en) * | 2017-12-07 | 2018-05-18 | 重庆精创联合环保工程有限公司 | The processing method of sanitary sewage |
| CN109319905A (en) * | 2018-10-22 | 2019-02-12 | 新疆环境工程技术有限责任公司 | Decolorising agent for dyeing and printing sewage |
| CN110228925A (en) * | 2019-06-21 | 2019-09-13 | 宁夏三瑞机械环保设备有限公司 | A kind of dehydration-type curing agent and preparation method thereof |
-
2001
- 2001-06-26 CN CNB011085797A patent/CN1192979C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241818A (en) * | 2013-05-29 | 2013-08-14 | 滁州友林科技发展有限公司 | Organic/inorganic compound type flocculant |
| CN103253752A (en) * | 2013-05-29 | 2013-08-21 | 滁州友林科技发展有限公司 | High-efficiency flocculant |
| CN103241818B (en) * | 2013-05-29 | 2014-06-18 | 滁州友林科技发展有限公司 | Organic/inorganic compound type flocculant |
| CN108046466A (en) * | 2017-12-07 | 2018-05-18 | 重庆精创联合环保工程有限公司 | The processing method of sanitary sewage |
| CN109319905A (en) * | 2018-10-22 | 2019-02-12 | 新疆环境工程技术有限责任公司 | Decolorising agent for dyeing and printing sewage |
| CN110228925A (en) * | 2019-06-21 | 2019-09-13 | 宁夏三瑞机械环保设备有限公司 | A kind of dehydration-type curing agent and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1192979C (en) | 2005-03-16 |
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Owner name: FUZHOU UNIV. Free format text: FORMER OWNER: LIU MINGHUA Effective date: 20100122 |
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Effective date of registration: 20100122 Address after: Fuzhou City Road 523, Post Code: 350002 Patentee after: Fuzhou University Address before: Fuzhou University of Fuzhou School of Environment and Resources Post Code: 350002 Patentee before: Liu Minghua Patentee before: Gong Yichang |
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Granted publication date: 20050316 Termination date: 20190626 |